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TECHNICAL REPORT
FD-12
FLAVORING MATERIALS FOR
HIGH CALORIC FOOD BARS
by
-4E. J HEWITT
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$. -3/^1 5 . 0 "7^? JUIY 1965
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EVANS RESEARCH AND DEVELOPMENT CORPORATION
New York 17. New York
Confroct No DA19 129 AMC 2113{x) (017012)
U. S. ARMY NATICK LABORATORIES Natick Massachusetts
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TECHNICAL REPORT FD-12
FLAVORING MATERIALS FOR HIGH CALORIC FOOD BARS
by
E. J. Hewitt
EVANS RESEARCH AND DEVELOPMENT CORPORATION New York 17, N. Y.
Contract No. DA19-129-AMC-2113(X) (01 7012)
Project Reference: 7X84-06-031 July 1965
U. S. Army Materiel Command U. S. ARMY NATICK LABORATORIES
Natick, Massachusetts 01746
FOREWORD
In the developmenc of operational feeding •yttame to meat •pacialliad military requiremanta, incraaaing aiaphaala ia directed toward minimising weight, volume and preparation for conaumption. In theory, theae featurea can be realized by the compression of dehydrated fooda into compact bare auitable for direct conaumption. Experience has demonstrated, however, that bars of compressed dehydrated food frequently have marginal accept- ability. To assure conaumption by military personnel, bare must have auitable phyaical and organoleptic propartlea, including flavor, after perioda of prolonged atorage. It ia well known that the natural flavor of many dehydrated fooda in attenuated, loat, or adveraely changed during atorage, especially at elevated temperature. Enhancement of flavor of compressed food bare through addition of flavoring suiteriala ia expected to reault in improved acceptability. Thia inveatlgation ia concerned with the behavior of repreaentative typea of flavoring materials in dehydrated food bars under varioua conditiona of atorage. Particular attention ia directed toward measures for preventing deterioration of theae flavora.
The inveatlgation covered by thia report waa performed by the Evana Reaearch and Development Corporation, 250 Eaat 43rd Street, New York 17, New York, under contract number DA19-129-AMC-2113. The Official Inveatlga- tion waa Dr. E. J. Hewitt. Hia collaborators were Mr. T. A. Smith, Mr. R. W. Groncki, Mr. P. L. Roller, Miss M. E. Donworth, Mr. P. Mech, Mr. T. Malone, Dr. P. del Valla, Mr. J. Zolotar and Mr. J. Hllovaky.
The Project Officer for the U. S. Army Natlck Laboratories waa Dr. Maxwell C. Brockaann of the Animal Producta Branch, Food Division. The Alternate Project Officer waa Dr. John Kapsalis of the Food Chemistry Branch, Food Diviaion.
FERDINAND P. MEHRLICH, Ph.D. Director Food Diviaion
APPROVED:
DALE H. SIBLING, Ph.D. Scientific Director
W. W. VAUGHAN Brigadier General, USA Commanding
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I CONTEMTS
Foreword
Litt of tables List of figures Abstreet
Introduction
Bxperlnentel I. Bland compression food bar
A. Screening of msterlels B. Experimental formulas C. Preparation of compressed food bars
II. Methods for flavor stabilization A. Encapsulation of flavors
1. Spray drying with gum arable 2. Dispersion In Carbowax 6000
B. Granulation C. Chemical ■tablllzatlon D. Dispersion of flavors In fat
III. Selection of flavors for storage tests IV. Storage stability tests
A. Preparation of samples for storage tests B. Results of six-month storage tests C. Sensory panel evaluation of flavored food bars D. Discussion of results of six-month shelf life
tests 1. Packaging conditions 2. Stabilization techniques
V. Improvement of bland food bar VI. Flavor enzyme studies
A. Preliminary Investigations B. Pineapple enzyme studies C. Discussion of pineapple enzyme studies
VII. Six-month storage—new flavors A. Sensory panel evaluation of flavored food bars B. Discussion of results of six-month shelf life
tests VIII. Effect of flavor adjuncts on flavor
A. Selection of flavor adjuncts and flavors B. Preparation of samples C. Evaluation»--accelerated tests
IX. Instrumental studies A. Preliminary Investigations B. Investigation of spray-dried lemon flavor
plus adjunct C. Investigation of spray-dried cherry flavor
plus adjunct D. Analysis of food bars E. Comparison of the dry vapor sampling technique
and the solid sampling technique
«j. v vil vlll
I 3 4 4 4 5 5 6 6 6 7 8 9 9
10 10 11 12 12 15
15 15 16 18 18 19 20 21 21 22
22 22 23 23 25 25 26
29
32 34
iV
LIST OF TABLES
I Composition and analyst« of unflavored food bars II Formulations of Cablets
III Hedonlc seals rstlngs of flsvorsd compressed food bars IV Composition of flavors and flavor-to-base ratios V Hedonlc scale rating of compressed food bars containing
reformulated flavors VI Sources of materials used In formulation of flavored
food bars VII Breakdown of total number of tablets produced with
formulas 17 snd 18 VIII Six-month storage evaluation of food bars.
IX Six-month storags evaluation of food bars. X Six-month storage evaluation of food bars.
XI Six-month storsge evaluation of food bars. XII Six-month storage evaluation of food bars. XIII Six-month storage evaluation of food bars. XIV Six-month storage evaluation of food bars. XV Six-nonth storage evaluation of food bars.
Spice XVI Six-month storage evaluation of food bars.
XVII Six-month storage evaluation of food bars. XVIII Six-month storage evaluation of food bars,
spice XIX Six-month storage evaluation of food bars. XX Six-month storage evaluation of food bars.
XXI Six-month storage evaluation of food bars. XXII Composition of formula number 19 XXIII Methods for preparation of enzymes and substrates
blueberry, horseradish, watercress XXIV Pineapple enzyme studies. Actual experimental procedures
for preparation of new enzymes XXV Pineapple enzyme studies. Actual experimental procedure
for preparation of substrate XXVI Composition of new flavors and flavor-to-base ratios XXVII Results of six-month storage tests on flavored food bars
stored In sealed metal cans XXVIII Results of six-month storage tests on flavored food bars
packed In aluminum foil pouches XXIX Frsparatlon of ssrdlne extract XXX Composition of flavor adjuncts and flavor. Curry flavor XXXI Composition of flavor adjuncts and flavor. Lemon flavor
XXXII Composition of flavor adjuncts and flavor. Cherry flavor
Banana Tomato spice Chill Coffee Chicken spice Cherry Vanilla Bacon-tomato
Spaghetti spice Chocolate Beef-tomato
Lemon Curry Rice spice
Pa^e
36 37 41 42
43 44
45
46 47 48 49 50 51 52 53
54 55 56
57 58 59 60 61
63
67
68 69
70
71 72 74 75
I LIST OF TABLES
XXXIII Results of •ix-month storage tests on flavor adjuncts 77 In curry-flavored ford bars packed in pouches
XXXIV Results of six-month storage tests on flavor adjuncts 78 in lemon-flavored food bars packed in pouches
XXXV Results of six-month storage tests on flavor adjuncts 79 in cherry-flavored food bars packed in pouches
XXXVI Results of six-month storage tests on flavor adjuncts 80 in curry-flavored food bars packed in sealed metal cans
XXXVII Results of six-month storage tests on flavor adjuncts 81 in leiron-flavored food bars packed in sealed metal cans
XXXVIII Results of six-month storage tests on flavor adjuncts 82 in cherry-flavored food bars packed in sealed metal cans
rl
imerzit
LIST OP FIGURES
1. Gat chroottogram Illustrating use of the tolid »ampllng technique for epray-drled lemon flavor plus flavor adjunct—10.7 «g. gum arable
2. Gat chroaetograa Illustrating use of the eolld «ampling technique for epray-drled lemon flavor plus flavor adjunct--10.7 mg. non fat dry milk eollde
3. Gas chromatograra llluatratlcg uce of the eolld sampling technique for spray-dried lemon flavor plus flsvor adjunct—11.1 mg. sodium chloride
84
85
vil
ABSTRACT
The object of the project wee to eeteblleh methode to etebllice flevore for flevor retention In high celorlc food here under verylng etorege conditions. In e high moisture food her (18-20% moisture) ell methods tested were Ineffective. In food hers, 5-8X moisture, good eteblllzetlon wee echleved by the cotf«Mn«tlon of Incorpcrstlng BHA In the beee her end encepsuletlng the edded flevor In polyoxyethylene oxide 6,000. These results ere based on sensory penel tests of blend food hers contelnlng 15 different type flevore stabilized by verloue methods end stored under e wide renge of conditions In different package types. Adjuncts such es gum ereblc end non-fat dry milk solids ere effective In retaining flevor ee meesured by gas-liquid chromatogrephy. Techniques were developed for both solid sampling end vepor sampling for extraction of flevor from food hers for gas- liquid Chromatographie analysis.
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FLAVORING MATERIALS FOR HIGH CALORIC FOOD RARS
INTRODUCTION
On September 17, 1962 Evans Research end Development Corporation was suthorlzed by the Quartermaster Food and Container Institute of the Armed Forces* to conduct studies on methods to improve the stability of flavors in high caloric food bars.
In the Statement of Work, the primary objective of the project was stated as follows: "To establish the adequacy of several methods for assuring the retention of added flavors in high caloric food bars efter a nominal wtorage period".
Sumnarlzed briefly below are the specifications of the project:
1. Flavoring materials end auxiliary components ware to conform to requireoents of the Food and Drug Adminis- tration.
2. Flavoring materials were Co be stabilised in any manner deemed advantageous.
3. The flavoring materials were to be natural or artificial. The number to be investigated was to be 12 to 18 types with the following restrictions:
Currently, Food Division, U. S. Army Natick Laboratories.
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a) No more than three common flavors, of which one might be citrus,
b) No more than two spice flavors,
c) One or two systems for flavor development by ac- tion of flavor release enzyme*, JLJL
d) Flavors to be studied should Include chill, sun dried fish, and soya hydrolysate.
4. Flavorings were to be Incorporated Into a bland or near- flavorless compressed food bar conforming to the general composition, as given below:
Percent (dry basis)
Fat 15-25
Protein 15-25
Carbohydrate 50-60
Ash (Incl. NaCl) 2- 4
5. Storage tests were to be run for six months and were to include the following variables:
Temperature - 100oF, 70oF, 40oF
2 cycles per week, max. 40oF, mln. 0oF
Initial Moisture - (a) Maxlmun molstve 27. (b) 5-8%
(c) 16-20%***
Package - (a) MetalIzed polyethylene polyester pouch
(b) Metal can, Oo headspace gas 135-145 mm
Hg.
(c) Metal can, O2 headspace gas below 1 nn Hq.
6. A description of the effect. If any, of the presence of acceptable concentrations of the following adjuncts on representative types of flavors: Sugar (sucrose), sodium chloride at maximum concentrations, food acid at acceptable levels of tartness, protein hydrolysate, flavor enhancers (such as inoslnlc acid derivatives).
U.S.Patent 2,924,521, assigned to Evans Research and Development
Corporation. **Thls was added in Phase II, the second 12-month period of the 24-month program; therefore, the number of flavoring materials to be studied should not be less than 15. ***In Phase II, the tests with "^istare 16-20% was to be elim- inated.
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7.
8.
The phenomenon of flavor masking was to be described In quantitative terms, and recommendations were to be given on how It can be avoided or substantially reduced. Observa- tions were to include relationship of fat, protein, sugar and polymeric carbohydrates to flavor masking.
Bars were to be evaluated for changes In Intensity and quality of flavor after the prescribed storage time by any objective method to correlate with an experienced flavor panel.
This Final Report Includes a consolidation of all experi- mental findings and results, notes, data, and conclusions.
SUMMARY
A method was developed to stabilize flavors for flavor retention in high caloric food bars. The method consists of two steps: (1) the addition of an approved antioxidant (BHA) to the base formula of the food bar, and (2) the encapsulation of the added flavor in poly oxyethylene oxide. This combination was found effec- tive in a wide range of storage conditions in food bars containing 5-8 percent moisture. The system, however, was not effective for a high-moisture-level bar (18-20 percent), and no success was achieved by any other method for stabilization of a high-moisture-level food bar.
No problems can be foreseen in large-scale use and exploitation of the method given in this report for stabilization of flavorings in food bars of average moisture (2-8 percent).
In the informational part of the project, certain flavor adjuncts were studied for their effect in retaining flavor. It was found that gum arable and non-fat dried milk solids were much more effective for flavor retention than sodium chloride. These results were obtained by a sensory panel and gas-liquid chromatography.
Techniques were developed for extraction of flavor from food bars and analysis by gas-liquid chromatography. The extraction and sampling can be accomplished by either a solid-sampling or vapor-sampling method. Further refinements have to be developed and tested before the gas-chromatographic method (consisting of sample preparation, extraction and Instrumental analysis) can be considered reliable for quality control or for systematic studies of changes of flavors in storage.
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EXPERIMENTAL DISCUSSION
I. BLAND COMPRESSION FOOD BAR
A. Screening of Materials
The first step In the flavor stabilization program was directed toward the development of a relatively bland compressed food bar. Specifications called for a general composition of:
Fat 15-257.
Protein 15-25%
Carbohydrate metabollzable 50-60%
Ash (Incl. NaCl) 2- 4%
Numerous possible constituents were screened Individ- ually for their flavor by Informal panel procedures, and only those materials with relatively bland flavors were given fur- ther consideration.
As the Initial trial formulation, a mixture of oatmeal, soy flour (LSP-15) and hydrogenated fat were arbitrarily selected. The Ingredients were combined In the quantities calculated to meet the analytical specifications. Wnen compressed Into a food tablet, this combination had an undesirable soy flavor.
Attempts were made to mask the soy flavor by adding confectionery sugar and non-fat dry milk solids. These Ingred- ients were also selected for their bland flavor and binding properties which would improve the over-all bar quality. Im- provement in physical quality was sufflclert to warrant their inclusion in subsequent formulations, although the predominant soy flavor was still apparent. Since the results Indicated that an alternate protein source was needed to replace the soy flour, a variety of protein sources was Investigated.
The materials screened to replace soy flour were prin- cipally in the casein and toasted soy fraction categories. Of all the materials screened, four were selected as being the most promising: calcium caseinate, high nitrogen casein, toasted soy protein and Promlne-D.
Replacement of oatmeal, rice and barley cereal as car- bohydrate sources was tested by preparing and evaluating other formulations containing oat flour, potato granules and white wheat flour. The results of the tests Indicated that all of these carbohydrate sources are interchangeable with respect to
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blandness. However, all three of these items also produced tab- lets with a slightly pasty texture.
B. Experimental Formulas
Based upon screening work described above, Formulas 15 and 17 were devised (see Table I).
