1
Authenticity testing of toddy (“Palm Wine”) using GC Ramanah G, Mala SMVD, Seniveratne MEJ Government Analyst’s Department,31, Isuru Mawatha,Pelawatta, Battaramulla,Rajagiriya, Sri Lanka. Introduction Statistical Package for the Social Sciences (SPSS) based on GC-FID data Materials and Methods Toddy Tapper with equipment Samples of toddy received by the Government Analyst Department from different areas and fermented sugar solution were categorized into four different groups. 1. Genuine toddy samples received from Excise Department designate G 2. Market toddy samples designate MMT 3. Toddy samples received from low courts designate CL 4. Sugar solution fermented Liquor samples prepared in lab (artificial toddy) designate A. Method of preparation fermented liquor in lab GC Conditions Statistic and chemo metric analysis Results and discussion 16% w/v sugar solution+ Baker’s Yeast FermentedLiquors A and B Mixture of a portion of genuine palm FermentedLiquors X,Y,Z Sap+ 3 Portion of 16% w/v sugar Solution+ Baker’s Yeast Distill 25.0 ml of each sample Collect 25.0 ml distillate Inject 0.5μl distillate to GC (Shimadzu 2010 plus) Column: RTX 624 (30m*0.32mm,1.8μm) Carrier gas: Nitrogen Oven: Temperature Program o 400C-3min o 100C/min to 2000C o 2000C -1min Total run time: 20 minutes Inlet: 2500c,Split 20:1 Sample Volume- 0.5 μl Detector FID: Temperature 2600c Based on GC-FID spectra and retention time and area recorded in the domain 0-13minutes, the chemo metric analysis was performed. By unsupervised method using IBM SPSS Statistics 20 the variability and discrimination between samples was made. Volatile Organic compounds Acetaldehyde, Ethanol, n Propanol, Ethyl acetate , Iso Butanol, Acetic acid, Iso Amyl alcohol were identified in both, the toddy sample and fermented sugar solution. There was a peak at retention time of 12.06 minutes in genuine toddy, which was absent in fermented sugar solution. Area ratios of different peaks were compared to find the authenticity or adulteration of toddy. A considerable difference was observed between genuine toddy and fermented sugar solution with nPropanol/iso Amyl alcohol peaks ratio. The relevant data is not shown. The multivariate analysis of IBM SPSS Statistics based on the fingerprint of GC-FID spectra of secondary derivative with in RT 0-13 minutes was carried out to discriminate the toddy samples according to prepara- tion method. This linkage shows three different clusters of data points (samples).Genuine toddy and market toddy were in group 1 and fermented sugar solution and toddy received from courts were in group 2 and other two samples from courts were in group 3. Further it shows group 1 and group 2 are siginificantly different from each other and group 3 is highly different from other two groups. Acknowledgement Authors would like to thank Government Analyst Mrs. S.Tennakoon and Additional Government Analyst Mr. A. Welianga for their support and advice, Excise Commissioner General and staff of Excise Department for providing the genuine toddy samples and unfermented sap, and Dr Samantha Weerasinghe , Depar- mant of Chemistry, University of Colombo and Dr. Champa Magolla, Department of Computer Science, University of Colombo for Statistical Analysis. References 1 Analyzing Alcohoic beverages by gas chromatograph (www.restek.com) 2 Physico chemical properties of fresh and stored coconot palm toddy (Singaravel.K, Alagusundaram.K, Hariharan.B) 3 Impurties in white sugar. (J.A.Amber and Byali,Bureau of chemistry and solis,Washigton,D.C. 4 Chemical composition changes of post-harvest coconut inflorescnce sap during natural fermentation (Qiuyu Xia,Rui Li,Songlin Zhao,Weijun Chen, Hua Chen, Bo Xin, Yulin Huang and Minmin Tang African Jou- ranal of biotechnology vol. 10(66), 26 october 2011 5 Toddy: Authentic or Adulterated, How Do We Know? C.S.Ranasinghe and W P K K Fernando Coconut Re- search Institute Lunuwila,Sri Lanka 6 A Rapid method for determination of ethanol in alcoholic beverages using capillary Gas Chromatography Mei-Ling Wang, Young-Meng Choong, Nan-Wei Su and Min-Hsiung Lee Journal of food and Drug Analysis Vol 11,No 2 2003 7 Authenticity Testing of Liquor Samples using LC-MS/MS and Statstical data processing Andre Shreiber Christober Borton and Anna Marques 8 Discrimination of cognacs and other distilled drinks by Mi- Infrared Spectroscopy Daniel Piceque.Pascale Liben,Georges corrieu Roger Cantagrel, Odile Lablanquie, and Guilaume Snakkers J.Agric.Food Chem,2006, 54 (15) 9 Rapid quantitative Analysis of ethanol and prediction of methanol content in Traditional fruit Brandies from Romania, using FTIR Spectroscopy and Chemometrics Teodora Emilia COLDEA, Carmen SOCACIU,Flo- rinela FETEA,Floricuta RANGA, Raluca Maria POP,Mira FLOREA 10 Agilent J& W DB-624 Ultra inert Capillary Column Screens Distilled Sprits by GC/MS Static Headspace Toddy (Palm Wine) is sweetish, heavy, milky white and vigorously effervescent alcoholic beverage.Toddy has a special place in traditional celebrations and ceremonies. Tapper applying cinnamon paste The coconut sap, an exudate obtained by ‘tapping’ the unopened inflores- cence of the coconut palm, is the major material used in the manufacture of alcoholic beverages in Sri Lanka. The sap is traditionally collected in earthen- ware pots and allowed to ferment in open pots for varying lengths of time. During this period, microorganisms from the atmosphere contaminate, multi- ply in the sugary liquid and finally transform the raw material into various products; mainly ethanol.The resulting solution contains about 7 percent (v/v) ethyl alcohol. It can either be consumed directly as toddy or distilled and aged in an indigenous tree species barrel of Oak or Halmilla(Berrayacordifolia), called arrack. Distillers usually obtain toddy from contractors and they are paid on the con- tent of pure toddy. There have been several complaints with respect to adulter- ated toddy received from contractors as artificial toddy canbe made by the fer- mentation of sugar solution. Therefore, the problem of adulterated toddy has to be solved and necessary steps have to be taken to prevent such sub-standard toddy entering the market. Solving this problem is a big challenge as sap and added sugar both contain sucrose which undergoes fermentation. Hence calcu- lation of exogenous sugar percent in toddy is difficult. Genuine Toddy Fermented Sugar Solution

