evolution of gc in india - past , pressent and future ver 2

7/26/2019 Evolution of GC in India - Past , Pressent and Future Ver 2

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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


2/31

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


3/31

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


4/31

Comparison of Flavor Sample Vs Reference


5/31

Comparison of Flavor Sample Vs Reference


6/31

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



4 Batch 1Middle-1 0.77



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


8/31

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


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


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


15/31

Quantification - SIM Mode

Scan

SIM


16/31

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


17/31

Olfactory GC in Creation R&D

Professional tester analyzing an aroma extract by GC/O


18/31

Olfactory GC in Creation R&D

The principle of flavor analysis by gas

chromatography-olfactometry, in combination with

gas chromatography mass spectrometry.


19/31

Odorants and Odor receptors

Nobel Prize in Medicine 2004


20/31

FlavoLogic uses aroma profiles for quality control of coffee


21/31

Fast GC


22/31

Fast GC

Foods, Flavors, and Fragrances

Note that, in addition to the

significant gains in speed,

resolution was well

Maintained throughout theMethod Translation process.


23/31

Capillary Flow TechnologyBackflush


24/31



25/31



26/31

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


27/31

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


28/31

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


29/31

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


30/31

Lemon Oil Chiral GC


31/31

Chiral GC - Applications

evolution of gc in india - past , pressent and future ver 2

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