As the panel found the pasty consistency of Formula 15 objectionable, Formula 17 was developed. Formula 17 is a some- what different product, utilizing corn flakes and dry milk sol- ids because Formula 15 could not be modified directly to yield the desired properties. Other ingredients were also tested, such as Edi-Pro or spun soya made by the Ralston Purina Company, but none offered enough advantages to warrant incorporation in the formulation. In Formula 17, the following ingredients were combined and produced a satisfactory bland food bar: non-fat dried milk solids, hydrogenated vegetable shortening, lactose, Proraine-D and ground corn flakes.
Formula 17 was found acceptable in a sensory panel evaluation using hedonic scale ratings. It was rated satisfac- tory for blandness, mouth feel and texture. It was studied, as discussed later, under accelerated shelf-life tests.
Due to the instability of Formula 17 in storage, it was necessary to find a substitute for the hydrogenated veg- etable shortening and, in its place, a solid cotton seed stearin was used. See Formula 18 in Table I. Formula 18 was used exten- sively in shelf-life studies which will be discussed later.
C. Preparation of Compressed Food Bars
The dry ingredients of Formula 17 (non-fat dried milk solids, Promine-D, hydrogenated vegetable shortening, lactose, and ground corn flakes) were weighed out and thoroughly mixed in a Hobart mixer.
The mixture was then granulated using the wet granula- tion process. This process consisted of the following: (1) ad- dition of water to form a plastic mass, (2) extrusion of the plastic mass into thin sheets, (3) drying of the sheets to the desired moisture level (5-8% or 2-37,), and (A) grinding of the sheets to the desired mesh size. The granulation was made into a tablet or food bar by a Stokes DS-3 machine. The pressure and dwell time in the press varied according to the nature of the flavor additive. The average pressure used was 5000 lbs. with a dwell time of two tenths of a second. Tablets were formed 3/16 inch in thickness and 5/8 inch in diameter, at a rate of
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—
1 to 1-1/2 pounds of tablets per minute. A vibrator feeder was used to insure proper filling of the die and a uniform tablet.
Bars from Formula 18 were prepared in the same manner except that 7,000 psi were used for compression.
Formulas 17 and 18 at this point appeared to be suit- able as a bland base for the flavor stability studies. These formulas produced satisfactory bars in which the flavors could be incorporated and at the same time complied with contract specif« icatlons on carbohydrate, protein, fat and ash. Analyses aie found in Table I.
II. METHODS FOR FLAVOR STABILIZATION
The primary concern of this project was the stabiliza- tion of flavor in compressed food bars. Several aspects of com- mercial stabilization were examined in an exploratory way to give some insight into the methods which would be most effective. The techniques used in these preliminary studies and the results are given in the following sections.
A. Encapsulation of Flavors
1. Spray Drying with Gum Arabic
In order to evaluate spray-dried flavors in compressed food bars, several samples of spray-dried citrus oils (207. oil and 80% gum) and vanilla flavor from several of the larger flavor houses were testad.
Approximately 5% of the spray-dried citrus oil compo- sition was added to base mix Formula No. 17. The same was done with pure spray-dried vanilla flavor. The mixes were then com- pressed in a Stokes OS-3 machine.
The resultant tablets were put into aluminum foil polyethylene polyester pouches and heated for one week at 120oF.
At the low moisture level (2 to 3%) and intermediate moisture level (5 to 8%), the spray-dried flavors were judged informally to have held up well. However, when enough moisture was incorporated into the food bar to bring the moisture up to the 20% level, the flavors (and the bars) had deteriorated con-» siderably and lost much strength after several days.
Although the flavors at the low and intermediate mois- ture range appeared to be stable in the food bars, it was found
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that a 5% level of spray-dried flavor could hardly be noticed when the food bar was tasted. The combination of the base mix and the spray-dried oils appears to mask the flavors. Specific- ally, orange flavor had to be increased from 57. to 157. on a weight basis until an informal panel was able to discern the actual fla- vor. At this higher level of flavor, the panel members could identify it immediately as orange but, after the bar completely dissolved in the mouth, the flavor level became overwhelming and distinctly unpleasant. It appears that:
1. Flavors at low levels could be tasted only as an aftertaste and were not perceptible during Chewing.
2. When a flavor was increased to a level where it could be immediately recognized, the flavor became objection- able in character.
3. Panel members complained, particularly with citrus products, that the aroma was pleasant, but an over- whelming peel oil character appeared at the high level during chewing.
A probable explanation for the masking of flavors by the spray-drying of the materials is the presence of the encap- sulating polymer in large quantity in the dried flavor. This masking effect is accentuated by the introduction of the spray- dried flavor into a product which itself has masking properties.
In addition, when high levels of spray-dried flavors were incorporated into the base mix, the general composition as specified in the contract for carbohydrate, protein, fat, ash would be unbalanced.
In view of these findings, a means for encapsulation other than spray-drying was sought where a smaller amount of polymer would be required.
2. Dispersion in Carbowax 6000
One product for encapsulation of flavors which appeared promising was polyethylene glycol (molecular weight 6000-7500), when used in the proportion of 407. polymer to 607. oil.
The polyethylene glycol selected was Carbowax 6000 which is a solid at room temperature. It melts at about 1550F, is highly soluble in water and has no taste or aroma to speak of. In addition, it is nontoxic and is permitted for use in compressed food products. Its main advantages are that it does not notice- ably mask flavors and rapidly releases them when dissolved in
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water. In some cases (orange oils) It has a tendency to round out or reduce the "chemical" sharpness of flavois. The flavor was dispersed In melted polyethylene glycol, cooled, and then ground.
In order to test the glycol-encapsulated flavors against a spray-dried vanilla (80% gum arable, 20% flavor), a pure bour- bon vanilla was dispersed in the polyethylene glycol at the 20% by weight level and ground. The two encapsulated flavors were placed into food bars and the bars tasted (5% flavor was added to the bars).
It was the opinion of an informal panel that the polyethylene glycol-encapsulated sample released more flavor than the spray-dried product and, therefore, bars containing ilavors encapsulated in polyethylene glycol should be placed under six month stability tests.
B. Granulation
One of the methods which can be utilized to stabilize flavors in a compressed food bar is the physical isolation of flavors from the greater portion of mix. This can be accom- plished by taking approximately 10% of the base mix, adding the flavor to this fraction and making a separate flavor granulation or flavor premix. The flavored premix is then combined with the remainder of the unflavored base mix and mechanically blended. After the blending operation, compressed bars can be made where within each bar there is a homogeneous distribution of flavor particles.
In order to determine whether this method of stabili- zation should be investigated fully, an initial test was made with lemon flavored food bars.
Lemon flavor was incorporated into bars of 5-8% mois- ture content by two different methods. In the first set of bars, the flavored premix described above, was added to the base mix. In the second set, the flavor was added to the bars by spraying the flavor itself directly onto the total granulation. Both sets of flavored base mixes were then blended, compressed into bars and stored for one week at 120oF, after which they were examined by an informal sensory panel.
A noticeable loss in flavor was reported in the bars containing the sprayed-on flavor, while the bars containing the lemon,produced by the granulation method,were judged to be con- siderably better than the unstabilized control bar in both fla- vor and aroma. It was then decided to conduct a preliminary six-month storage test on this lemon flavored bar.
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C. Chemical Stabilization
Chemical stabilization has proven to be the most effec- tive means of insuring the quality of flavor during accelerated shelf-life tests and six-month tests at 100oF. These tests were conducted on the flavors themselves. In the earlier experiments, the chemical antioxidants, butylated hydroxyanisole (BHA) and 2, 4,5,-trihydroxybutyrophenone (THBP) were screened for use as stabilizing agents with citrus oils (lemon, orange and lime) and spice oils (parsley and cinnamon).
The untreated oil and oils treated with either BHA (0.1% by weight) or THBP (0.057. by weight) were heated to 500C and air sparged. While being air sparged the samples were fre- quently examined for odor change by an informal panel. When changes were detected the test was stopped. Changes in the odor of the untreated citrus oils were found after 15 hours.
The BHA and THBP treated samples remained stable for 60 hours, indicating an extension of the shelf-life of the citrus oils of 400%. The BHA and THBP treated spice oils were stable more than twice as long as the untreated control samples. How- ever, no conclusions were drawn about the comparative superiority in stabilization effectiveness of the two antioxidants. It was decided to incorporate BHA in the base mix as an over-all chemical stabilizer which would be effective for both the flavor and in- gredients in the bland food bar.
D. Dispersion of Flavors in Fat (Cottonseed Stearines)
One method for addition of flavor to bars is the incor- poration of flavors in the shortening in the base mix. The ad- vantages of this technique are that the flavor is isolated from the high moisture portion of the product and a uniform distribu- tion of the flavor is attained.
In the initial accelerated tests to determine the val- idity of this method, a lemon flavor was incorporated into the melted shortening. The mixture was then cooled, ground, and added to base mix Formula No. 17. Food bars based on this mix- ture were stored for one week at 120oF.
Results indicated that a food bar based on base mix Formula No. 17 and flavored by dispersing the flavor in the fat portion was preferred over a bar with the flavor directly mixed or sprayed on the granulation. Therefore, f.t appeared promising to carry out six month stability tests on bars in which the fla- vor is dispersed in the fat.
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The three methods of stabilization selected for the flavor-stability storage tests were encapsulation with Carbowax 6000, granulation, and dispersion in cottonseed Stearine.
III. SELECTION OF FLAVORS FOR STORAGE TESTS
The selection of flavors was based on preferences given in the booklet on Food' Preferences of Men in the United States Armed Forces . The flavors were derived from natural and synthet- ic sources. In general the natural flavors were used at higher levels than the synthetics in order to obtain a satisfactory fla- vored food bar. Therefore, in some cases it was found necessary to modify ihe composition of the unflavored bar in order to in- corporate the necessary amounts of natural flavor. During the course of the work a number of other observations were made which influenced the selection of the flavors. In some samples, it was noted that the compressed unflavored bar had the tendency to en- mesh or entrap much of the added flavor. In other instances, when the flavor was increased to a satisfactory level, unpleasant off tastes were noted by the panel. It was therefore necessary to discard many of the flavors which were developed earlier in the program.
Finally, as a result of sensory tests, fifteen flavors were indicated as satisfactory for the extensive stabilization and storage studies required by the program. The flavors were: cinnamon-apple, curry, chili, chocolate, coffee, vanilla, spag- hetti-spice, rice spice, beef-tomato, tomato spice, chicken spice, bacon and tomato, banana, lemon, and cherry. Their composition and flavor-to-base ratio are given in Table II and their hedonic scale ratings when incorporated in the food bar are given in Table III. In order to have replacements for the flavors which might not stand up under the stability tests, the reformulation of flavors was continued throughout the project. Some of these reformulations are given in Table IV, and their hedonic scale ratings when used in the food bar are given in Table V. Sources cf materials used in formulations are given in Table VI.
IV. STORAGE STABILITY TESTS
The contract specifications required that storage tests
*Peryam, D.R., Polemis, B.W., Kamen, J.M , Eindhoven, J. and Pilgrim, F.J., QM. Research and Development Command, Quarter- master Food and Container Institute for the Armed Forces, January, 1960.
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be run for 6 months to Include the following variables:
Temperature - 100oF, 70oF, 40oF
Initial Moisture - (a) Maximum moisture 27.
(b) 5-87.
(c) 16-207.
Package - (a) Metalized polyethylene polyester pouch
(b) Metal can, O2 headspace gas 135-145 mm Hg
(c) Metal can, O2 headspace gas below 1 mm Hg.
In the storage work the above variables were followed with the following exceptions:
1. It was not possible to prepare food bars with moisture content 27. or lower. The 27. food bar did not readily undergo the compression in a Stokes DS-3 tabletting machine. The 27. moisture base mix under a pressure of 5,000 psi gave tablets which capped, crumbled readily when handled and were unusually dry to the taste.
2. In preliminary tests it was found also that food bars formulated at 207. moisture deteriorated so quickly (major discoloration, off-flavor development and increase in hardness) that the recommendation was made to drop this variable which was accepted by the Quartermaster Corps.
3. In packaging the specifications require O2 headspace of less than 1 mm Hg. This could not be obtained by flush- ing with air; therefore, N2 was used.
A. Preparation of Samples for Storage Tests
Using Formulas 1 age tests were prepared ace See Table II for formulat flavors were stabilized by dispersion in fat, and enc flavor was blended in with bland food bar and compres discussed earlier all the level.
7 and 18, the flavored food bars for stor- ording to the method outlined on page 5. ions of tablets including flavor. The three methods, namely granulation,
apsulation in Carbowax 6000. The dried the granulated ingredients for the
sed according to the method given. As samples were compounded at 5-87. moisture
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The sample tablets were placed in storage in the follow- ing containers according to specifications:
1. Aluminum-foil polyethylene polyester pouch.
2. Sealed metal can, air-packed, each can containing two per- forated glassine pouches to determine flavor transfer on storage (one pouch contained flavored tablets and the second contained unflavored tablets).
3. Same as No. 2 except nitrogen-flushed to remove oxygen.
Table VII gives the numerical breakdown of the number of samples and tablets placed under storage.
B. Results of Six-Month Storage Tests
1. Bars Prepared from Formula No. 17
As explained in the previous sections, tablets formulated with bland food bar Formula 17 and containing flavor were placed in storage. Although the control bar made from base mix Formula No. 17 appeared stable in the earlier tests at l20oF for 3 months, the same bars were not sufficiently stable to withstand the storage at 100oF for six months. The deterioration of the bars was due to the insta- bility of the hydrogenated vegetable shortening. On this basis a modification in the bland food bar base was made.
The composition of the bland food bar was left unchanged with the exception of the fat. In place of hydrogenated vegetable shortening, solid cottonseed Stearine was substituted in the formula and this fat was stabilized with BHA. The new base mix, the compo- sition of which is given in Table I, was designated as Formula 18.
2. Bars Prepared from Formula 18
The entire line of flavored bars, repeating those which had already been under shelf life studies in bland food bar Formula 17, were remade using base mix No. 18 and placed under study as discussed below.
C. Sensory Panel Evaluation of Flavored Food Bars
Six trained members of the Evans Research Sensory Panel evaluated the bars organoleptlca lly, giving an hedonlc scale rating (hedonic scale - 0 to 9) to the food bars. It should be restated that the score given to the basic, bland bar was 4,1. The results are presented in tabular form in Tables VIII-XXI.
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The following discussion of results of the six-month evaluation of food bars is limited to the 100oF tests; each of the fourteen types of flavored food bars is discussed individually.
1. Banana Bar
After six months of storage, the banana food bars which were stabilized by the granulation method were rated acceptable under all three methods of storage, i.e., nitrogen-packed in tin cans, air-packed in tin cans, and pouch-packed in air. For this natural material, all packaging systems appear to be acceptable. Little or no flavor transfer was organoleptically noted. Hedonic scale ratings are presented in Table VIII.
