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Accelerating Shelf-life Tests (ASLT) New formulations always have to be analyzed in terms of physical stability beside chemical and sensory evaluation leading to time-consuming development processes. The industry consequently employs ASLTs to accelerate these changes. In difference to beer a systematic approach to evaluate the effect of artificial storage conditions for rapid tests in emulsion based beverages is not available yet. Therefore, different tests were compared in regard to physical changes of beverages with orange oil emulsion. C) Low Homog. Pressure 12 % Emulsifier (OSA-starch) 6 % Orange oil 6 % Weighting agent HP-homogenization: 1x 250/50 bar x 90 = 5710 nm Comparative study of accelerated shelf-life tests on physical ageing of beverages containing weighted flavor emulsions Conclusion Motivation Sören Rossmann, Verena Wolff, Ulrich Müller, Jan Schneider North Rhine Westfalia Institute of Food Technology ILT.NRW, Lemgo, Germany References www.ilt-nrw.de [1] Piorkowski, D. T. and McClements, D. J. (2014): Beverage emulsions: Recent developments in formulation, production, and applications, Food Hydrocolloids, 42. [2] Tan, C.-T.: Beverage Emulsions, in Friberg, S. E. and Larsson, K. (Eds.)(1997): Food emulsions, 3. ed., rev. and expanded, Dekker, New York. [3] Reiner, S. J.; Reineccius, G. A. and Peppard, T. L. (2010): A Comparison of the Stability of Beverage Cloud Emulsions Formulated with Different Gum Acacia- and Starch- Based Emulsifiers, Journal of Food Science, 75,5. [4] Lim, S. S.; Baik, M. Y.; Decker, E. A.; Henson, L.; Michael Popplewell, L.; McClements, D. J. (2011): Stabilization of orange oil-in-water emulsions: A new role for ester gum as an Ostwald ripening inhibitor, Food Chemistry, 128,4. Results Contact ILT.NRW Beverage Technology Sören Rossmann [email protected] Emulsion based beverages Beverage emulsions are an important product for the preparation of increasingly popular beer-based mixed drinks and soft drinks in order to incorporate water insoluble colors or flavors (flavor emulsion), to generate turbidity (cloud emulsion) or both combined [1]. Compared to other oil-in-water food emulsions, beverage emulsions are a unique class of type, as they are highly concentrated semi-finished products and after being processed in- to drinks finally consumed considerably diluted [2]. Experimental Setup A) Reference Emulsion 12 % Emulsifier (OSA-starch) 6 % Orange oil 6 % Weighting agent HP-homogenization: 2x 300/50 bar B) Reduced Ester Gum 12 % Emulsifier (OSA-starch) 10 % Orange oil 2 % Weighting Agent HP-homogenization: 2x 300/50 bar x 90 = 736 nm x 90 = 620 nm D) Reduced Emulsifier 6 % Emulsifier (OSA-starch) 6 % Orange oil 6 % Weighting agent HP-homogenization: 2x 300/50 bar x 90 = 785 nm Emulsions A to D were diluted to Ready-to-drink beverages for stability analyzing: 0,12 % emulsion diluted with beverage base (10 °Bx sucrose, pH 3,2) Instability indices showing the deterioration of the beverages containing emulsions A to D (different produĐt defeĐtsͿ over a storage period of 50 days (accelerated) and 180 days (real-time storage), respectively. To compare the efficiency of the ASLTs, exponential functions were fitted to the measured values, which allow calculation of the accelerating factors of the ASLTs against the real-time storage. Particle size distribution of the beverages with the four emulsions A to D directly after preparation (left) and after storage under accelerating conditions (right). 50 days storage under accelerating storage conditions: (Comparative real-time storage: 180 d at 20 °C) Before storage After storage EnhanĐing physiĐal instaďilities ďy integrating artifiĐial „produĐt defeĐts“: Agitation 20 °C, 120 min -1 Light box 40 °C, 5000 Lx Thermostat cabinet, 40 °C Instability- mechanism [1,4] A) Reference emulsion 8.2 9.1 7.9 (Diffusion) B) Reduced Ester Gum 7.7 5.8 6.5 Ostwald Ripening C) Low Homog. Pressure 11.0 9.1 9.6 Creaming D) Reduced Emulsifier 9.2 8.7 7.9 (Diffusion) The examined ASLTs are capable of accelerating the physical deterioration of emulsion- based beverages remarkably. Accelerating factors of 5.8 up to 11.0 were achieved regardless of the predominant instability mechanism. Surprisingly, the periodic agitation without elevated temperatures reveal the highest acceleration. Unfortunately, agitation exhibits large deviations in the resulting extent of instability compared to real-time storage. Considering all intrinsic deficiencies of the emulsion beverages, the warm storage with additional illuminance shows the deterioration most similar to the real-time storage. Since the differences in time are not extreme this test condition reveals as most promising. It is thus obvious that the results cannot be easily transferred to other emulsion formula- tions. Nevertheless, for practical purposes the results of the presented work can serve as a basis for the development and assessment of accelerated shelf-life tests. Lab-shaker Light box: 5000 Lx, 40 °C Thermostat cabinet: 40 °C 12 h·d -1 at120 min -1 6500 K daylight lamps dark Physical stability was analyzed with: - Turbidity measurement (Optek): direct analyzing of scattered light in the bottle - Particle size measurement (Malvern): laser diffraction - Calculation of instability index: InstaďilitLJ indedž = 1 turďiditLJ τ;tͿ initial turbidiy τ 0 Physical stability problems Despite the use of stabilizing ingredients and in- tensive mechanical forces like high-pressure homogenization, physical instability phenomena are a great issue: CreaŵiŶg ;RiŶgiŶgͿ Turbidity Loss Sedimentation Inhomogeneity The reason is the inherent instability of beverage emulsions as generally known from macroemul- sions. In addition, governmental regulations restrict the application of stabilizers. Visible ringing of an orange soft drink Reference Emulsion Reduced Ester Gum Low Homogenization Pressure Reduced Emulsifier Storage time [d] Storage time [d] Storage time [d] Storage time [d] Instability index [-] Instability index [-] Instability index [-] Instability index [-] dark agitation Accelerating factors of the ASLTs Acknowledgements: This work was funded under the program FHprofUnt (FKZ: 03FH037PX3) by the Federal Ministry of Education and Research (BMBF) of the German Government.
Transcript
Page 1: Comparative study of accelerated shelf-life tests on ... · PDF fileweighted flavor emulsions Conclusion ... (2014): Beverage emulsions: Recent developments in formulation, production,