Ramanah G, Mala SMVD, Seniveratne MEJ€¦ · Hariharan.B) 3 Impurties in white sugar. (J.A.Amber and Byali,Bureau of chemistry and solis,Washigton,D.C. 4 Chemical composition changes

  • Upload
    others

  • View
    1

  • Download
    0

Embed Size (px)

Citation preview

Page 1: Ramanah G, Mala SMVD, Seniveratne MEJ€¦ · Hariharan.B) 3 Impurties in white sugar. (J.A.Amber and Byali,Bureau of chemistry and solis,Washigton,D.C. 4 Chemical composition changes

Authenticity testing of toddy (“Palm Wine”) using GCRamanah G, Mala SMVD, Seniveratne MEJGovernment Analyst’s Department,31, Isuru Mawatha,Pelawatta,

Battaramulla,Rajagiriya, Sri Lanka.

Introduction

Statistical Package for the Social Sciences (SPSS) based on GC-FID data

Materials and Methods

Toddy

Tapper with equipment

Samples of toddy received by the Government Analyst Department from di�erent areas and fermented sugar solution were categorized into four di�erent groups. 1. Genuine toddy samples received from Excise Department designate G 2. Market toddy samples designate MMT 3. Toddy samples received from low courts designate CL 4. Sugar solution fermented Liquor samples prepared in lab (arti�cial toddy) designate A.

Method of preparation fermented liquor in lab

GC Conditions

Statistic and chemo metric analysis

Results and discussion

16% w/v sugar solution+ Baker’s Yeast FermentedLiquors A and B

Mixture of a portion of genuine palm FermentedLiquors X,Y,ZSap+ 3 Portion of 16% w/v sugarSolution+ Baker’s Yeast

Distill25.0 ml of each sample

Collect25.0 ml distillate

Inject 0.5µl distillate to GC (Shimadzu 2010 plus)

Column: RTX 624 (30m*0.32mm,1.8µm)Carrier gas: NitrogenOven: Temperature Program o 400C-3min o 100C/min to 2000C o 2000C -1minTotal run time: 20 minutesInlet: 2500c,Split 20:1Sample Volume- 0.5 µlDetectorFID: Temperature 2600c

Based on GC-FID spectra and retention time and area recorded in the domain 0-13minutes, the chemo metric analysis was performed. By unsupervised method using IBM SPSS Statistics 20 the variability and discrimination between samples was made.