2. Tomato Spice Bar
Of all the 100oF samples of tomato spice food bars tested, no particular method of preservation of flavor or pack- aging proved to be better than the other. Organoleptically, no flavor transfer was found. The results are recorded in Table IX.
3. Chili Bar
For the chili-flavored food bars, the nitrogen-packed samples were slightly preferred over the regularly can-packed bars. No noticeable flavor transfer was found in the canned samples. Among the three flavor preservation systems used, no difference was found in the canned items except one failure which was found in the pouch-packed bars stabilized by the cottonseed Stearine method. A slight preference, however, exists for the nitrogen-packed bars. The results are presented in Table X.
4. Coffee Bar
For the coffee-flavored bars, only one unacceptable sample was found, that of the pouch-packed sample, stabilized by the granulation method, which developed a strong, bitter taste. A slight preference for the air-packed samples in cans was noted, and a slight flavor transfer was noted in the canned-packed bars. The results of ihe panel evaluations ire presented in Table XI.
5. Chicken Spice Bar
The chicken spice bars were rated acceptable under all conditions. The hedonic scale ratings showed the nitrogen-packed bars to ba preferred slightly over the air-packed can-ied bars and the pouch-packed bars. No significant organoleptic difference between the flavor-preservation systems could be found. Little or no flavor transfer was found in the canned samples. The re- sults are recorded in Table XII.
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_v . Cherry Bar
All methods of flavor preservation were rated unaccept- able with the pouch-packed cherry samples. In contrast, all three methods with the can-packed bars were found acceptable, with a preference for the nitrogen-packed bars; flavor transfer was noted as very slight in the can-packed samples. The hedonic ratings are presented in Table XIII.
7. Bacon and Tomato Spice Bar
The bars which were air-packed in cans were preferred over the nitrogen- and pouch-packed samples. The cottonseed- stearine-stabilized samples in pouch packs definitely failed in achieving acceptable ratings. Vo flavor transfer was found in tne can-packed bars. The results are recorded in Table XIV.
8. Imitation Vanilla Bar
All samples were rated above the 4.1 score of unflavored food bar. The lowest of the scores was found in the pouch-packed samples. Nitrogen-packed bars were slightly preferred over the air-packed canred samples. Only a slight flavor transfer was found in the unflavored samples packed in pouches with the flavored can-packed bars. Results are recorded in Table XV.
9. Spaghetti Spice Bar
No Spaghetti Spice bars were rated below the 4.1 basic food bar score. The nitrogen-packed bars rated highest in accept- ability; the air-packed bars placed second; and the pouch-packed bars third. No flavor transfer was noted in the can-packed sam- ples. In Table XVI are presented the hedonic scale ratings.
10. Chocolate Bar
The nitrogen-packed bars were preferred over the air- packed and pouch-packed bars. No samples scored below the 4.1 basic blend bar score although the pouch-packed samples received the lowest ratings. A slight flavor transfer was noted in the can-packed samples. The ratings are presented in Table XVII.
11. Beef-Tomato Spice Bar
The nitrogen-packed bars were preferred. No difference was noted between the flavor stabilization systems, and generally only a slight flavor transfer was noted vith the can-packed samples. The hedonic scale ratings are given in Table XVIII.
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12. Lemon Bar
No significant preference was given to the bars of any of the three methods of stabilization or of any of the storage methods. All samples were acceptable with a slight fla- vor transfer noted In the can-packed bars. The ratings are pre- sented In Table XIX.
13. Currv Bar
The nitrogen-packed bars were preferred. No sample was rated below 4.1, but the lowest scores were given to pouch- packed bars. No flavor transfer was noted In the food bars packed In cans. The results are recorded In Table XX.
14. Rice Spice Bar
For the Rice Spice bars, the nitrogen-packed samples were preferred over the air-packed. No food bar was rated be- low 4.1, but the lowest scores were given to the pouch-packed bars. Little or no flavor transfer was found between flavored and un- flavored samples packed together In cans. The results are pre- sented In Table XXI.
D. Discussion cf Results of Six-Month Shelf Life Tests
1. Packaging Conditions
The six-month storage tests Indicated that the most protective storage system was that of food bars nitrogen-packed in tin cans. Food bars air-packed in cans were rated second while those packed in pouches were rated third.
Twenty-five samples were rated below 5 cm the hedonic scale; of these twenty-five, twenty-two samples had been pouch- packed while only three had been packed in cans. Two of the twenty-five had been packed in nitrogen, and the remaining twenty- three under regular atmospheric conditions in air.
Based upon the above test results, the preferred method of packaging would be nitrogen-packed in tin cans. It must be pointed out, however, that the majority of pouch-packed samples are acceptable, but that their organoleptic ratings arc not as high.
2. Stabilization Techniques
All the food bars tested were stabilized by the use of
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BHA at 0.1 percent levels of flavor and fat content. Upon ex- amination of the hedonic panel ratings, no significant difference was found in the food bars which were packed in cans using granu- lation, Carbowax, and cottonseed Stearine techniques. This is probably due to the fact that the tin can offers maximum protec- tion to its contents, particularly when nitrogen is used in place of air. Of the twenty-five samples which were rated under 5, only si., were Carbowax while nine were granulation and ten vere cotton- seed stearine. Six of the same twenty-five samples fell below the basic bland food bar rating of 4.1. One was a Carbowax bar, two were granulation bars, and three were cottonseed stearine bars.
Based upon the six-month storage tests, the best method of s abilization of food bars is Carbowax encapsulation in pouches. All three stabilisation methods, however, were found to be accept- able with food bars which had been packed in cans.
The most acceptable method of packaging was found to be the nitrogen-pack in tin cans.
V. IMPROVEMENT OF BLAND FOOD BAR
As explained in the previous section, Formula 18 contain- ing corn flakes was found to be acceptable, but with the following limitations after 6-month storage tests:
1. Corn flakes tend to mask and contribute a characteristic flavor of its own.
2. Corn flakes pick up moisture in storage and tend to accelerate the deterioration of the food bar.
3. The texture quality contributed by the corn flakes after storage is not sufficient to substantiate its use in the food bar.
It was decided, therefore, to develop new formulations which are described below.
New Formulations
The babic bland food bar (Fo-mula 18) which was found not to be completely satisfactory was composed of non-fat dry milk solids (35.27%), cottonseed stearine (8.82%), lactose (27.347.), Promine D (10.93%), and ground corn flakes (17.64%).
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A new ingredient sold under the trade name "Lolac" was found, which proved to be a good carbohydrate-protein source and replacement for corn flakes In Formula 18. Several formula- tions were developed for an Improved bland food bar, as described below:
Formula 19 - Corn flakes was removed, the quantity of Promlne D was lowered, and Lolac (high lactose dry milk solids) was added in amount to compensate for these changes.
The advantage, therefore, of using bars made from Formula 20 would be its blandness which will permit a more precise evaluation of flavors, particularly for enzyme flavor systems. As most enzyme flavors are not particularly pronounced, a more deli- cate medium for experimental testing Is needed. The section on enzyme flavor systems is in a later part of this report.
The compositions and analyses of Formulas 19, 20, 21 for the Bland Food Bar are given in Table XXII.
No storage tests were run with Formula 20 as food bars containing flavor as with Formula 18 because of Insufficient time to repeat the storage series.
*Lolac is sold by Foremost Dairies, Inc., and is a special carbohydrate-protein dry product derived from milk.
Formula 20 - This was a totally new formula consisting of Lolac, cottonseed stearin, and lactose.
Formula 21 - This was also a new formula containing Lolac with the quantity of Promlne D lowered, and cottonseed stearin unchanged.
The new formulations were granulated using water and tabletted using a Carver press at a pressure of 6000 psi with a one-inch die. The food bars made in this manner from the various formulations were hedonically rated as acceptable. The ratings were actually higher than those for Formula 18. Samples of the three formulations were stored at 130-135OF for 10 days at which time their acceptability was again rated. Although it was general- ly considered as borderline. Formula 20 was judged to be the most bland of the three.
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VI. FLAVOR ENZYME STUDIES
The contract specified that one or two systems for flavor development by action of enzymes on a suitable precursor should be studied under U.S. Patent 2,924,521, assigned to Evans Research and Development Corporation. The object of using flavor enzymes in connection with the broad problem of flavor stabiliza- tion was to incorporate an enzyme and substrate in a food bar which will develop a flavor when placed in the mouth. Thus the flavor will be in an inactive form until eaten.
A. Preliminary Investigations
These investigations were designed to explore the possibilities and determine the problems in the applications of flavor enzymes as a flavor precursor in food bars. The two es- sential components of such an enzyme system are the enzyme itself and the substrate.
The preliminary investigations were made with blue- berry, horseradish, and watercress.
1. Extraction of Enzymes--The general procedure was as follows:
The berries, leaves or other materials were pulverized in a Waring blender. The resulting material was ex- tracted with a buffer solution, then centrifuged. To the extract, cold acetone or methanol was added to pre- cipitate the enzyme.
The precipitate was dissolved in water and dried by a freeze-drying operation.
The details of experimentation for the different mate- rials for extraction are given in Table XXIII.
2. Preparation of Substrate--The general procedure W5»s as follows. See also Table XXIII.
The berries, leaves, or other materials were boiled in water to inactivate the enzymes. The mixture was cooled and filtered and preserved by either freezing, oven- drying, or freeze-drying.
3. Incorporation into Food Bar--
The enzymes and substrates were incorporated into the formula for Bland Food Bar Formula #20 as given in Table XXII, and compressed.
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4. Preliminary Evaluation of Enzyme Systems In Food Bars
Blueberry--Enzyme preparations from fresh blue- berry and from dry leaves were tested on fresh blueberry substrate. The amount of flavor enhancement was not sufficient for incorporation in the Bland Food Bar, therefore no further work was done with blueberry. The emphasis was shifted to pineapple which was tested ex- tensively as discussed in a later section of this report.
Horseradish--In the Bland Food Bar, a good horse- radish flavor was obtained, but the appeal of a "horse- radish bar" was not too high. Therefore, the enzyme and substrate was incorporated into a "shrimp-cocktail bar", containing dehydrated shrimp and spices. This product developed an off-flavor very quickly on ag^ng due to deterioration of the shrimp. This enzyme system might be more effective in a meat food bar.
Watercress--Good odor was obtained when 0.010 g of enzyme, 1.5 g substrate and 2 grams of food bar were combined. However, this flavor effect was obtained only at very high concentrations. It is possible that the watercress system would be more effective when com- bined with a lemon-fish flavor, or with a salad flavor.
B. Pineapple Enzyme Studies
The main effort on the study of flavor enzymes for flavor stabilization of food bars was done with pineapple. Pineapple was selected because it is generally available and cheap, it has high flavor acceptance, and it has strong flavor character which is necessary for the food bar.
The object in the pineapple enzyme research program was to isolate and utilize an enzyme or enzymes from the pineapple plant and fruit which would serve to create a pineapple flavor from odorless, tasteless substrates.
1. Procedure for Extraction of Pineapple Enzymes--
The basic approach was to extract various portions of the plant and fruit under different pH conditions and with specific solvents to isolate the protein fraction. The particular enzyme systems readily isolated under the selected extraction procedure were precipitated out of solution by using suitable media such as acetone, ethanol, and ammonium sulfate, usually at reduced temperatures. The precipitated enzyme fraction was
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carefully slurried in water (after additional purifi- cation) and freeze-dried into a fine powdc-i. Alter- nately, the extract could be freeze-dried without pre-treatment. If treated properly, it will not lose its specific functional qualities through heat treat- ment or subsequent denaturization. The details for the preparations of enzymes and substrates for pine- apple are given in Tables XXIV and XXV.
2. Preparation of Food Bars
Pineapple flavored food bars were prepared utilizing Formula No. 20 base mix which was prepared specifically for its blandness, with Substrate E and Enzyme 9 in a 2.5-inch die. See Tables XXIV and XXV. The die, containing 25 grams of base mix No. 20 and 4 percent flavor level, was placed in a Carver Press and 10,000 psi pressure was applied for 20-30 seconds. These compression conditions produced a food bar of the desired qualities which measured 2-1/2 inches in dia- meter and 1/4 inch in thickness.
3. Test for Specificity of Enzymes
To test the specificity of the enzymes, the substrate and enzyme (0.5 grams of Substrate E and 0.05 grams of Enzyme 9) were placed in water. A high level of enzyme and substrate was used against respective blanks to definitely assure that any enzyme activity present would be observed.
C. Discussion of Pineapple Enzyme Studies
A prototype pineapple food bar has been prepared using pineapple Enzyme 9 and Substrate E at the 4 percent flavor level. Smaller pencentages of the flavor level were employed, but the flavor, though present, was too weak to be acceptable. The final enzyme-to-substrate level ratio tested was 1:5.
Future work should be directed towards development of enzyme-substrate systems which would give a more concentrated flavor which is needed for the food bar application. This is not surprising since most natural flavors are weaker than imitations.
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VII. SIX-MONTH STORAGE - NEW FLAVORS
The contract required storage tests in two phases for a total of not less than 15 flavors. Twelve of these flavors were tested in the first phase and four new flavors were tested in the second phase. In this, the latter phase, sun-dried fish and soya hydrolysate were specifically requested. In addition, strawberry and orange were included in this phase because of anticipated poor stability of several of the flavors out of the twelve tested in the first phase. This would guarantee a mini- mum of 15 flavors studied in both phases.
The four new flavors were prepared in Formula 18 as described on page 11. See Table XXVI.
In this storage test the best method for flavor stabilization was used which was encapsulation in Carbowax 6000, and anti-oxident (BHA) in the base mix. The contract allowed for exclusion of those methods which were not satisfactory in the first storage series.
Samples of each flavor of food bar was packed for storage under three sets of conditions: (1) air-packed in tin cans, (2) nitrogen-packed in tin cans, (3) pouch packed in air. In order to determine flavor transfer, flavored bars were can-packed with unflavored bars. Storage was at 100 F, 70 F and 40 F and cycled twice per week.
A considerable number of panels were run in order to determine the hedonic preference and flavor changes for the food bars after storage.
A. Sensory Panel Evaluation of Flavored Food Bars - New Flavors
Six trained members of the Evans Research Sensory Panel evaluated the bars organoleptically, giving hedonic scale rating (hedonic scale - 0 to 9) to the food bars. It should be restated that the score given to the basic bland bar was 4.1. The results are presented In tabular form in Tables XXVII and XXVIH. Each of the different flavored food bars are discussed individually.
1. Sardine Bar (Carbowax Encapsulated)
After six months of storage, the sardine food bars were stabilized by the Carbowax method and were rated acceptable under all three conditions of storage, i.e., nitrogen-packed in tin cans, air-packed in tin cans, and pouch-packed in air. For this natural material, all packaging systems appear to be accept- able. Little or no flavor transfer was organoleptically noted. See Table XXIX for preparation of sardine extract.
