A novel approach to assess the quality and authenticity of Scotch Whisky based on gas chromatography coupled to high resolution mass spectrometry

Similar documents
Profiling of Aroma Components in Wine Using a Novel Hybrid GC/MS/MS System

Identification of Adulteration or origins of whisky and alcohol with the Electronic Nose

CHAPTER 8. Sample Laboratory Experiments

Somchai Rice 1, Jacek A. Koziel 1, Anne Fennell 2 1

Journal of Chemical and Pharmaceutical Research, 2017, 9(9): Research Article

One class classification based authentication of peanut oils by fatty

Analytical Report. Volatile Organic Compounds Profile by GC-MS in Cupcake Batter Flavor Concentrate

ADVANCED BEER AROMA ANALYSIS. Erich Leitner TU Graz, Institute of Analytical Chemistry and Food Chemistry, Graz, Austria

Analytical Report. Volatile Organic Compounds Profile by GC-MS in Clove E-liquid Flavor Concentrate. PO Box 2624 Woodinville, WA 98072

Analytical Report. Table 1: Target compound levels. Concentration units are ppm or N/D, not detected.

Comprehensive analysis of coffee bean extracts by GC GC TOF MS

Somchai Rice 1, Jacek A. Koziel 1, Jennie Savits 2,3, Murlidhar Dharmadhikari 2,3 1 Agricultural and Biosystems Engineering, Iowa State University

High resolution mass approaches for wine and oenological products analysis

Analytical Method for Coumaphos (Targeted to agricultural, animal and fishery products)

Metabolomic Profiling of Wines using LC/QTOF MS and MassHunter Data Mining and Statistical Tools

Analytical Traceability of Food and Feed

Determination of Caffeine in Coffee Products According to DIN 20481

Determination of Pesticides in Coffee with QuEChERS Extraction and Silica Gel SPE Cleanup

RESOLUTION OIV-OENO ANALYSIS OF VOLATILE COMPOUNDS IN WINES BY GAS CHROMATOGRAPHY

AppNote 2/2003. Wine Discrimination using a Mass Spectral Based Chemical Sensor KEYWORDS ABSTRACT

Solid Phase Micro Extraction of Flavor Compounds in Beer

GAS-CHROMATOGRAPHIC ANALYSIS OF SOME VOLATILE CONGENERS IN DIFFERENT TYPES OF STRONG ALCOHOLIC FRUIT SPIRITS

Analysis of Volatile Compounds of Jasminum nitidum [Acc.JN.1] Flowers

Fast Analysis of Smoke Taint Compounds in Wine with an Agilent J&W DB-HeavyWax GC Column

AppNote 4/2003. Fast Analysis of Beverages using a Mass Spectral Based Chemical Sensor KEYWORDS ABSTRACT

Application Note: Analysis of Melamine in Milk (updated: 04/17/09) Product: DPX-CX (1 ml or 5 ml) Page 1 of 5 INTRODUCTION

Analysis of Volatile Compounds from the Concrete of Jasminum multiflorum Flowers

Table 1: Experimental conditions for the instrument acquisition method

ADVANCED ANALYTICAL SENSORY CORRELATION TOWARDS A BETTER MOLECULAR UNDERSTANDING OF COFFEE FLAVOUR

The Good and the Bad Influence of. Polyfunctional Thiols in Beer Hops. Grapefruit or a Cat Box? Application Scientist: Matthew Curtis

Jana Hajšlová, Milena Zachariasova and Monika Tomaniova

Extraction of Acrylamide from Coffee Using ISOLUTE. SLE+ Prior to LC-MS/MS Analysis

16th International CEEPUS Symposium and Summer School on Bioanalysis, Warsaw, Poland, July 06-12, 2016

Identification and Semiquantitation of Monoterpene Glycosides in Ripening Muscat of Alexandria Grapes

TSKgel TECHNICAL INFORMATION SHEET No. 131

Determination of Methylcafestol in Roasted Coffee Products According to DIN 10779

Determination of Ochratoxin A in Roasted Coffee According to DIN EN 14132

Agilent J&W DB-624 Ultra Inert Capillary Column Screens Distilled Spirits by GC/MS Static Headspace

Tyler Trent, SVOC Application Specialist; Teledyne Tekmar P a g e 1

Solid Phase Micro Extraction of Flavor Compounds in Beer

Analytical Strategies to Confirm the Generic Authenticity of Scotch Whisky

Increasing Toast Character in French Oak Profiles

Organic Chemistry 211 Laboratory Gas Chromatography

PECTINASE Product Code: P129

AppNote 1/2003. Fast Analysis of Food and Beverage Products using a Mass Spectrometry Based Chemical Sensor KEYWORDS ABSTRACT