Volatile Organic compounds Acetaldehyde, Ethanol, n Propanol, Ethyl acetate , Iso Butanol, Acetic acid, Iso Amyl alcohol were identi�ed in both, the toddy sample and fermented sugar solution. There was a peak at retention time of 12.06 minutes in genuine toddy, which was absent in fermented sugar solution. Area ratios of di�erent peaks were compared to �nd the authenticity or adulteration of toddy. A considerable di�erence was observed between genuine toddy and fermented sugar solution with nPropanol/iso Amyl alcohol peaks ratio. The relevant data is not shown.

The multivariate analysis of IBM SPSS Statistics based on the �ngerprint of GC-FID spectra of secondary derivative with in RT 0-13 minutes was carried out to discriminate the toddy samples according to prepara-tion method.

This linkage shows three di�erent clusters of data points (samples).Genuine toddy and market toddy were in group 1 and fermented sugar solution and toddy received from courts were in group 2 and other two samples from courts were in group 3. Further it shows group 1 and group 2 are sigini�cantly di�erent from each other and group 3 is highly di�erent from other two groups.

Acknowledgement

Authors would like to thank Government Analyst Mrs. S.Tennakoon and Additional Government Analyst Mr. A. Welianga for their support and advice, Excise Commissioner General and sta� of Excise Department for providing the genuine toddy samples and unfermented sap, and Dr Samantha Weerasinghe , Depar-mant of Chemistry, University of Colombo and Dr. Champa Magolla, Department of Computer Science, University of Colombo for Statistical Analysis.

References

1 Analyzing Alcohoic beverages by gas chromatograph (www.restek.com)2 Physico chemical properties of fresh and stored coconot palm toddy (Singaravel.K, Alagusundaram.K, Hariharan.B)3 Impurties in white sugar. (J.A.Amber and Byali,Bureau of chemistry and solis,Washigton,D.C.4 Chemical composition changes of post-harvest coconut in�orescnce sap during natural fermentation (Qiuyu Xia,Rui Li,Songlin Zhao,Weijun Chen, Hua Chen, Bo Xin, Yulin Huang and Minmin Tang African Jou-ranal of biotechnology vol. 10(66), 26 october 20115 Toddy: Authentic or Adulterated, How Do We Know? C.S.Ranasinghe and W P K K Fernando Coconut Re-search Institute Lunuwila,Sri Lanka6 A Rapid method for determination of ethanol in alcoholic beverages using capillary Gas Chromatography Mei-Ling Wang, Young-Meng Choong, Nan-Wei Su and Min-Hsiung Lee Journal of food and Drug Analysis Vol 11,No 2 20037 Authenticity Testing of Liquor Samples using LC-MS/MS and Statstical data processing Andre Shreiber Christober Borton and Anna Marques8 Discrimination of cognacs and other distilled drinks by Mi- Infrared Spectroscopy Daniel Piceque.Pascale Liben,Georges corrieu Roger Cantagrel, Odile Lablanquie, and Guilaume Snakkers J.Agric.Food Chem,2006, 54 (15)9 Rapid quantitative Analysis of ethanol and prediction of methanol content in Traditional fruit Brandies from Romania, using FTIR Spectroscopy and Chemometrics Teodora Emilia COLDEA, Carmen SOCACIU,Flo-rinela FETEA,Floricuta RANGA, Raluca Maria POP,Mira FLOREA10 Agilent J& W DB-624 Ultra inert Capillary Column Screens Distilled Sprits by GC/MS Static Headspace

Toddy (Palm Wine) is sweetish, heavy, milky white and vigorously e�ervescent alcoholic beverage.Toddy has a special place in traditional celebrations and ceremonies.

Tapper applyingcinnamon paste

The coconut sap, an exudate obtained by ‘tapping’ the unopened in�ores-cence of the coconut palm, is the major material used in the manufacture of alcoholic beverages in Sri Lanka. The sap is traditionally collected in earthen-ware pots and allowed to ferment in open pots for varying lengths of time. During this period, microorganisms from the atmosphere contaminate, multi-ply in the sugary liquid and �nally transform the raw material into various products; mainly ethanol.The resulting solution contains about 7 percent (v/v) ethyl alcohol. It can either be consumed directly as toddy or distilled and aged in an indigenous tree species barrel of Oak or Halmilla(Berrayacordifolia), called arrack.

Distillers usually obtain toddy from contractors and they are paid on the con-tent of pure toddy. There have been several complaints with respect to adulter-ated toddy received from contractors as arti�cial toddy canbe made by the fer-mentation of sugar solution. Therefore, the problem of adulterated toddy has to be solved and necessary steps have to be taken to prevent such sub-standard toddy entering the market. Solving this problem is a big challenge as sap and added sugar both contain sucrose which undergoes fermentation. Hence calcu-lation of exogenous sugar percent in toddy is di�cult.

Genuine Toddy

FermentedSugar Solution