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2. Strawberry (Carbowax Encapsulated)
All samples after six months of storage were rated acceptable with ratings about that of the 4.1 score of the \in- flavored food bar. All packing systems appear to be acceptable, with little or no flavor transfer organoleptically noted.
3. Soya (Carbowax Encapsulated)
The soya flavored food bars, after six months of storage, were rated acceptable under all conditions of storage and packaging. No flavor transfer was noted in the food bars packed in cans or pouches.
Aj Orange (Carbowax Encapsulated)
The orange flavored food bars were organoleptically rated as acceptable under all systems of storage and packaging. No flavor transfer was noted by the panel members.
B. Discussion of Results of Six-Month Shelf Life Tests-New Flavors
1. Packaging Conditions
In the six-month storage tests all methods of packaging yielded organoleptically acceptable food bars. Food bars packed in cans were rated first while those packed in pouches were rated second. Little or no difference was organo- leptically noted between those food bars packed in air or nitro- gen.
2. Stabilization
The food bars tested, stabilized by the use of Tenox IV at 0.1 percent levels of flavor and fat content and the Carbowax method, were found to be stable and satisfactory.
VIII. EFFECT OF FLAVOR ADJUNCTS ON FLAVOR
A. Selection of Flavor Adjuncts and Flavors
The contract required a description of the changes, if any, caused by the presence of flavor adjuncts which were specifi- cally given as sugar, sodium chloride, food acid such as citric acid, protein hydrolysate, and flavor enchancers such as inosinic
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acid derivatives. These adjuncts were to be tested at various concentrations consistent with consumer acceptability.
In addition, the contract required that the food bars containing these adjuncts be evaluated for changes in Intensity and quality of flavor after six-month storage. The evaluations were to be done by a trained sensory panel and correlated by an objective method.
The flavor adjuncts were to be tested in representative chemical types of flavor. Curry - representative of a natural spice, Lemon - representative as an essential oil. Cherry - rep- resentative as an artificial type. These were to be incorporated into a bland compressed food bar and Formula 18 was used for this purpose.
The materials selected as adjuncts for testing were non- fat dry milk solids, carboxymethylcellulose, gum arable, dextrin (50 percent soluble - 50 percent Insoluble), salt, citric acid, monosodium glutamate product (95 percent with 5 percent disodium guanylate), disodium guanylate, and lactose.
B. Preparation of Samples
Solution of the above adjuncts and flavors were made and processed in a Bowen Laboratory Spray-Drier. The formulas used, the ratio of flavor to flavor adjuncts, and the spray- drying designation number (the "E" number) are presented in Table XXX (Curry), Table XXXI (Lemon), and Table XXXII (Cherry* Condi- tion and results of spray-drying are presented in Tables XXXIII, XXXIV, and XXXV, Curry, Lemon, and Cherry, respectively. Spray- drying was utilized as a process test as it involved solution and heat processing of flavor and ingredient components. In ad- dition, it is an Important working tool of the flavor and food field.
The above flavors and flavor adjuncts as an homogeneous spray-dried powder were Incorporated into a bland bar (Formula 18) and subjected to six months of storage (under packaging materials and temperature conditions specified previously). Controls were prepared consisting of spray-dried flavor without the adjuncts using gum arable and carboxymethylcellulose.
C. Evaluations - Accelerated Tests
As a preliminary step, accel« were utilized to gain a rapid insight into the changes brought about
As a preliminary step, accelerated storage tests at 120 F
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by aging. Organoleptically, the accelerated tests produced the following results after 4 weeks:
1. Curry - The gum arabic control sample remained acceptable, with little or no change noticeable by the panel. The general re- sult of the addition of flavor adjuncts was that a raisin-wheat aroma, particularly with the protein fractions was developed. In the sample containing citric acid, the curry flavor was modified with the predominant flavor note being citrus in character and the coriander flavor note from the curry being more dominant than in the control sample.
2. Lemon - As was found in the curry samples, the gum arabic control gave very good results as did carboxymethylcellulose control with no noticeable changes in the flavor. The nonfat dry milk solids masked (entrapped)some of the flavor and aroma of lemon samples. In the sample containing dextrin, there was a noticeable loss or entrap- ment of flavor. The sample containing lactose yielded a lemon fla- vor that is sweet and similar to the product known as "Realemon".
3. Cherry - Again, the gum arabic control functioned the best, while the proteins and other ingredients all induced changes in flavor and aroma intensity and character. The changes in the cherry flavor ranged from a modified flowery type cherry note to a protein-cherry flavor.
Prior to instrumental studies to determine the intensity and quality of the changes in flavor, the above samples were evaluated by an experienced flavor panel. The organoleptical ratings are to be found in Tables XXXVI, XXXVII, and XXXVIII. Where the flavor panel found differences, the samples were then subjected to instrumental studies. All of the samples evaluated were found to be acceptable, with hedonic rating above that of the bland unflavored food bar.
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IX. INSTRUMENTAL STUDIES
The contract specified that food bars contain- ing flavors and flavor adjuncts were to be evaluated by an objective method to correlate with sensory panel tests. Gas-l'-uid chromatography was used in these objective studies.
The purpose in testing the combinations of flavors and flavor adjuncts was to determine what influence or effect flavor adjuncts had on flavor after storage.
A. Preliminary Investigations
Gas chromatography, employing solid sampling, dry vapor sampling, and wet vapor sampling techniques were used to investigate the effects of three adjuncts (gum arable, non-fat dry milk solids and sodium chloride) on spray-dried cherry and/or lemon flavors. Although this was only a preliminary investigation, the information ob- tained demonstrated the unique value of gas chromatography in such studies.
Based on these preliminary studies, it was found that it was not possible to operate the instrument routine- ly under experimental conditions which reproducibly de- tected the flavoring materials in 10 milligram samples of food bar. Possibly the amount of flavoring material ini- tially applied was lost during sample preparation, or the component materials of the food bar actually retain most of the flavoring materials. In either case, even more sensi- tive detector conditions were required, and more elaborate extraction techniques must be used to recover the flavor possibly entrapped by a single or by several bar components.
The effort to develop the solid sampling technique for routine use was due to the inherent advantages of this technique which makes it especially promising for the analy- sis of volatile flavor components in food bars. A very small amount of material, about 5 grams for each food Sar sample, was available for analysis. Therefore, replicate analyses must be obtained by using aliquots of this 5 grams of material. The nature of the chemical flavors used, the use of adjuncts, the use of a matrix composed of complex interferrlng substances and relatively low concentration of any one component of the complex chemical flavor, all indi- cate that the sample will require preliminary heating to release the volatile flavor components from the bulk of the
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sample. The solid sampling technique uses a 10 milligram aliquot of the original sr.mple sealed in a glass capsule. This glass capsule can be heated in the injection port of the gas Chromatograph at a selected temperature for a se- lected Lime. Then, the glass capsule is crushed, releas- ing the volatile components of the sample for analysis by gas chromatography.
B. Invest nation of Spray-Dried Lemon Flavor Plus Adjunct
1. Effects of Adjuncts on Lemon Flavor
The following spray-dried lemon flavor plus ad- junct samples were examined for lemon flavor by gas chroma- tography:
Number
E 6813 E 6815 E 681t;
Flavor
Lemon (40%) Lemon (A47o) Lemon (42%)
Adjunct
Gum Arabic Non-Fat Dry Milk Solids Sodium Chloride
The percentages refer to the hypothetical lemon flavor content. They are not a measure of the actual lemon flavor content of the final, spray-dried flavor plus adjunct. At a later stage of this report it will be shown that these experiments have suggested a gas Chromatographie approach whereby the actual lemon flavor content could be determined.
In this experiment gas chromatography was used to determine the approximate amount of lemon flavor that could be detected by exomining aliquots of each of the above samples. This will not determine the total lemon flavor content of the samples. Due to sorption, each of these ad- juncts retains a greater or lesser amount of lemon flavor on its surface. To the extent that the adjunct makes the lemon flavor unavailable for detection, it has masked the lemon flavor. The total lemon flavor content of each spray- dried lemon flavor plus adjunct sample was equal to the lemon flavor content as determined in this experiment, minus the lemon flavor content made unavailable for detection due to retention by the adjunct. Indirectly, the ability of adjuncts to reduce lemon flavor was measured.
Indication that adjuncts were reducing the amount of lemon flavor actually available for detection would be
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presumptive evidence that materials in the base mix Formula No. 18 might be further reducing the lemon flavor actually available for detection. Still more losses or changes due to storage might further reduce the amount of lemon flavor available for detection to a concentra- tion too small for detection by this very sensitive method. Analysis of these spray-dried samples of lemon flavor plus adjunct simplified the problem since the lemon flavor content is higher at this stage than in the final food bar, and there are no complications due to any interactions with components of base mix Formula No.18. Demonstration of this point would explain the failure of the solid sampling and dry vapor sampling techniques to detect lemon flavor in food bars, although calculations based on available data indicated that theoretically a 10 milligram sample did contain sufficient lemon flavor for detection.
For the reasons cited above, three samples of lemon flavor plus adjunct were analyzed by the solid sampling technique, although sufficient sample was avail- able to permit us0 of a vapor sampling technique. A des- cription of the procedure followed in the solid sampling technique will be included in a later section of this report.
2. Results and Discussion - Lemon Flavor Plus Adjunct
Lemon flavor was detected in approximately 11 milligram aliquots of all three samples. The three major components of lemon flavor were present at such concentra- tions that it was necessary to operate the instrument at less sensitive conditions in order to detect these compon- ents as on-scale peaks. Reproducibility was greater than the usual + 5 - 10% expected from liquid or vapor sampling techniques. Differences were demonstrated in the relative amounts of lemon flavor detected for each of the three spray-dried lemon flavor plus adjunct samples.
The resulfs obtained indicated that the past failures to detect flavor in food bars was due to the availability of much less than the theoretically expected amount of lemon flavor for detection. In part the dis- crepancy was caused by some adjuncts sorbing much less flavor than others. The exact losses of flavor due to re- tention of part of the lemon flavor by other adjuncts under these conditions of gas chromatography still remains unknown. Losses of flavor due to reaction through physical
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and chemical means can only be inferred at this time. In a later section of this report such losses will be demon- strated. It should be noted that even with spray-dried powders there still was not completely satisfactory homo- genlty of the sample, leading to poor reproducibility. As mentioned before, the differences between the samples were so large, the poor reproducibility did not destroy the re- liability of the results in this case.
When interpreting the chromatograms (Figures 1, •i 3) it was evident that three peaks contained the bulk of the lemon flavor detected. Use of one or all three of these peaks furnished a means of comparing the amount of lemon flavor in the three samples. These peaks are designated by the letters X, Y and Z. The heights of peaks X, Y and 7 were measured in inches, on a given chroma- tograra. The peak height in inches was multiplied by the Range Product setting of the instrument for that peak. The resulting number is the peak height in inches, if it were possible to operate the instrument at its most sensitive setting namely, a range setting of one and an attenuation setting of one. This fortunate condition was never realized in practice. At best, a range product setting of 16 was used, and sometimes 32 or 64 had to suffice. This idealiza- tion device is one arbitrary way to standardize and simplify the presentation of data from many chromatograms obtained at various levels of instrumental sensitivity, in order to obtain useful information and generalizations.
The following data was obtained by this method:
Sample Flavor Adjunct Idealized Peak Height in Inches at Range Product ■ 1
X Y Z E 6813 Lemon (40%) Gum Arabic 576 3,840 580 E 6815 Lemon (44%) NFDMS 3,040 21,120 3,520 E 6818 Lemon (42%) Sodium 80 658 106
Chloride
In each of these samples, the peaks X, Y and Z had essentially the same retention times as corresponding peaks detected in liquid lemon flavor. As further substan- tiation of the same identity of each of the peaks in the three samples, the peaks X, Y and Z exist in all three samples in the same relative proportions. Peak Y was much larger Cabout 7 times) than Z and X. Peak Z was only slight- ly larger than X and for practical purposes these two peaks can be considered as essentially equal.
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C. Investigation of Spray-Dried Cherry Flavor Plus Adjunct
The following spray-dried cherry flavor plus ad- junct samples were examined for cherry flavor by gas chroma- tography:
Sample No. Flavor Adjunct
E 6854 Cherry Gum Arabic E 6855 Cherry Non-Fat Dry Milk Solids E 6858 Cherry Sodium Chloride
In this experiment the effect of adjuncts on cherry flavor was determined by two sampling techniques which were intended to be analogous to smelling and tast- ing the samples. In the dry vapor sampling technique, a one-gram aliquot of a given sample was heated for 10 minutes at 90OC in a 10 cc Erlenmeyer flask sealed by an odorless rubbrr serum cap and 5 cc of headspace vapors were removed and analyzed by gas chromatography. In the wet vapor sampling
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Dividing the amounts of X, Y and Z detected in sample E 6818 into the corresponding values fcr these peaks in samples E 6813 and E 6815, presents the data in a more meaningful way.
Idealized Peak Height Sample Flavor Adjunct Relative to Sample E 6818
X Y Z E 6813 Lemon (40%) Gum Arabic 7.2 5.9 5.5 E 6815 Lemon (447») NFDMS 38.0 32.2 33.3 E 6818 Lemon (427.) Sodium 1.0 1.0 1.0
Chloride
When non-fat dried milk solids (NFDMS) was the adjunct, it released approximately 32 times as much lemon flavor during analysis as did sodium chloride as the adjunct. The gum arable released approximately 6 times as much lemon flavor as the sodium chloride adjunct. By an extension of the above procedure, the NFDMS released approximately 6 times as much lemon flavor as the gum arable adjunct.
This experiment clearly demonstrated that under these conditions the amount of lemon flavor detected by gas chromatography in spray-dried lemon flavor plus adjunct de- creased with the adjuncts as follows: non-fat dried milk solids, gum arable, and sodium chloride. Figures 1, 2, 3 are copies of representative chromatograms obtained in this experiment.
technique, 5 cc of boiling distilled water was added to another gram aliquot of the same sample which was heated for 10 minutes at 90 C in a 10-cc Erlenmeyer flask sealed by an odorless rubber serum cap and 5 cc of heapspace vapors were removed and analyzed by gas chromatography.
The dry vapor sample would detect the cherry flavor released from the spray-dried cherry flavor plus ad- junct by the heating Gtep, The wet vapor sample would detect the cherry flavor released from the spray-dried cherry flavor plus adjunct by solution in the water (an extraction) as well as by the heating step. This procedure was felt to simulate in a very crude way the role of saliva in the mouth releasing flavor from the adjunct. At some future time it was planned to examine the water itself for cherry flavor by gas chroma- tography.