Determination of the concentration of caffeine, theobromine, and gallic acid in commercial tea samples

Rapid Analysis of Soft Drinks Using the ACQUITY UPLC H-Class System with the Waters Beverage Analysis Kit

Profiling and Identification of Hop-Derived Bitter Compounds in Beer Using LC-MS/MS

Bromine Containing Fumigants Determined as Total Inorganic Bromide

RECENT DEVELOPMENTS IN FOOD SCREENING BY NMR. Claudia Napoli Bruker Italia

Effects of Adulteration Technique on the NIR Detection of Melamine in Milk Powder

The Benefits of GC/MS Coupled with a Headspace Trap to Monitor Volatile Organic Compounds in the Production of Beer

The MacAllan Amber NZ Double (30ml) $19

The Determination of Pesticides in Wine

Chemosystematic Study of Diterpenoids in Green Coffee Beans

AppNote 13/2002. Classifi cation of Coffees from Different Origins by Chemical Sensor Technology INTRODUCTION

Comes from the term Water of Life. Eau-De-Vie Aqua Vitae Alkol Usquebagh

Determination of natamycin in wines Résolution OIV-SCMA

Frontiers in Food Allergy and Allergen Risk Assessment and Management. 19 April 2018, Madrid

Dr. Bert Popping

Investigating the factors influencing hop aroma in beer

INTERNATIONAL STANDARD

Flavourings Legislation and Safety Assessment

[ application note note ] ]

Investigation of Volatile Compounds from the Concrete of Jasminum auriculatum Flowers

OenoFoss. Instant quality control throughout the winemaking process. Dedicated Analytical Solutions

Institute of Food Research. Ian Colquhoun

Adding water to Single Malt Whisky

Supplementary Material

Rapid Tea Analysis on Poroshell 120 SB-C18 with LC/MS

Emerging Applications

Whisky pricing: A dram good case study. Anirudh Kashyap General Assembly 12/22/2017 Capstone Project The Whisky Exchange

Life Science and Chemical Analysis Solutions. Key Words: GCxGC-TOFMS, SPME, Food and Flavors. LECO Corporation; Saint Joseph, Michigan USA

Flavour release and perception in reformulated foods

Experiment 6 Thin-Layer Chromatography (TLC)

CHAPTER 8. Sample Laboratory Experiments

5. Supporting documents to be provided by the applicant IMPORTANT DISCLAIMER

Food Safety in Wine: Removal of Ochratoxin a in Contaminated White Wine Using Commercial Fining Agents

AppNote 6/2013. Using TDU-Pyrolysis-GC-MS to Investigate Aged Whiskey Samples and Their Oak Barrels ABSTRACT INTRODUCTION

The Impact of Vineyard Origin and Winery on the Elemental Profile of Red Wines

Samples: Standard solutions of rutin, quercetina, rosmarinic acid, caffeic acid and gallic acid. Commercial teas: Green, Ceilan, Hornimans and Black.

Elemental Analysis of Yixing Tea Pots by Laser Excited Atomic. Fluorescence of Desorbed Plumes (PLEAF) Bruno Y. Cai * and N.H. Cheung Dec.

Characterisation of New Zealand hop character and the impact of yeast strain on hop derived compounds in beer

Application of GC/MS method for the identification of brandies and cognacs

Zoe Grosser, Vinson Leung, Jim Fenster, Brian LaBrecque Horizon Technology, Inc., Salem, NH USA

Qualitative Analysis of Age and Brand of Unblended Brandy by Electronic Nose

PRODUCT INFORMATION PRODUCER SUMMARY

A NEW APPROACH FOR ASSESSING

Influence of climate and variety on the effectiveness of cold maceration. Richard Fennessy Research officer

Flavour Legislation Past Present and Future or From the Stone Age to the Internet Age and Beyond. Joy Hardinge

Wine analysis to check quality and authenticity by fully-automated 1

VINOLOK (VINOSEAL) closure evaluation Stage 1: Fundamental performance assessment

