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November 24, 2012
Application of GC in Flavors and Fragrances
Dr. K. R.Swaminathan
International Flavor & Fragrances India Private Ltd, Chennai
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GC Flavor and Fragrance Industry
Identification & quantification
Process control and monitoring
Quality control and detection of non permittedmaterials
Product Development
Shelf life stability studies
Investigation of sensory complaints in end products
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GCQualitative Tool
Peak to peak comparison of the chromatograms of the
sample with reference
Missing Peak? Or Missed addition
Extra Peak? Or Wrong addition
Over Addition?
Cross Contamination
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Comparison of Flavor Sample Vs Reference
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Comparison of Flavor Sample Vs Reference
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Determination of % Dose of
Flavored Tea
S.N
oSample ID
% of Flavor Intensity in
bergamot Tea w.r.t Linalyl
Acetate
1 Batch 1Bottom-1 0.21
2 Batch 1Bottom-2 0.21
3 Batch 1Bottom-3 0.21
4 Batch 1Middle-1 0.77
5 Batch 1Middle-2 0.79
6 Batch 1Middle-3 0.84
Marker Quantification in Lab
blended Flavoured Tea Sample
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0
2000
4000
6000
8000
10000
12000
14000
16000
0 10 20 30 40 50 60
Area(pA*sec)
RT (min)
S1S2S3
Flavoured Tea Analysis
Different marker compounds eluting at different RT in three varieties of tea
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0
1000000
2000000
3000000
4000000
5000000
6000000
0 h 1 h 2 h 3 h
AreaCount
Time
Area count of p-Mentha 1,3 dien-7-al
Series1
20000000
30000000
40000000
50000000
60000000
0 h 1 h 2 h 3 h
Areacount
Time
Area count of Cuminal plus Carvone
Area
6000000
6500000
7000000
7500000
8000000
8500000
9000000
0 h 1 h 2 h 3 h
Areacount
Time
Area count of gamma Terpinene
Area count
5000000
5200000
5400000
5600000
5800000
6000000
6200000
6400000
6600000
6800000
0 h 1 h 2 h 3 h
Areacount
Time
Area count of Limonene plus para cymene
Area count
GCMS headspace analysis of Roasted cumin flavour
Application time sample
Measurement as a function of Application time
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0
50000
100000
150000
200000
250000
300000
0 2 4 6 8
Areacount
weeks
Area count of Cinnamaldehyde
PCSF+ PCSF+ control PCSF
0
50000
100000
150000
200000
250000
300000
0 2 4 6 8
Areacount
Weeks
Area count of Anethole
PCSF+ PCSF+ control PCSF
0
2000000
4000000
6000000
8000000
0 2 4 6 8
Areacount
Weeks
Area count of Cuminal and Carvone
PCSF+ PCSF+ control PCSF PCS
0
100000
200000
300000
0 2 4 6 8
Areacount
Weeks
Area count of Dihydrocarvone
PCSF+ PCSF+ control PCSF
Shelf Life Study of Savoury product
( seasoning plus liquid top note)
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min10 20 30 40
pA
0
10
20
30
40
50
60
70
80
FID1 A, (D:\CHEM32\1\TEMP\ECMEXPORT\2362-000007.D)
3.3
26
3.4
79
3.7
47
4.1
27
4.2
01
5.1
96
9.3
38
9.6
41
10.1
47
10.9
18
11.1
56
11.4
52
12.0
67
12.5
34
12.8
36
13.4
43
16.2
53
17.3
24
18.0
12
min10 20 30 40
pA
0
10
20
30
40
50
60
70
80
FID1 A, (D:\CHEM32\1\TEMP\ECMEXPORT\2362-000010.D)
3.3
23
3.4
76
3.7
15
4.1
23
9.3
28
9.6
35
10.1
36
11.1
43
11.4
40
12.0
46
12.1
58
12.5
13
12.8
01
13.2
36
Chromatographic profiling of Powder blends
Sample
Gold
Standard
Significant intensity and peak differences in 8-20 min region.
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Detection of Trace Contaminants
Toluene in Flavor Samples
Diethyl Phthalate in Flavor & Fragrance Sample
BHA & BHT in Flavor & Fragrance Sample
Residual Solvents in in Flavor & Fragrance Raw
Material Sample
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Diethyl phthalate in Fragrance Raw Material
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Detection of Trace Contaminants
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Residual Solvents
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Quantification - SIM Mode
Scan
SIM
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Gas Chromatography Olfactometry
Multidimensional GC System
Complete software control
Capillary Flow Technology
Integrated cold trap system
Cooled Injection System CIS
MACH/Agilent LTM Olfactory Detection Port - ODP
Preparative Fraction Collector - PFC
Multi Purpose Sampler - MPS
Thermal Desorption System - TDS
Twister Desorption System - TDU
Agilent Technologies GC/MSD
Olfactory Detector Port allows the sensing of compounds by the human nose
as they elute from the column of a gas chromatograph. The effluent is split as
it leaves the column so that it arrives simultaneously at the nose and at
another detector such as a mass spectrometer
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Olfactory GC in Creation R&D
Professional tester analyzing an aroma extract by GC/O
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Olfactory GC in Creation R&D
The principle of flavor analysis by gas
chromatography-olfactometry, in combination with
gas chromatography mass spectrometry.
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Odorants and Odor receptors
Nobel Prize in Medicine 2004
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FlavoLogic uses aroma profiles for quality control of coffee
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Fast GC
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Fast GC
Foods, Flavors, and Fragrances
Note that, in addition to the
significant gains in speed,
resolution was well
Maintained throughout theMethod Translation process.
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Capillary Flow TechnologyBackflush
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Capillary Flow TechnologyBackflush
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Capillary Flow TechnologyBackflush
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2D GC / GC X GC
Use of two columns to resolve a sample
Current column technology is very near the theoretical limit
However, it is still not possible to resolve all components in acomplex mixture
Basic assumption is that no column can resolve all components
of interest
Coupling two columns can help achieve complex separations
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2D - GC
In GCGC we usually couple a long 1D column directly to a short
2D column (or a regular elution column to a fast elution column)
As examples of generic GCGC applications,
a low polarity (5% phenyl) column coupled with a short polar
(wax phase) column is useful for essential oils
Sensitivity coupled with specificity
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2D - GC
Tobacco smoke: over 1000 peaks identified, each actually
contains 2 or more components
PCBs: 207 species but only about 180 resolved
Coffee: over 600 components identified
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Chiral Separations
Enantiomers have
Identical volatility
and
Identical polarity
Need for a stationary phase that would be able to distinguish enantiomeric species
MP cannot separate them
Usual SP cannot separate them
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Lemon Oil Chiral GC
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Chiral GC - Applications