Results and Discussion - Cherry Flavor Plus Adjunct
The benzaldehyde peak was detected in all samples at concentrations necessitating the use of less than the usual sensitive conditions. Significant differences were detected between all three samples. Important differences were detected between the same sample by dry and wet vapor sampling
Sample Idealized Peak Height in No. Flavor Adjunct Inches at Range Product ■ 1
Dry Wet E 6854 Cherry Gum Arabic 1,719 5,549 E 6855 Cherry NFDMS 6,617 1,719 E 6858 Cherry Sodium Chloride 277 1,455
Using the dry vapor sampling technique most cherry flavor was detected for the NFDMS adjunct, gum arable was intermediate and sodium chloride was lowest. Using the wet vapor sampling technique the previous sequence was changed, i.e., most cherry flavor was detected for the gum arable adjunct, NFDMS was intermediate but not very signi- ficantly greater than sodium chloride. Although more cherry flavor was detected by the wet vapor sampling technique for gum arable and sodium chloride adjuncts, the reverse was true for the NFDMS adjunct.
The above data was converted to make it rela- tive to cherry flavor detected in the sodium chloride adjunct sample.
- 30 -
Idealized Peak Height SamPle at Range Product - 1 - No. Flavor Adjunct Relative to No. 6858
Dry Wet
E6854 Cherry Gum Arabic 6.1 3.8 E6855 Cherry NFDMS 23.9 1.2 E6858 Cherry Sodium Chloride 1.0 1.0
By the dry vapor sampling technique, NFDMS ad- junct released approximately twenty-four times as much cherry flavor as did sodium chloride adjunct and approxi- mately four times as much cherry flavor as did gum arable adjunct. Gum arable adjunct released approximately six times as much cherry ilavor as did sodium chloride adjunct
{as determined by the dry vapor sampling technique. By the wet vapor sampling technique gum arable adjunct released approximately four times as much cherry flavor as NFDMS ad- junct and sodium chloride adjunct, the latter two being approximately equal in effect.
In the case of cherry flavor the dry vapor sampling technique demonstrated that NFDMS adjunct was most efficient in releasing cherry flavor, gum arable adjunct was significantly less efficient and sodium chloride was least efficient.
This data agrees well with the conclusions reached earlier for lemon flavor with these adjuncts. In effect both experiments measured the ability of mild heat- ing to desorb flavors from adjuncts. An additional unknown amount of cherry flavor still remained sorbed to each of the adjuncts in differing amounts.
The wet vapor sampling technique was used to de- termine the extent to which the water would replace the cherry flavor from the active sites of the adjuncts. It was assumed that the amount of flavor detected in all cases should be greater than for corresponding samples analyzed by the dry technique. The results obtained indicated this was true for gum arable adjunct, which now released the most cherry flavor. It was also true for the sodium chloride adjunct which by the wet technique released almost as much cherry flavor as the NFDMS under the same wet technique.
Comparing data for the same adjunct when ex- amined by the dry and wet techniques, the wet technique accomplished an increase of approximately 5 times for the sodium chlcrlde adjunct, approximately 3 times for the gum
- 31 -
arable adjunct, and a decrease of almost four times for the NFDMS adjunct. Solution of the sodium chloride In water with release of the cherry flavor probably resulted In the large Increase for this adjunct. Gum arable Is used for spray-drying by the Industry because it does readily release flavor In solution. In the case of the NFDMS, It Is possible that the resulting solution was more effective in absorbing the cherry flavor than was the dry NFDMS.
The data suggest a complementary relationship exists between the data obtained by the dry and wet techniques. The dry NFDMS released most flavor and the wet gum arable re- leased most flavor. The numerical values obtained are very similar and probably not too significantly different. The cherry flavor released by wet NFDMS and dry gum arable had identical numerical values by coincidence. Both wet and dry, the sodium chloride values were always lowest. It is possible that the NFDMS and gum arable adjuncts actually sorbed essen- tially the same amount of cherry flavor during the spray-drying treatment. The NFDMS released most of the sorbed flavor on dry heating. The gum arable released most of the sorbed flavor on solution. With this information as a starting point, it should be possible to utilize both techniques to develop a method to permit measurement of the total amount of flavor initially present on the adjunct after spray-drying or any other charg- ing treatment.
D. Analysis of Food Bars
EyalUations mrde by the sensory panel detected flavor differences between food bars Incorporating Lactose- Lemon, Mertase 5-Lemon and Guanylate-Lemon which had been stored at 40 F as control samples, and identical food bars which had been stored at 100 F. Therefore, these lemon flavored samples were selected for analysis by GLC to de- termine if a correlation between sensory panel and instru- mental results could be demonstrated. Cherry-flavored food bars would have been preferred for this comparison due to the comparative ease and speed of analyzing for the major flavor component, benzaldehyde, by gas chromatography as opposed to the difficulty and two hours required to re- solve the many components of the complex lemon flavor. Since none of the cherry-flavored food bars demonstrated any de- tectable flavor differences between those stored at 40 F and the others stored at 100OF, as determined by the sensory panel, it Was necessary to use the lemon flavored food bars.
- 32 -
1. Procedure
For each of the six lemon flavored food bar samples, all of the food bars remaining from the panel tests were ground to the finest powder obtainable on the Wiley Mill. It was reported earlier that such a finely milled powder is essential to obtaining a more homogeneous sample, which in turn is critically important when using the solid sample technique in order to obtain more repro- ducible and hence reliable data. Approximately five grams of powder were obtained for each of the six food bar samples to be examined,viz* Lactose-Lemon 40 F, Lactose-Lemon 100OF, Mertase 5-Lemon 40 F, Mertase 5-Lemon 100OF, Guanylate- Lemon 40 F, and Guanylate-Lemon 100 F. A five gram total sample was insufficient material to permit use of the vapor sampling (dry or wet) technique with enough replicate samples. Therefore, the only recourse was to use the more sophisticated and far less convenient solid sampling tech- nique, since this technique required aliquots of only 10-20 milligrams per analysis.
A tared capillary tube sealed at one end is filled to the appropriate level with the ground powder. The tube is weighed and sealed. The capillary is placed in the solid sampler device, which is positioned in the in- jection port of the gas Chromatograph. After heating for the selected time at the selected temperature, the plunger of the solid sampler is depressed, crushing the glass tube and releasing the volatiles into the injection port of the gas Chromatograph for analysis.
2. Results and Discussion
Peaks were detected for each of the six samples. Much more material was usually detected in a few of the samples, such as Lactose-Lemon 40 and Mertose 5-Lemon 40 , than in the other samples. Good reproducibility was not achieved. Replicate adiquots of the same sample gave peaks ranging in size from one inch to several inches. The bulk of the material detected appeared to be higher boiling com- pounds not detected in the original lemon flavor itself. These peaks in many cases were far larger than the peaks corresponding to the original liquid lemon flavor.
Reproducibility probably was not acMeved for aliquots of the same powdered sample due mostly to a lack
- 33 -
of sufficient homogeneity in the sample. As was noted pre- viously, in earlier work better reproducibllity was achieved when the food bars were powdered to the finest extent poss- ible on the Wiley Mill as opposed to simple pulverizing by means of a pestle and mortar. Apparently treatment in the Wiley Mill and subsequent stirring of the fine powder to produce an evenly colored product still did not mix the sample sufficiently well so that aliquots taken at random were exactly equivalent in composition. A further step must be added to the sample preparation procedure in crder to achieve the requisite homogeneity. Perhaps mixing on the roller mill for a sufficient time might achieve satisfactory homogeneity without any appreciable loss or change of the volatile flavor components. It is not likely that instrumen- tal sensitivity fluctuated to such an extent during a day or even several days.
The compounds having much greater retention times than those for the major constituents of the lemon flavor could be due to a number of factors. These compounds may be due to components of base mix Formula No. 18 itself or of the adjunct. The peaks detected may represent such components either unchanged or changed by storage at 40 F and 100 F, respectively. If these peaks are due to lemon flavor, they would be the result of changes in the original flavor due
o o to storage at 40 F and 100 F, since they are not the major components detected in the initial liquid lemon flavor.
The difficulty with reproducibllity and lack of sufficient time precluded further work on this phase of the proj ct. Assuming the reproducibllity problem can be solved, the technique shows promise in determining the effects on the initial added flavor due to adjunct, base mix and storage conditions.
Developing a solid sampler capable of accommo- dating 100 milligram samples would permit operation of the instrur^nt at less sensitive conditions thus reducing in- terference from extraneous sources and providing better in- strumental stability.
E. Comparison of the Dry Vapor Sampling Technique and the Solid Sampling Technique
The procedure described for the dry vapor sampling of spray dried cherry flavor plus adjunct was applied to one
- 34 -
set of spray dried lemon flavor plus adjuncts. These samples were examined by the solid sampling technique as reported on Page 25. The data from both techniques are here compared to determine the more sensitive technique.
Idealized Peak Height in Inches at Range Product ■ 1
Solid Sampling Dry Vapor Sampling Adjunct (10 milligrams) (1 gram)
X Y Z X Y Z
Gum Arabic 576 3,840 580 11,90A 39,680 13,696 NFDMS 3,040 21,120 3,520 75,528 272,640 65,920 SOruiira 4A 80 638 106 1,080 5,376 992 Chloride '
Generally speaking, especially for the Y peaks of the lemon flavor, the dry vapor sampling technique yielded values that were approximately ten times those of the solid sampling technique. The solid sample was 1/100 the size of the sample for the dry vapor technique. This cancels the ten-fold advantage in peak size detected by the dry vapor sampling technique. Further, it indicates that the solid sampling technique is approximately ten times as sensitive as the dry vapor sampling technique.
- 35 -
TUE I
COMPOSITION AND ANALYSIS OF UNFLAVORED FOOD BARS
Formula No. 15
Composition: Rice Cereal 46.107. Hydrogenated Vegetable Shortening 7.70% Nonfat Dry Milk Solids 15.407. Confectionery Sugar 15.407. Promine u (clarified) 15.407.
Analysis*: Carbohydrate 57.007. Protein 25.007. Fat 15.007. Ash 3.007.
*On a dry basis
Formula No. 17
Composition: Nonfat dry milk solids 35.277. Hydrogenated vegetable shortening 8.827. Lactose 27.347. Prominc D (clarified) 10.937. Ground corn flakes 17.647.
Analysis*: Carbohydrate 59.747. Protein 26.227. Fat 10.067. Ash 3.987.
*On a dry basis
Formula No. 18
Composition: Nonfat dry r^ilk solids 35.277. Cottonseed Stearine* 8.82/. Lactose 27.347. Promine D (clarified) 10.937. Ground Corn flakes 17.647,
Analysis**: Carbohydrate ^'^J0
Protein 26.227. Fat: 10.067. Ash 3.987.
*Stabillzed with Tenox IV **On a dry basis
" 36 "
TABLE II
FORMULATIONS OF TABLETS - FOR STORAGE TESTS
Cinnamon-Apple
The following changes were made In base mix 17: Cft/Grms
Nonfat dry milk solids (20)* 35.27 Hydrogenated vegetable shortening (18) 8.82 Apple flour (23) 27.3A Promine-D (clarified) 10.93 Ground corn flakes (9) 7.64 Sugar, confectionery (1) 10.00 Cinnamon (11) 8.00
Chocolate
Bise mix 200 Cocoa - 227, fat (10) 15 Vanilla Nodes - spray dried (11) 15 Sugar, confectionery (1) 10
Spaghetti Spice
Base mix 200 Spaghetti spice 5
composed of:
Tomato powder (10) ^0.0 Onion (8a) 11.3 Paprika (6) 4.0 Garlic (3a) 3.1 Basil (8a) 1.0 Monosodium glutamate (17) 0.8 Pepper (8a) 0.6 Celery (8a) 0.5 Oregano (11) 0.5 Rosemary (8a) 0.1
*Figure8 in parentheses correspond to suppliers listed in Table VI
- 37 -
TABLE II (Continued)
Rice Spice
Base mix Rice spice
composed of:
Onion (8a) Salt QM Curry* (8a) Celery (8a) Chicken fat (14) Thyme (8a) Parsley (8a) Bay (8a)
Beef-Tomato
Base mix Freeze dried beef (17) Tomato powder (10) Monosodlum glutamate (17) Protein hydrolysate (20) Garlic powder (8a) Onion salt (8a) Mustard (5)
Curry
Base mix Curry
composed of:
Coriander (8b) Cumin (13.) Fenugreek (15) Black pepper (8a) Cardamon (8b) Mace (11) Allspice (11) Cinnamon (8b) Mustard (5) Paprika (6) Ginger (8b) Celery (8a) Orange oil (7,19,21) Cayenne (8a)
Wt/G rms
200 5
21. 00 4. 35 2. 45 2. 00 2. 00 1. 35 0. 03 0. 01
100 30 10
-«
2 1 1 0. 5
200 3
•
250 100 100 60 50 40 35 35 20 15 10 5 5 0. 5
*Blend made according to Federal Specifications EE-P-600.
- 38
*
TABLE II (Continued)
Tomato Spice
Base mix Tomato spice
composed of:
Dehydrated tutnato (10) Onion (8a) Garlic (8a) Paprika (6) Basil (8a) Monosodium glutamate (17) Oregano (11) Pepper (8a) Celery (8a)
Chicken Spice 2
Banana
Chili
Base mix Freeze-dried chicken (22) Carrot powder (4) Celery (11) Chicken extract powuer (3) Disodium inosinate (12) Monosodium glutamate (17) Protein hydrolysate (20) Spice mix for chicken* (8a) Onion salt (8a) Thyme (11)
Base mix Banana crystals (16)
Base mix Chili spice
composed of:
Chili pepper (6) Dehydrated tomato (10) Paprika (6) Cumin (11) Coriander (8a) Red pepper (6) Oregano (11) Ceicry (8a)
Wt/Grms
200 5
43. 8 16. 1 4. 9 4. 5 1 3 0. 9 0. 5 0. 5 0. 4
150 30 3 2
0. 5 0. 5
90 10
200 8
11. 20 6. 44 4. 48 1. 68 1. 40 1. ,40 0. ,84 0. .56
«Blend made according to Federal Specifications EE-P-600.