GC/MS BATCH NUMBER: W10104

Food Defense: The Academic Perspective

Smoke Taint Update. Thomas Collins, PhD Washington State University

VQA Ontario. Quality Assurance Processes - Tasting

Quantitative Measurement of Sesquiterpenes in Various Ginger Samples by GC-MS/MS

2nd working meeting of the Regional Expert Advisory Working Group on Wine in South Estern Europe 14/12/ /12/2015, Skopje, Macedonia

Determination of Melamine Residue in Milk Powder and Egg Using Agilent SampliQ Polymer SCX Solid Phase Extraction and the Agilent 1200 Series HPLC/UV

Detecting Melamine Adulteration in Milk Powder

Transcription:

Ensuring the Integrity of the European food chain A novel approach to assess the quality and authenticity of Scotch Whisky based on gas chromatography coupled to high resolution mass spectrometry Michal Stupak, Ian Goodall, Monika Tomaniova, Jana Pulkrabova, Jana Hajslova The role of modern analytical approaches in fighting with food fraud

Scotch Whisky and its adulteration Scotch Whisky Scotch Whisky is made in Scotland from three raw materials: cereals, yeast and water. Compulsory sales descriptions: Single Malt, Single Grain, Blended Malt, Blended Grain and Blended Scotch Whisky. The regional geographical indications: Campbeltown, Islay, Highland, Lowland, and Speyside. The role of modern analytical approaches in fighting with food fraud

Scotch Whisky and its adulteration Scotch Whisky Scotch Whisky is made in Scotland from three raw materials: cereals, yeast and water. Compulsory sales descriptions: Single Malt, Single Grain, Blended Malt, Blended Grain and Blended Scotch Whisky. The regional geographical indications: Campbeltown, Islay, Highland, Lowland, and Speyside. Adulteration of Scotch Whisky Dilution or replacement of Scotch Whisky with a cheaper spirit Shorter period of maturation in oak cask than declared (min three years for whisky) Substituting a low-cost whisky for a more expensive product The role of modern analytical approaches in fighting with food fraud 3

Scotch Whisky and its adulteration Scotch Whisky Scotch Whisky is made in Scotland from three raw materials: cereals, yeast and water. Compulsory sales descriptions: Single Malt, Single Grain, Blended Malt, Blended Grain and Blended Scotch Whisky. The regional geographical indications: Campbeltown, Islay, Highland, Lowland, and Speyside. Adulteration of Scotch Whisky Dilution or replacement of Scotch Whisky with a cheaper spirit Shorter period of maturation in oak cask than declared (min three years for whisky) Substituting a low-cost whisky for a more expensive product Strategy for monitoring of quality, safety and authenticity!!! The role of modern analytical approaches in fighting with food fraud

Aim of study To develop a new non target screening strategy based on GC-QTOF for the fingerprinting of whisky components. Agilent 7b GC-QTOF The role of modern analytical approaches in fighting with food fraud 5

Aim of study To develop a new non target screening strategy based on GC-QTOF for the fingerprinting of whisky components. Samples: Agilent 7b GC-QTOF 18 samples of authentic whiskies (malt and blended) fakes The samples characterised by age, maturation cask(s), level of peating provided by Dr. Ian Goodall (The Scotch Whisky Research Institute) The role of modern analytical approaches in fighting with food fraud 6

Experimental Sample preparation Sample + Ethyl acetate + Water Filtration of ethylacetate fraction using NaSO4 Evaporation Re-dissolve in ethyl acetate The role of modern analytical approaches in fighting with food fraud 7

Experimental Sample preparation Sample + Ethyl acetate + Water Filtration of ethylacetate fraction using NaSO4 Evaporation Re-dissolve in ethyl acetate Instrumental analysis GC system Column: HP-INNOWAX (5m x. mm x. µm) Injected volume: 1 µl Injection: Splitless (5 C) Agilent 7b GC-Q-TOF Oven temperature program: 6 C (1min), C/min to 4 C (8 min) MS system Electron Ioinzation (EI), positive chemical ionization (PCI) Mass range: 5-5 amu Resolution: 13 FWHM The role of modern analytical approaches in fighting with food fraud 8

Experimental Sample preparation Sample + Ethyl acetate + Water Filtration of ethylacetate fraction using NaSO4 Evaporation Re-dissolve in ethyl acetate Instrumental analysis GC system Column: HP-INNOWAX (5m x. mm x. µm) Injected volume: 1 µl Injection: Splitless (5 C) Agilent 7b GC-Q-TOF Oven temperature program: 6 C (1min), C/min to 4 C (8 min) MS system Electron Ioinzation (EI), positive chemical ionization (PCI) Mass range: 5-5 amu Resolution: 13 FWHM Statistical data processing Deconvolution UknowAnalysis (B.8., Agilent Technologies) The role of modern analytical approaches in fighting with food fraud 9