Accelerating Shelf-life Tests (ASLT)

New formulations always have to be analyzed in terms of physical stability beside

chemical and sensory evaluation leading to time-consuming development processes. The

industry consequently employs ASLTs to accelerate these changes. In difference to beer a

systematic approach to evaluate the effect of artificial storage conditions for rapid tests in

emulsion based beverages is not available yet. Therefore, different tests were compared in

regard to physical changes of beverages with orange oil emulsion.

C) Low Homog. Pressure

12 % Emulsifier (OSA-starch)

6 % Orange oil6 % Weighting agent

HP-homogenization:

1x 250/50 bar

x90= 5710 nm

Comparative study of accelerated shelf-life tests on physical ageing of beverages containing

weighted flavor emulsions

Conclusion

Motivation

Sören Rossmann, Verena Wolff, Ulrich Müller, Jan Schneider

North Rhine Westfalia Institute of Food Technology ILT.NRW, Lemgo, Germany

References

www.ilt-nrw.de

[1] Piorkowski, D. T. and McClements, D. J. (2014): Beverage emulsions: Recent developments in formulation, production, and applications, Food Hydrocolloids, 42.

[2] Tan, C.-T.: Beverage Emulsions, in Friberg, S. E. and Larsson, K. (Eds.)(1997): Food emulsions, 3. ed., rev. and expanded, Dekker, New York.

[3] Reiner, S. J.; Reineccius, G. A. and Peppard, T. L. (2010): A Comparison of the Stability of Beverage Cloud Emulsions Formulated with Different Gum Acacia- and Starch-

Based Emulsifiers, Journal of Food Science, 75,5.

[4] Lim, S. S.; Baik, M. Y.; Decker, E. A.; Henson, L.; Michael Popplewell, L.; McClements, D. J. (2011): Stabilization of orange oil-in-water emulsions: A new role for ester gum

as an Ostwald ripening inhibitor, Food Chemistry, 128,4.

Results

ContactILT.NRW

Beverage Technology

Sören Rossmann

[email protected]

Emulsion based beverages

Beverage emulsions are an important product for the preparation of increasingly popular

beer-based mixed drinks and soft drinks in order to incorporate water insoluble colors or

flavors (flavor emulsion), to generate turbidity (cloud emulsion) or both combined [1].