- 39
Lemon
Coffee
Vanilla
i
TABLE II (Continued)
Base mix Lemon flavor
composed of:
Exchange lemon oil (24) Lemon oil 5x (19) Veltol - 27. in benzyl alcohol (17) Terpeneless lemon oil (8c)
Base mix Sugar (1) Instant coffee
Base mix Spray dried vanilla nodes (13)
Candy Cherry
Base mix Cherry flavor (101 benzyl alcohol)
Cherry Flavor Formula
A. Ethyl Oenanthate Candy base mix Tolyl aldehyde Benzaldehyde N.F.
B. Candy base mix Eugenol Anisyl acetate Anisyl aldehyde Amyl cinnamic aldehyde Absolute Jasmin Vanillin Ethyl tolylglycidate
Wt/Grms
200 0.75
100 50 10 5
200 10 6
200 10
200 2
1.2 8.5 12.5 55.8
2.0 9.0 9.0 15.0 1.0
24.0 25.0
Bacon and Tomato
Base mix Dehydrated tomato powder Hickory smoked yeast Bacon fat (stabilized)
100 1.0 0.5 1.0
- 40 -
TABLE III
HEDONIC SCALE RATINGS OF FLAVORED
COMPRESSED FOOD BARS
Flavor Individual Ratings
Average A B c D 1 F 0 H I J
Cinnamon Apple 8 9 8 8 9 8 7 9 - - 8.3 Chocclate 6 8 6 6 7 8 7 7 ■ - 7.1 Spaghetti Spice 8 7 8 8 8 2 7 7 8 - 7.0
Rice Spice 7 7 8 8 7 6 6 6 - - 6.9
Beef-Tomato 7 6 7 8 6 6 6 7 - - 6.6
Curry 7 7 8 l| 7 U 7 8 7 - 6.6
Tomato Spice 5 5 5 6 6 7 8 7 - - 6.1
Chicken Spice 2 6 6 5 7 6 7 $ 6 - - 6.0
Banana 6 6 7 7 3 6 6 6 6 - 5.9
Chili 5 7 1 5 9 7 7 6 - - 5.9
Lemon 5 6 5 7 7 U 7 6 - - 5.9
Coffee 6 5 8 6 7 7 U 2 7 5.8
Vanilla 5 7 6 3 8 7 U 3 5 5.3
Chicken Spice 1
6 5 h ? 1 5 2 7 - U.o
Bland Food Bar 17
5 3 6 3 l| 3 7 2 3 5 U.l
- 41 -
TABLE IV
COMPOSITION OF FLAVORS AND FLAVOR-TO-BASE RATIOS
FOR REFORMULATED FLAVORS
Chocolate
Base mix Cocoa (22% fat) Spray-dried vanilla Sugar, confectionery Saccharin sodium Imitation vanilla
OrlRlnal Modified Formulation Fo rmulatlon
200* 200* 15 5 15 0 10 0 0 0.02 0 2
Coffee
Base mix Sugar Instant coffee Imitation vanilla Saccharin sodium
Chicken Spice
Base mix Freeze-drled chicken Carrot powder Celery dehydrated Chicken extract powder Dlsodlum Inoslnate Monosodlum glutamate Protein hydrolysate Spice mix for chicken Onion salt Thyme Onion dehydrated Chicken fat Dlsodlum Inoslnate and dlsodlum guanylate
200 200 10 0 6 3 0 0.1 0 0.02
150 100 30 0 3 0 2 0
1 0 0 0.2 0.5
0.5 0 0.5 0 0 0.3 0 2
0.1
rParts by weight. - 42 -
TABLE V
HEDONIC SCALE RATING OF
COMPRESSED FOOD BARS CONTAINING
REFORMULATED FLAVORS
Flavor i i [ndlvldual Ratings 1 Average! A B C D E F G H I J
1 Coffee k 6 7 8 6 3 6 It - - 5,5 1
Chocolate 5 6 6 5 6 7 6 6 - - 5.9 1 Vanilla 6 6 6 7 5 1» 6 5 - - 5.6
Bacon fc Tomato 6 5 7 8 6 7 8 5 - - 6.5 |
Beef Tomato 5 7 6 5 7 7 5 6 8 6 6Ji |
Chicken Spice 7 6 6 5 6 5 7 7 7 5 6.1 j
Cherry 6 5 6 6 7 5 7 I 6 6 7 6.1 j
Bland Food Bar 5 31 6 3 Ü 3 7 2 3 5 lui |
43 -
TABLE VI
SOURCES OF MATERIALS USED IN FORMULATION OF FLAVORED FOOD BARS
1. American Sugar Refining Company, New York
2. Armour & Company, Chicago
3. Beatrice Foods, Inc., Chicago
4. California Vegetable Concentrates, Modesto, Calif.
5. Durkee Famous Foods, Cleveland, Ohio
6. Gentry, Glendale, Calif.
7. Haarmann & Reimer Corp., Union, N.J.
8. Chas. L. Huisking & Co., Inc., Lyndhurst, N.J.
a) Saromex S b) Saromex D c) Essential Oils
9. Kellogg Company, Battle Creek, Mich.
10. Milton Klein Company, Inc., Jamaica, N.Y.
11. McCormick & Co., Inc., Baltimore, Md.
12. Merck & Co., Inc., Rahway, N.J.
13. Norda, New York
14. Ocoma Foods Co., New York
15. S. B. Penick & Co., New York
16. Plant Industries, Inc., Plant City, Fla.
17. Chas. Pfizer & Co., New York
18. Procter & Gamble Co., Cincinnati, Ohio
19. Pierre Robertet, Inc., Naw York
20. Sheffield Chemical, Norwich, N.Y.
21. Taconic Natural Oils Co., Inc., New York
22. United Fruit Co., New York
23. Vacu-Dry, Oakland, Calif.
24. Warner-Jenkinson Mfg. Co., St. Louis, Mo.
44
TABLE VII
BREAKDOWN OF TOTAL NUMBER OF TABLETS PRODUCED
WITH FORMULAS 17 AND 18
Method of Stabilization Storage Conditions
350C 70oF 10üoF Cycling Metalized Polyethylene
I Polyester Pouches: 180 Pouches Containing 5,400 Tablets
Granulation 420 420 420 4?0
j Dispersion in Fat 420 420 420 420
\ Encapsulation 420 420 420 420 it-k
j Control 90 90 90 90
Tablet Subtotal 1350 1350 1350 1350
Cans - Air Packed: - ' ' -■ ■ ■■■- ■ ■ - ■ -"v-^'f
168 Cans Containing 10,080 Tablets 1
| Granulation 420 420 420 420
j Dispersion in F.t 420 420 420 420
Encapsulation 420 420 420 420
Control 1260 1260 1260 1260
Tablet Subtotal 2520 2520 2520 2520
Cans - Nitrogen Packed: •kick
168 Cans Containing 10,080 Tablets
| Granulation 420 420 420 420
| Dispersion in Fat 420 420 420 420
| Encapsulation 420 420 420 420
1 Control** 1260 1260 1260 1260
Tablet Subtotal 2520 2520 2520 2520
GRAND TOTAL 25,560 Pouches Containing Flavored Tablets
^Cycling between 0° and 350F. ^^Unsealed metalized polyethylene polyester pouches.
Each can contained two glassine pouches each containing 30 tablets.
- 45 -
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COMPOSITION OF FORMULA NUMBER 19
Composition;
Analysis**:
Lolac Cottonseed Stearine* Lactose Promine D Non-Fat Dry Milk Solids
Protein Fat Carbohydrate
14 15 23
3 35
24.3 17.0 50.4
COMPOSITION OF FORMULA NUMBER 20
Composition;
Analysis**;
Lolac Cottonseed Stearine* Lactose
Protein Fat Carbohydrate
50 15 35
25 15 50
COMPOSITION OF FORMULA NUMBER 21
Composition; Lolac Cottonseed Stearine* Lactose Promine D
30 15 45 4
Analysis**; Protein Fat Carbohydrate
19.7 16.0 57.4
* Stabilized with Tenox IV ** On a dry basis
- 60 -
I
TABLE XXI11
METHODS FOR PREPARATION OF ENZYMES AND SUBSTRATES
Blueberry. Horseradish. Watercress
1. Blueberry
(a) Extraction of Enzymes from blueberries
500 grams of the berries were pulverized in a Waring Blendor with dry ice. This was extracted with 500 ml of 1.77. sodium borate (pH 4.5 adjusted to pH 8.0 with 307, sodium hy- droxide), with stirring for two hours at room temperature (final pH ■ 7.4). The mixture was centrifuged and precipita- ted with an equal volume of cold acetone. After a 10-minute wait, the mixture was centrifuged and the precipitate slurried in water. The resultant preparation was freeze-dried.
(b) Substrate preparation from berries
Fresh frozen blueberry substrate was prepared by boiling 400 grams of the berries for 10 minutes with 400 ml water. The mixture was cooled and filtered through cheese- cloth. The filtrate was stirred for 15 minutes with 57. Nuchar, filtered and frozen.
(c) Extraction of Enzymes from Blueberry Leaves
60 grams of the leaves were treated in a Waring Blendor with 450 cc of phosphate buffer (pH 7.0) for two hours at room temperature. The resultant material was filtered through cheesecloth and filtrate precipitated with an equal volume of cold acetone. The precipitate was centrifuged and freeze-dried.
(d) Substrate preparation from leaves
Blueberry leaf substrate was prepared by boiling 87 grams of dry leaves with about 800 cc water for 5 minutes. The mixture was cooled, run through a Waring Blendor and filtered through cheesecloth. The filtrate was stirred for 15 minutes with 57, Nuchar, filtered and frozen.
- 61
TABLE XXIII (Continued)
2. Horseradish
(a) Substrate
Horseradish substrate was prepared from both fresh and commercial dehydrated material. The fresh horseradish was cut into strips, boiled for 15 minutes with water, then dried in a forced draft oven for 3-1/2 hours at 80oC. The dried strips were then ground in a Waring Blendor. The commercial dehydrated powder was boiled for 15 minutes and tben lyophilized.
(b) Enzyme
Fresh horseradish was pulverized in a Waring Blendor with dry ice. The powder was extracted with an equal volume of cold distilled water for 1 hour at 50C. Following extract- ion, the solids were removed by filtßring through cheesecloth, and the filtrate further clarified by centrifugation. An equal volume of cold acetone was added to the supernatent and the resultant precipitate was centrifuged. The precipitate was slurrled in water and lyophilized.
3. Watercress
(a) Substrate
100 grams of powdered dehydrated watercress was boiled for 15 minutes in water. The material was centrifuged and lyophilized.
(b) Enzyme
Myrosinase enzyme, prepared from white mustard seeds was used. 600 grams of white mustard seeds were ground with dry ice in a Waring Blendor and extracted with 2400 ml of cold water for 1 hour. This was filtered through cheesecloth and centrifuged. The supernatent was precipitated with an equal vo^vme of 90% ethanol and centrifuged. The resulting precip- itate vas washed with 70% ethanol, centrifuged, suspended in 2 liters of water, filtered and lyophilized.
- 62 -
TABLE XXIV
PINEAPPLE ENZYME STUDIES
ACTUAL EXPERIMENTAL PROCEDURES FOR PREPARATION OF NEW ENZYMES
The pineapple used was fresh fruit obtained locally. An effort was made to purchase a quantity of fruit suitable for experimentation so that variance due to crop and ripeness of fruit was minimal. The fruit was bought In large batches and stored In a refrigerator at approximately 450F. The act- ual history, i.e. age, variety, processing, and storage con- ditions, of the pineapple purchased is not known. During the experiment it was observed that the fruit was ripe and possess- ed a delightful aroma and characteristic flavor.
The fruit was divided by h nd into its various sections, such as core^fruit, peel or skin, and leaves. Im- mediately after sectioning, the fruit was processed and/or frozen to minimize deterioration.
The freeze-drying was accomplished in a Model 15 RePP sublimator according to suggested operating procedures. The liquid samples were placed in suitable trays (small or large trays were used depending upon the amount of sample) and frozen in the freeze-drier until a temperature of approximately -50 F was obtained. The condensers were then activated until their tenperature reached -AG F or lower. The vacuum pump was turned on. When the McLeod Gauge showed a pressure of 50 microns or less, the shelf heat was turned on at setting of 80 F.
The dried fruit substrate or enzyme was removed when the product temperature was equal to the shelf temperature. The shelf temperature was kept low to prevent any possible deterioration or inactlvation of the sample due to excessive heating.
The following enzyme preparations were made:
1. The juice of two fresh pineapples was extracted through a Juice X Extractor to yield one liter of juice. The juice was centrifuged, acetone precipitated with an equal volume of -30OC acetone, and again centrifuged. The precipitate was slurried in water and freeze-dried to yield 1.5 grams of Enzyme 1.
- 63 -
TABLE XXIV
(Continued)
2. One fresh pineapple was peeled, and 1000 grams was extracted in a Waring Blendor with 400 ml of 1.7 percent so- dium tetraborate at 50C. The solution, having an initial pH 9.5 before the addition of the pineapple, had a pH 4 after mixing. The resulting pH was not readjusted. The solution was extr&cted for 5 minutes, filtered through cheese cloth, and centrifuged. The extract was precipitated with an equal volume of -30 C acetone, and the precipitate was slurried in water and freeze-dried to yield 1.5 grams of Enzyme 2.
3. Another fresh pineapple was extracted with 400 ml of phosphate buffer (pH 8). After mixing in the Waring Blen- dor, the pH became 2 and was then adjusted to pH 6.0 with 2N NaOH. The solution was filtered through cheese cloth, centrifuged, precipitated with acetone, and freeze-dried as above to yield 1,4 grams of Enzyme 3.
4. 100 grams of pineapple leaves were extracted with 200 ml of a 1.7 percent solution of sodium tetraborate, filtered, and centrifuged. The extract was pH 8 and was precipitated with acetone as above to yield 0.5 grams of Enzyme 4.
5. 100 grams of pineapple leaves were extracted with 0.1M citrate phosphate buffer (pH 5.6), filtered, centrifuged, and precipitated with acetone as above to yield 0.4 gram of Enzyme 5.
6. 300 grami of pineapple peel were extracted with 200 ml of a 1.7 percent sodium tetraborate as above, fil- tered, and centrifuged. The extract (pH 7.0) was precip- itated with acetone to yield 1.7 grams of Enzyme 6.
7. 300 grams of pineapple peel were extracted with a citrate phosphate buffer (pH 5.6), filtered, centrifuged, and precipitated with acetone as above to yield 0.3 grams of Enzyme 7.
8. Pineapple peel was extracted with 30 percent sodium carbonate and then neutralized with acetic acid. This was freeze-dried without acetone precipitation to yield 43.1 grams of Enzyme 8.
9. Pineapple core was extracted with 40 ml of 30 percent sodium carbonate and neutralized with acetic acid and freeze- dried to yield 28.2 grams of Enzyme 9.
- 64 •
TABLE XXIV
(Continued)
10. 189 grams of core were extracted with an equal weight of cold water with 10 ml of 30 percent sodium carbonate. The extract was filtered, precipitated with acetone, and freeze- dried as in preparation to yield 0.45 grams of Enzyme 10.
11. 406 grams of pineapple peel were extracted with an equal weight of ice water and 30 percent sodium carbonate was added until a pH 8.0 was obtained. The extract was precip- itated with acetone as above to yield 2.5 grams of Enzyme 11.
12. 1019 grams of pineapple were extracted with an equal weight of ice water and buffered to pH 8 with 30 percent sodium carbonate as above. The extract was filtered and pre- cipitated with acetone to yield 0.75 grams of Enzyme 12.