Experimental Sample preparation Sample + Ethyl acetate + Water Filtration of ethylacetate fraction using NaSO4 Evaporation Re-dissolve in ethyl acetate Instrumental analysis GC system Column: HP-INNOWAX (5m x. mm x. µm) Injected volume: 1 µl Injection: Splitless (5 C) Agilent 7b GC-Q-TOF Oven temperature program: 6 C (1min), C/min to 4 C (8 min) MS system Electron Ioinzation (EI), positive chemical ionization (PCI) Mass range: 5-5 amu Resolution: 13 FWHM Statistical data processing Peak Alignment Deconvolution MPP (13., Agilent Technologies) UknowAnalysis (B.8., Agilent Technologies) The role of modern analytical approaches in fighting with food fraud 1

Experimental Sample preparation Sample + Ethyl acetate + Water Filtration of ethylacetate fraction using NaSO4 Evaporation Re-dissolve in ethyl acetate Instrumental analysis GC system Column: HP-INNOWAX (5m x. mm x. µm) Injected volume: 1 µl Injection: Splitless (5 C) Agilent 7b GC-Q-TOF Oven temperature program: 6 C (1min), C/min to 4 C (8 min) MS system Electron Ioinzation (EI), positive chemical ionization (PCI) Mass range: 5-5 amu Resolution: 13 FWHM Statistical data processing Recursive analysis Peak Alignment Deconvolution MassHunter (B.8., Agilent Technologies) MPP (13., Agilent Technologies) UknowAnalysis (B.8., Agilent Technologies) The role of modern analytical approaches in fighting with food fraud 11

Experimental Sample preparation Sample + Ethyl acetate + Water Filtration of ethylacetate fraction using NaSO4 Evaporation Re-dissolve in ethyl acetate Instrumental analysis GC system Column: HP-INNOWAX (5m x. mm x. µm) Injected volume: 1 µl Injection: Splitless (5 C) Agilent 7b GC-Q-TOF Oven temperature program: 6 C (1min), C/min to 4 C (8 min) MS system Electron Ioinzation (EI), positive chemical ionization (PCI) Mass range: 5-5 amu Resolution: 13 FWHM Statistical data processing Normalization Recursive analysis Peak Alignment Deconvolution Microsoft Excel (Microsoft) MassHunter (B.8., Agilent Technologies) MPP (13., Agilent Technologies) UknowAnalysis (B.8., Agilent Technologies) The role of modern analytical approaches in fighting with food fraud 1

Experimental Sample preparation Sample + Ethyl acetate + Water Filtration of ethylacetate fraction using NaSO4 Evaporation Re-dissolve in ethyl acetate Instrumental analysis GC system Column: HP-INNOWAX (5m x. mm x. µm) Injected volume: 1 µl Injection: Splitless (5 C) Agilent 7b GC-Q-TOF Oven temperature program: 6 C (1min), C/min to 4 C (8 min) MS system Electron Ioinzation (EI), positive chemical ionization (PCI) Mass range: 5-5 amu Resolution: 13 FWHM Statistical data processing PCA PLS-DA Normalization Recursive analysis Peak Alignment Deconvolution SIMCA (13..3., UMETRICS) Microsoft Excel (Microsoft) MassHunter (B.8., Agilent Technologies) MPP (13., Agilent Technologies) UknowAnalysis (B.8., Agilent Technologies) The role of modern analytical approaches in fighting with food fraud 13

Experimental Sample preparation Sample + Ethyl acetate + Water Filtration of ethylacetate fraction using NaSO4 Evaporation Re-dissolve in ethyl acetate Instrumental analysis GC system Column: HP-INNOWAX (5m x. mm x. µm) Injected volume: 1 µl Injection: Splitless (5 C) Agilent 7b GC-Q-TOF Oven temperature program: 6 C (1min), C/min to 4 C (8 min) MS system Electron Ioinzation (EI), positive chemical ionization (PCI) Mass range: 5-5 amu Resolution: 13 FWHM Statistical data processing Identification of marker(s) PCA PLS-DA Normalization Recursive analysis Peak Alignment Deconvolution NIST library 17, Exact mass, isotopic pattern, EI*, PCI**, RI*** *electron impact **positive chemical ionization ***retention indexes SIMCA (13..3., UMETRICS) Microsoft Excel (Microsoft) MassHunter (B.8., Agilent Technologies) MPP (13., Agilent Technologies) UknowAnalysis (B.8., Agilent Technologies) The role of modern analytical approaches in fighting with food fraud 14