Compared to other oil-in-water food emulsions, beverage emulsions are a unique class of

type, as they are highly concentrated semi-finished products and after being processed in-

to drinks finally consumed considerably diluted [2].

Experimental Setup

A) Reference Emulsion

12 % Emulsifier (OSA-starch)

6 % Orange oil6 % Weighting agent

HP-homogenization:

2x 300/50 bar

B) Reduced Ester Gum

12 % Emulsifier (OSA-starch)

10 % Orange oil2 % Weighting Agent

HP-homogenization:

2x 300/50 bar

x90= 736 nm x90= 620 nm

D) Reduced Emulsifier

6 % Emulsifier (OSA-starch)

6 % Orange oil6 % Weighting agent

HP-homogenization:

2x 300/50 bar

x90= 785 nm

Emulsions A to D were diluted to Ready-to-drink beverages for stability analyzing:

0,12 % emulsion diluted with beverage base (10 °Bx sucrose, pH 3,2)

Instability indices showing the deterioration of the beverages containing emulsions A to D

(different produ t defe ts over a storage period of 50 days (accelerated) and 180 days

(real-time storage), respectively. To compare the efficiency of the ASLTs, exponential

functions were fitted to the measured values, which allow calculation of the accelerating

factors of the ASLTs against the real-time storage.

Particle size distribution of the beverages with the four emulsions A to D directly after

preparation (left) and after storage under accelerating conditions (right).

50 days storage under accelerating storage conditions:

(Comparative real-time storage: 180 d at 20 °C)

Before storage After storage

Enhan ing physi al insta ilities y integrating artifi ial „produ t defe ts“:

Agitation

20 °C, 120 min-1

Light box

40 °C, 5000 Lx

Thermostat

cabinet, 40 °C

Instability-

mechanism [1,4]

A) Reference emulsion 8.2 9.1 7.9 (Diffusion)

B) Reduced Ester Gum 7.7 5.8 6.5 Ostwald Ripening

C) Low Homog. Pressure 11.0 9.1 9.6 Creaming

D) Reduced Emulsifier 9.2 8.7 7.9 (Diffusion)

The examined ASLTs are capable of accelerating the physical deterioration of emulsion-

based beverages remarkably. Accelerating factors of 5.8 up to 11.0 were achieved

regardless of the predominant instability mechanism. Surprisingly, the periodic agitation

without elevated temperatures reveal the highest acceleration. Unfortunately, agitation

exhibits large deviations in the resulting extent of instability compared to real-time

storage. Considering all intrinsic deficiencies of the emulsion beverages, the warm storage

with additional illuminance shows the deterioration most similar to the real-time storage.

Since the differences in time are not extreme this test condition reveals as most

promising.

It is thus obvious that the results cannot be easily transferred to other emulsion formula-

tions. Nevertheless, for practical purposes the results of the presented work can serve as a

basis for the development and assessment of accelerated shelf-life tests.

Lab-shaker Light box: 5000 Lx, 40 °C Thermostat cabinet: 40 °C

12 h·d-1 at120 min-1 6500 K daylight lamps dark

Physical stability was analyzed with:

- Turbidity measurement (Optek):

direct analyzing of scattered light in the bottle

- Particle size measurement (Malvern):

laser diffraction

- Calculation of instability index:

Insta ilit inde = 1− tur idit τ tinitial turbidiy τ0

Physical stability problems

Despite the use of stabilizing ingredients and in-

tensive mechanical forces like high-pressure

homogenization, physical instability phenomena

are a great issue:

Crea i g Ri gi g Turbidity Loss

Sedimentation Inhomogeneity

The reason is the inherent instability of beverage

emulsions as generally known from macroemul-

sions. In addition, governmental regulations

restrict the application of stabilizers. Visible ringing of an orange soft drink

Reference Emulsion Reduced Ester Gum

Low Homogenization Pressure Reduced Emulsifier

Storage time [d]

Storage time [d]Storage time [d]

Storage time [d]

Inst

ab

ilit

yin

de

x[-

]In

sta

bil

ity

ind

ex

[-]

Inst

ab

ilit

yin

de

x[-

]In

sta

bil

ity

ind

ex

[-]

dark agitation

Accelerating factors of the ASLTs

Acknowledgements: This work was funded under the program FHprofUnt (FKZ: 03FH037PX3)

by the Federal Ministry of Education and Research (BMBF) of the German Government.

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