13. Eight hundred grams of unprocessed core and peel from a fresh pineapple frozen overnight was ground in a Waring Blendor with one liter of water and 60 ml of 33-1/3 percent sodium carbonate solution, so that the slurry was positive to phenolthalein. The sample was filtered through 8-fold cheese- cloth and Whatman No. 4 filter paper, acidified to pH 5, and freeze-dried to obtain Enzyme 13.
14. Four hundred fifty-six grams of fresh pineapple core and an equal weight of Ice was placed in a Waring Blendor. To the mixture was added 200 milligrams of Pectionol 10M. The mixture was stirred and allowed to stand overnight. The sample was then heated to 180 F with stirring, cooled immediately with ice, and filtered through Whatman No. 4 and then No. 2 filter paper to yield 1400 ml of filtrate. To the filtrate was added 15 ml of 33-1/3 percent sodium carbonate solution. The solution was stirred, and 1400 ml of cold acetone (0 C was added in small increments with constant stirring. The mixture was placed in a freezer overnight. The preparation was centrifuged at 2000 R.P.M. for 20 minutes and the precipitate was slurried in water and freeze-dried to yield Enzyme 14.
15. To the residue from the filtration in Enzyme 14 preparation was added 600 ml of water and 2 ml of 33-1/3 per- cent sodium carbonate solution. The sample was filtered through Whatman No. 2 filter paper. The filtrate was satura- ted with sodium chloride and again filtered through Whatman No. 2 filter paper to yield residue which is Enzyme 15.
- 65 -
r
TABLE XXIV
(Continued)
16. Five hundred grams of pineapple skin (cold) was blended in a Waring Blendor with 600 ml of water and stirred for 2 hours. The sample was filtered through 8-fold cheese- cloth, Whatman No. 4, No. 1, and No. 2 filter paper In se- quence, to yield approximately one liter of filtrate. An equal volume of cold 95 percent ethanol was added, and the material was centrlfuged at 2000 R.P.M. for 20 minutes. The residue was slurrled In water, and the residual ethanol evaporated. The enzyme slurry was freeze-dried to yield 1.7 grams of Enzyme 16.
17. Two hundred twenty-seven grams of pineapple leaves and 900 ml of water and Ice were ground In a Waring Blendor (final pH of 4.0). The material was filtered through 8-fold cheesecloth. Five grams of Nuchar was added, and the mixture was stirred for 10 minutes and filtered through Hyflo Supercel. The solution was freeze-drled to yield 5.7 grams of Enzyme 17,
18. One hundred nine grams of pineapple core and 100 ml of water were mixed In a Waring Blendor and brought to pH 8.5 with 30 ml of 33-1/3 percent sodium carbonate solution. The sample W-JS f 1 .tered through cheesecloth, neutralized to pH 7.0 with hydrochloric acid, and again filtered through cheesecloth. The volume of the filtrate was 175 ml. This filtrate was freeze-dried to yield 11.2 grams of Enzyme 18.
- 66 -
TABLE XXV
PINEAPPLE ENZYME STUDIES
ACTUAL EXPERIMENTAL PROCEDURE FOR PREPARATION OF SUBSTRATE*
The substrate was prepared in a similar, but not as complex, procedure. The substrates made from the fruit can be freeze-dried if desired, but in commercial practice the pro- cessed foods themselves are the basic substrates of flavor precursors. While it is difficult to isolate the proper enzyme systems, care must also be taken to select the proper flavor substrates for the flavor enzyme associated with the total flavor desired,
1. One hundred forty-one grams of blanched pineapple fruit slices were freeze-dried and then ground to form a powder. The yield was 25 grams of Substrate A.*
2. One hundred nine grams of blanched pineapple core plus 100 ml of water were mixed in a Waring Blendor and brought to pH 8.5 with 30 ml of a 33-1/3 percent sodium car- bonate solution. The sample was filtered through cheesecloth, neutralized to pH 7.0 with hydrochloric acid, and again filtered through cheesecloth. The volume of the filtrate was 175 ml. This filtrate was freeze-dried to yield 11.2 grams of Substrate B.
3. One hundred forty grams of blanched pineapple was comminuted in a Waring Blendor, then frozen and freeze-dried to yield 21.6 grams of Substrate C.
4. Two hundred thirty grams of blanched pineapple were put through a Juice X Extractor to yield 130 ml of liquid, which was then freeze-dried to yield 13.6 grams of Substrate D.
5. Seven hundred grams of pineapple was ground in a Waring Blendor. The material was heated to 140-145oF with constant stirring; Pectionol 10M was added to the material. The mixture was stirred for 2 hours and brought to 180oF in 20 minutes to inactivate the enzymes. The material was then filtered through Whatman No. 4 and through Whatman No. 2 filter paper. Two grams of Nuchar activated charcoal was added, and the mixture was stirred for 20 minutes and filtered through Hyflo Supercel and freeze-dried to yield 20.7 grams of dry Substrate E.
6. Substrate E (approximately 1/2 of Substrate E) was rehydrated and frozen to yield 250 ml of Substrate F.
I
^Henceforth, substrates of which the preparation is reported in this section will be referred to as "Substrate A", "Substrate B", etc. - ^7 -
TABLE XXVI
COMPOSITION OF NEW FLAVORS AND FLAVOR-TO-BASE RATIOS
Sardine Parts by Weight
Base Mix Formula No. 18 96 Sardine Extract (Freeze-drled) 4
Strawberry
Base Mix Formula No. 18 Strawberries (Freeze-drled) 10
soya
Base Mix Formula No. 18 85 Soy Sauce Mix (Freeze-drled) 15
Soy Sauce Mix consists of: Lactose 150 Km. Soy Sauce 450 gm. Wine Vinegar 30 gm.
Orange
Base Mix Formula No. 18 85 Oiange Crystals (McKees) 15
- 68 -
TABLE XXVII
RESULTS OF SIX-MONTH STORAGE TESTS ON FLAVORED 7001? BARS
STORED IN SEALED METAL CANS
Flavor
Storage Temperature
and Media
T e s t e r s Average Hedonic Rating
Flavor
1 2 3 4 5 6 Total Transfer
Sardines
100oF-0xvßen 6 8 6 5 5 5 35 5.8 None 100UF-Nitrogen 6 7 7 5 6 5 36 6.0 k None 70uK-0xyRen 5 8 6 5 6 6 36 6.0 None 70UF-Nitrop,en 6 8 6 5 6 6 37 6.1 None 40oF-0xyßen 6 8 7 6 7 41 6.8 None 40oF-Nitroßen 6 7 8 6 7 41 6.8 None
R* - Oxygen 6 7 6 6 7 39 6.5 None R* - Nitrogen 6 8 6 6 7 , 40 6.6 None
Strawberry
l
100oF-0xygen 7 9 8 6 7 44 7.3 None 100UF-Nitrogen 7 7 7 7 7 42 7.0 None 70oF-0xygen 8 9 8 7 8 9 49 8.1 None 70oF-NitroKen 8 9 8 7 8 9 49 8.1 None 40oF-0xygen 9 9 7 7 9 9 50 8.3 None 40oF-Nitrogen 9 9 7 7 9 9 50 8.3 None
R* - Oxygen 9 9 8 7 9 9 51 8.5 None R* - Nitrogen 9 9 , 8 I 7 i 9 9 51 8.5 None
Soy
100oF-0xygen 6 8 7 6 6 6 39 6.5 None lOO^-Nitrogen 6 8 7 7 6 7 41 6.8 None 70oF-0xygen 8 8 6 6 6 41 6.8 None 70oF-Nitrogen 8 7 7 6 42 7.0 None 40oF-0xygen 8 7 7 6 42 7.0 None 40oF-Nitrogen 8 7 7 6 42 7.0 None
R* - Oxygen 8 7 7 6 42 7.0 None R* - Nitrogen kJL ^8^ 7 6 43 7.1 None
Orange
IGO^-Oxygen 5 6 8 6 6 6 37 6.1 None IGO^-Nitrogen 5 7 7 6 5 6 36 6.0 None 70oF-0xygen 6 7 7 7 6 6 39 6.5 None 70oF-Nitrogen 6 6 7 7 5 7 38 6.3 None 40oF-0xygen 6 7 6 7 6 7 39 6.5 None 40oF-Nitrogen 6 7 6 7 5 8 39 6.5 None
R* - Oxygen 6 7 6 7 6 7 39 6.5 None R* - Nitrogen 7 7 6 7 5 7 39 6.5 None
♦Recycling - 69 -
TABLE XXVIII
RESULTS OF SIX-MONTH STORAGE TESTS ON FLAVORED FOOD LARS
PACKED IN ALUMINUM FOIL POUCHES
Flavor Storage Temperature
Testers Average Hedonic Rating 1 2 3 4 5 6 Total
Sardines
100OF 6 6 5 5 6 5 33 5.5
70OF 6 6 6 6 6 5 35 5.8
40oF 6 6 6 6 6 5 35 5.8
Recycling 6 6 6 5 6 5 34 5.6
Strawberry
|
100OF 6 7 6 7 5 38 6.3
70OF 6 7 7 7 6 40 6.6
40OF ■7 4 8 8 8 8 4 7.6
Recycling 7 8 8 8 7 4 7.5
Soy
100OF 6 6 7 6 5 35 5.8
70OF 6 6 6 7 6 6 37 6.1
40OF 6 6 6 7 7 6 38 6.3
Recycling 7 6 6 6 7 6 38 6.3
Orange
100OF 6 5 5 6 5 6 35 5.8
70OF 6 7 5 6 6 7 37 6.1
40OF 7 7 7 6 6 7 40 6.6
Recycling 7 7 7 6 5 7 39 6.5
70 -
TABLE XXIX
PREPARATION OF SARDINE EXTRACT
Tne sardine extract was prepared from commercially canned sardines which were thoroughly drained of the oil used in packing. The sardines were ground in a variable-speed Waring blendor and extracted twice with ethyl alcohol (957.) to remove the oil fractions (approximately 500 grams of ethyl alcohol were used per 675 grams of ground sardines. A slurry was prepared using 500 ml of water to 675 gms of ground sar- dines and then heated to 80oC and allowed to simmer for four hours under constant agitation. The remaining liquids were decanted and freeze-dried. The freeze-drying was accomplished in a Model 15 RePP sublimator; the liquid extract was placed in stainless steel trays and frozen in the freeze-dryer until an internal temperature of -50oF was obtained. The condensers were then activated until their temperature reached -40°?, when the vacuum pump was turned on. When the McLeod Gauge showed a pressure of less than 50 microns, the shelf heat was turned on at a setting of 70oF.
The dried extract was removed when the product tem- perature was equal to the shelf temperature, which was kept low to prevent any possible deterioration of the sample. The dried water extract had a very good fish flavor and aroma; the alcohol extract was high in fish aroma and very low in fish flavor. The remaining extracted fish residue was lacking in fish flavor and aroma.
71 -
Lactose Ad j unc t:
Salt Adj unc t:
Citric Acid Adjunct:
TABLE XXX
COMPOSITION OF FLAVOR ADJUNCTS AND FLAVOR
CURRY FLAVOR COMPOSITION
Curry Concentrate Part s by Weight
Coriander Powder 750 Cumin Powder 300 Fenugreek Powder 300 Black Pepper Powder 180 Cardamon Powder 150 Mace Powder 120 Allspice Powder 105 Cinnamon Powder 105 Mustard Powder 60 Paprika Powder 45 Ginger Powder 30 Celery Powder 15 Cayenne Powder 15 Orange Oil 15
Base Mix To Flavor - Adiunct Ratio
Base Mix Formula No. 18 85 Curry/Lactose Mix 15
consisting of: Lactose 200 Curry Flavor 50 Carboxymethylcellulose 7H0P 10
Base Mix Formula No. 18 92.5
Curry/Salt Mix 7.5
consisting of: Salt 200
Curry Flavor 130 Carboxymethylcellulose 7H0P 3
Base Mix Formula No. 18 95.8
Curry/Citric Mix 4.2
consisting of: Citric Acid 67
Curry Flavor 200 rat-hnvvmpt-hvlcellulose 7H0P 2.5
72 -
TABLE XXX
(Continued)
COMPOSITION OF FLAVOR ADJUNCTS AND FLAVOR
CURRY FLAVOR COMPOSITION
(Conti nued)
Mertaste 5 Adjunct:
Base Mix Formula No. 18 Curry/Mertaste 5' Mix
consisting of: Mertaste 5' Curry Flavor Carboxymethylcellulose 7HOP
9$.8 4.2
50 150
3
Disodium Guanylate Adjunct:
Base Mix Formula No. 18 Curry/Disodium Guanylate Mix
consisting of: Disodium Guanylate Curry Flavor Carboxymethylcellulose 7H0P
96.8 3.2
4 200
2
- 73 -
TABLE XXXI
COMPOSITION OF FLAVOR ADJUNCTS AND FLAVOR
LEMON FLAVOR COMPOSITION
Lemon Concentrate Parts by Weight
Exchange Lemon Oil 1000 Lemon Oll 5X 500 Veltol - 2% In Ethyl Alcohol 100 Terpenless Lemon Oil 50
Base Mix to Fl>avor/Proteln/Salt/Carbohydrate Ratio
Base Mix Formula No. 18 92.5 Lemon/Lactose Mix 7.5
consists of: Lactose 200 Lemon Flavor Oil 50 Carboxymethylcellulose 7HOP 5
Base Mix Formula No. 18 96.3 Lemon/Salt Mix 3.7
consists of: Salt 200 Lemon Flavor Oil 150 Carboxymethylcellulose 7HOP 8
Base Mix Formula No. 18 98.6 Lemon/Mertaste 5' Mix 1.4
consists of: Mertaste 5' 150 Lemon Flavor Oil 450 Carboxymethylcellulose 7H0P 2
Base Mix Formula No. 18 98.1 Lemon/Disodium Guanylate Mix 1.9
consists of: Disodium Guanylate 3 Lemon Flavor Oil 150 Gum Arabic 100
- 74 -
TABLE XXXII
COMPOSITION OF FLAVOR ADJUNCTS AND FLAVOR
CHrRRY FLAVOR COMPOSITION
Cherry Concentrate Parts by Weight
Ethyl Oenanthate 1.2 Tulyl Aldehyde 12.3 Benzaldehyde N.F. 55.8 Candy Base Mix 8.5 Ethyl Alcohol 78.0
Candy Base Mix
Eugenul 2.0 Anisyl Acetate 9.0 Amyl Cinnamic Aldehyde 15.0 Absolute Jasmin 1.0 Vanillin 24.0 Ethyl Tolylglycidate 25.0 Anisyl Aldehyde 9.0
Base Mix to Flavor/Protein/Salt/Carbohydrate Ratio
Base Mix Formula No. 18 91 Cherry/Lactose Mix 9
consists of: Lactose 400 Cherry Flavor Concentrate 100 Carboxymethylcellulose 7H0P 5
Base Mix Formula No. 18 96.4 Cherry/Salt Mix 3.6 consists of:
Salt 300 Cherry Flavor Concentrate 225 Carboxymethylcellulose 7H0P 4
Base Mix Formula No. 18 98.2 Cherry/Mertaste 5' 1-8
consists of: Mertaste 5' 150 Cherry Flavor Concentrate 450 Carboxymethyl Cellulose 7H0P 2
- 75 -
TABLE XXXII
(Continued)
COMPOSITION OF FLAVOR ADJUNCTS AND FLAVOR —i— — r ■-■ ■-■ -ifr - iPM ■ IIW-B it i \ ^ m i t mm ■ HI IIPMIHMWII IMII I
CHERRY FLAVOR COMPOSITION
(Continued)
Base Mix Formula No. 18 97.5 Cherry/Disodium Guanylate Mix 2.5 consists of:
Disodium Guanylate 3 Cherry Flavor Concentrate 150 Cum Arabic 100
- 76 -
TABLE XXXIII
RESULTS OF SIX-MONTH STORAGE TESTS ON FLAVOR ADJUNCTS
IN CURRY-FLAVORED FOOD BARS PACKED IN POUCHES
Flavor Adjunct
Storage Temperature
T e ! 3 t e r J 5 Average Hedonic Rating 1 2 3 4 5 6 Total
Lactose
100OF 7 6 5 7 7 6 38 6.3
70OF 6 6 5 7 6 6 36 6.0
40OF 6 6 5 6 6 7 36 6.0
Recycling^ 6 6 5 6 6 7 36 6.0
Salt
100OF 6 6 6 5 5 6 34 5.6
70OF 6 6 6 6 6 5 35 5.8
40oF 7 6 6 6 6 7 38 6.3
RecyclinR 7 6 6 6 6 6 37 6.1
Citric
100oF 6 6 6 5 6 6 35 5.8
70OF 6 6 5 5 6 6 34 5.6
40oF 7 6 6 5 6 6 36 6.0
Recycling 7 6 6 5 6 6 36 6.0
Dlsodium Gyanylate
100OF 6 5 5 5 5 6 32 5.3
70OF 6 6 6 6 6 5 35 5.8
40OF 6 6 6 6 6 6 36 6.0
Recycling 5 6 6 6 6 6 35 5.8
- 77 -
TABLE XXXIV
RESULTS OF SIX-MONTH STORAGE TESTS ON FLAVOR ADJUNCTS
IN LEMON-FLAVORED FOOD BARS PACKED IN POUCHES
Flavor Adjunct
Storage Temperature
T e s t e r J 3 Average Hedonic Rating 1 2 3 4
. —_
5 6 Total
Lactose
100OF 6 6 6 7 7 6 38 6.3
70OF 7 6 7 7 7 7 41 6.8
40OF 7 6 7 7 8 8 43 7.1
Recycling 7 7 7 7 8 7 43 7.1
Salt
100OF 5 6 5 6 6 6 34 5.6
70OF 6 6 5 6 6 6 35 5.8
40OF 6 6 6 6 6 7 37 6.1
Recycling 5 6 6 7 5 6 35 5.8
Gyanylate
100OF 5 5 5 6 7 6 34 5.6
70OF 5 6 6 6 6 6 34 5.6
40oF 6 7 6 6 6 6 37 6.1
Recycling 7 6 7 6 6 6 38 6.3
Mertaste
100oF 5 5 5 6 5 6 32 5.3
70OF 5 5 5 6 6 5 32 5.3
40OF 6 6 7 7 6 6 38 6.3
Recycling 6 6 6 6 6 7 37 6.1
78 -
TABLE XXXV
RESULTS OF SIX-MONTH STORAGE TESTS ON FLAVOR ADJUNCTS
IN CHERRY-FLAVORED FOOD BARS PACKED IN POUCHES
Flavor Adjunct
Storage Temperature
Testers Average Hedonic Rating 1 2 3 4 5 6 Total
Lactose
100OF 5 6 6 6 7 6 36 6.0
70OF 6 6 6 6 7 6 37 6.1
40OF -» 6 6 7 7 5 40 6.6
Recycling 7 6 5 7 7 6 38 6.3
Salt
100OF 5 6 5 5 6 5 32 5.3
70OF 5 6 5 6 7 5 34 5.6
40OF 6 6 6 6 7 5 36 6.0
RocyclinR 5 6 5 6 7 6 35 5.8
Disodium Gyanylate
100OF 5 5 5 5 5 5 30 5.0
70OF 6 6 5 5 6 6 34 5.6
40OF 6 7 6 6 6 6 37 6.1
Recycling 6 6 6 6 5 6 35 5.8
Mertaste 5
100OF 6 7 6 6 6 6 37 6.1
70OF 7 7 6 6 6 6 38 6.3
40OF 6 7 7 7 6 6 39 6.5
Recycling 6 6 6 6 1 7 7 38 6.3
- 79 -
TABLE XXXVI
RESULTS OF SIX-MUNTU STORAGE TESTS ON FLAVOR ADJUNCTS
IN CURRY-FLAVORED FOOD BARS PACKED IN SEALED METAL CANS
Flavor Storage
Temperature and
Media
Testers Average Hedonic Rating
Flavor Adj unc t
1 2 3 4 5 6 Total Transfe
40OF-0xygen 7 6 5 6 6 6 36 6.0 None 40WF-Nitrogen 7 6 5 6 6 6 36 6.0 None R* -Oxygen 7 6 5 6 6 6 36 6.0 None
Lactose R* -Nitrogen 7 6 5 6 6 6 36 6.0 None 70oF-0xygcn 6 6 5 7 7 7 38 6.3 None 70oF-Nitrogen 6 1 6 5 7 7 7 38 6.3 None
100UF-Oxygen 7 6 4 8 6 6 37 6.1 None 100UF-Nitrogen 8 S 4 6 7 7 38 6.3 None 40oF-0xygen 6 7 5
l 3 6 6 35 5.8 None 40oF-Nitrogen 6 7 5 6 5 6 34 5.6 None
Carboxy Methyl Cellulose
K* -Oxygen 6 7 5 6 6 6 36 6.0 None RVc -Nitrogen 6 7 5 6 6 6 36 6.0 None
70ÜF-Oxygen 6 7 3 6 | 3 6 35 5.8 None 70oF-Nitrogen 6 7 5 6 3 0 35 5.8 None
100oF-Oxygen 6 7 4 5 6 6 34 5.6 None 100"F-Nitrogen 6 6 5 5 6 Ar 34 5.6 None 40üF-OxygGn 5 6 6 7 7 7 38 6.3 None 40oF-Niti-ogen 5 6 6 7 7 7 38 6.3 None R* -Oxygen 5 6 6 7 7 6 37 6.1 None
Citric R* -Nitrogen 5 6 6 6 7 6 36 6.0 None Acid 70UF-Oxygeil 5 6 6 7 7 7 38 6.3 None
70ÜF-Nitrogen 5 6 6 b 7 6 36 6.0 None 100UF-Oxygen 5 5 6 6 7 7 36 6.0 None 100uF-NiCrogen 5 5 6 7 7 7 37 6.1 None
40oF-Oxygen 6 6 6 7 6 6 37 6.1 None 40oF-Nitrogen 6 6 7 7 6 6 38 6.3 None R* -Oxygen 6 6 7 7 5 6 37 6.1 None
Mertaste 5 R* -Nitrogen 6 6 6 7 6 6 37 6.1 None 70oF-0xygen 6 6 ; 7 7 6 6 38 6.3 None 70C>F-Nitrogen 6 6 6 7 6 6 37 6.1 None
100oF-0xygen 6 e 6 7 6 6 37 6.1 None 100oF-Nitrogen 6 5 5 7 7 5 35 5.8 None
40UF-Oxygen 6 5 6" 5 5 34 5.6 None 40UF-Nitrogen 6 5 5 6 5 34 5.6 None R* -Oxygen 6 5 6 5 j 35 5.8 None
Gyanylate R* -Nitrogen 6 5 5 5 6 34 5.6 None 70UF-Oxygen 6 5 6 6 7 37 6.1 None 70UF-Nitrogen 7 5 7 6 6 38 6.3 None
. 100UF-Oxygen 6 7 5 6 5 6 35 5.8 None 100WF-Nitro«en 6 7 6 6 6 5 36 j 6.0 | None
*Recycling - 80 -
TABLE XXXVII
RESULTS OF SIX-MONTH STORAGE TESTS ON FLAVOR ADJUNCTS
IN LEMON-FLAVORED FOOD BARS PACKED IN SEALED METAL CANS
Flavor Ad j unc t
| Storage Temperature
I and | Media
T < 2 S t e r s Average Hedonic
Flavor
1 2 3 4 ! 5 1 6 Total Transfer
Lactose
40oF-0xygen 8 ' 6 5 i 7 i 7 1 6 39 6.5 None f 40oF-Nitro>>en 8 i 7 ! 5 ; 7 : 7 6 ! 40 6.6 None
1 R* -Oxygen 8 \ 7 1 3 i 7 7 6 40 6.6 None R* -Nitrogen 6 ! 7 ! 5 ! 7 1 7 ] 6 ' 38 6.3 None
70oF-0xygen 6 ' 6 I 5 i 6 1 6 i 6 35 5.8 None I 70oF-Nitrogen 6 ! 6 5 : e 6 ■ 6 35 5.8 None
100oF-0xygen 5 1 7 4 I 6 5 1 6 1 33 5.5 None 1 100oF-Nitrogen I 5 j 8 "7 ! 5 5 < 6 33 5.5 None
Salt
40UF-Oxyßen iT" 1 6 ^ 6 6 r'6 \ 6 36 6.0 None 40uF-NitroRen 6 ! 5 6 7 6 5 35 5.8 None
R* -Oxygen 6 ! 6 7 6 6 6 37 6.1 None R* -Nitrogen 6 1 6 7 6 6 6 37 6.1 None
70UF-Oxygen 6 1 7 7 6 6 6 38 6.3 None 70UF-Nitrogen 6 1 7 7 6 6 7 39 6.5 None
100UF-Oxygen 5 \ 7 6 6 5 7 36 6.0 None 100UF-Nitrogen 5 ! 7 6 5 5 7 35 5.8 None
Gyanylate
40VJF-Oxyßen 17 !' 7 7 8 7 6 42 7.0 None 40oF-Nitrogen 7 7 7 8 8 7 44 7.3 None
R* -Oxygen 7 6 7 7 7 7 41 6.8 None R* -Nitrogen 6 6 7 8 8 7 42 7.0 None
70oF-0xygen 8 5 6 6 5 7 37 6.1 None 70oF-Nitrogen 7 5 6 6 6 6 36 6.0 None
100oF-0xygen 6 5 5 5 5 5 31 5.1 None 100oF-Nitrogen 6 5 I 5 5 6 32 5.3 None
Mertaste
40UF-Oxygen 7 6 ! 6 7 6 7 39 6.5 None 40UF-Nitrogen 7 6 i 6 1 7 1 6 7 j 3S l 6.5 None
R* -Oxygen 7 6 6 1 7 i 6 36 6.3 None R* -Nitrogen 6 6 7 j 7 6 7 39 6.5 None
70oF-0xygen 6 5 6 7 5 7 36 6.0 None 70°" Nitrogen 6 5 ! 6 ! 5 5 6 32 5.5 None
100oF-0xygen 6 5 | 5 ! 5 1 5 i 5 31 5.1 None 100oF-Nitrogen 6 1 5 1 6 1 5 1 5 i 5 ! 32 5.3 None
•
*Recycl ing
- 81 - »
TABLE XXXVIII
RESULTS OF SIX-MONTH STORAGE TESTS ON FLAVOR ADJUNCTS
IN CHERRY-FLAVORED FOOD BARS PACKED IN SEALED METAL CANS
Flavor Storage
Temperature and
Media
T . e s t e r s Average Hedonic Rating
Flavor Adjunct
1 2 3 4 5 6 Total Transfer
400F-Oxyßen 7 8 7 6 7 6 41 6.8 None 40oF-Nitrogen 7 8 7 7 7 6 42 7.0 None R* -Oxygen 7 8 7 6 7 6 41 6.8 None
Lactose R* -Nitrogen 7 7 7 7 7 5 40 6.6 None 70UF-Oxygen 6 7 7 7 7 5 39 6.5 None 70UF-Nitrogen 6 7 7 7 7 5 39 6.5 None
lOO^F-Oxygen 6 6 7 6 6 5 36 6.0 None 100UF-Nitrogen 6 6 7 __7__ JL 5 3S 6.3 None 40UF-Oxygen 5 D i' e 5 6 6 34 5.6 None 40UF-Nitrogen 5 5 6 6 5 6 33 5.5 None R* -Oxygen 5 6 6 5 5 6 33 5.5 None'
Salt R* -Nitrogen 5 6 6 6 5 6 34 5.6 None 70UF-Oxygen 5 6 6 6 5 6 34 5.6 None 70UF-Nitrogen 5 6 5 6 5 6 33 5.5 None
1000F-Oxygen 5 6 5 5 5 6 32 5.3 None 100UF-Nitrogen 5 6 5 5 6 6 33 5.5 None
40UF-Oxvgen 6 j 7 6 6 5 37 6.1 None 40UF-Nitrogen 6 7 6 6 5 37 6.1 None R* -Oxygen 6 7 6 6 5 37 6.1 None
Dlsodlum R* -Nitrogen 6 7 7 6 5 38 6.3 None Gyanylate 70UF-Oxygen 6 6 6 6 5 36 6.0 None
70ÜF-Nitrogen 6 6 7 6 5 37 6.1 None 100UF-Oxygen 6 6 6 6 5 6 35 5.8 None 1Ü00F-Nitrogen 6 6 6 6 4 6
6 34
39
5.6 None
40UF-Oxygen 7 "e"1 7 6 6.5 None
40oF-Nitrogen 7 6 7 7 5 39 6.5 None R* -Oxygen 7 6 6 6 5 37 6.1 None
Mertaste 5 R* -Nitrogen 7 6 6 7 6 39 6.5 None 70UF-Oxygen 6 6 6 6 i 37 6.1 None 70oF-Nitrogen 7 6 6 6 6 38 6.3 None
100UF-Oxygen 7 6 7 6 6 39 6.5 None 100UF-Nitrogen 7 7 7 6 6 40 1 6.6 None
♦Recycling
- 82 -
ij m - Kl V liiliil II, M ll
i 11 HI i
•:.'? rr : J. J
I I ,.-=+•
"3»
• 4
I I i
ii il
lii i
1. iiiil II
I JJ
'
lU
mi
- *L -