Which cask(s) were used for the whisky maturation?? The role of modern analytical approaches in fighting with food fraud 15

Classification of whisky differing in cask used in maturation The cask(s) used for maturing and its duration may influence the whisky character All malt whiskies were maturated in oak cask previously used for the bourbon production Some of them were transfered from bourbon cask into the cask used for the maturation of various wine (sherry, port, red and white) The role of modern analytical approaches in fighting with food fraud 16

Classification of whisky differing in cask used in maturation The cask(s) used for maturing and its duration may influence the whisky character All malt whiskies were maturated in oak cask previously used for the bourbon production Some of them were transfered from bourbon cask into the cask used for the maturation of various wine (sherry, port, red and white) 8 x1 Sample aged in bourbon/wine casks 3 1 8 x1 3 Sample aged in bourbon cask 1 4.4 4.8 5. 5.6 6. 6.4 6.8 7. 7.6 8. 8.4 8.8 9. 9.6 1. 1.4 1.8 11. 11.6 The role of modern analytical approaches in fighting with food fraud (min)

Classification of whisky differing in cask used in maturation The cask(s) used for maturing and its duration may influence the whisky character All malt whiskies were maturated in oak cask previously used for the bourbon production Some of them were transfered from bourbon cask into the cask used for the maturation of various wine (sherry, port, red and white) 8 x1 Sample aged in bourbon/wine casks 3 1 8 x1 3 Sample aged in bourbon cask 1 4.4 4.8 5. 5.6 6. 6.4 6.8 7. 7.6 8. 8.4 8.8 9. 9.6 1. 1.4 1.8 11. 11.6 The role of modern analytical approaches in fighting with food fraud (min)

Whisky samples according cask PCA bourbon b cask b bourbon/wine casks Distribution of malt samples aged in different cask(s) PCA. The role of modern analytical approaches in fighting with food fraud 19

Whisky samples according cask PCA PLS-DA bourbon b cask b bourbon/wine casks bourbon b cask bourbon/wine b casks Distribution of malt samples aged in different cask(s) PCA. Distribution of malt samples aged in different cask(s) PLS-DA. The role of modern analytical approaches in fighting with food fraud

Whisky samples according cask 3.5 VIP-plot PLS-DA 3.5 3 3.5.5 1.5 Marker 1 Marker Marker 3 Marker 4 1.5 1 1.5.5 3 3.5 4 SIMCA 13. - 4/17/18 :44:33 PM (UTC+ 1.5 bourbon b cask bourbon/wine b casks 1 4 6 8 1 1 14 16 18 4 6 SIMCA 13. - 4/17/18 :44:33 PM (UTC+) Distribution of malt samples aged in different cask(s) PLS-DA. The role of modern analytical approaches in fighting with food fraud 1

Whisky samples according cask 1e+6 Marker 1 5e+5 Marker 8e+5 4e+5 6e+5 4e+5 e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 3e+5 e+5 1e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 5 1 15 5 3 35 4 45 5 55 6 5 1 15 5 3 35 4 45 5 55 6 8e+5 Marker 3 SIMCA 13. - 1/4/18 9:4 1.e+6 Marker 4 SIMCA 13. - 1/4/18 9:4 1e+6 6e+5 4e+5 e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 8e+5 6e+5 4e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks e+5 5 1 15 5 3 35 4 45 5 55 6 SIMCA 13. - 1/4/18 9 5 1 15 5 3 35 4 45 5 55 6 SIMCA 13. - 1/4/18 9:3 The role of modern analytical approaches in fighting with food fraud

Whisky samples according cask 1e+6 Marker 1 5e+5 Marker 8e+5 4e+5 6e+5 4e+5 e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 3e+5 e+5 1e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 5 1 15 5 3 35 4 45 5 55 6 5 1 15 5 3 35 4 45 5 55 6 8e+5 Marker 3 SIMCA 13. - 1/4/18 9:4 1.e+6 Marker 4 SIMCA 13. - 1/4/18 9:4 1e+6 6e+5 4e+5 e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 8e+5 6e+5 4e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks e+5 5 1 15 5 3 35 4 45 5 55 6 SIMCA 13. - 1/4/18 9 5 1 15 5 3 35 4 45 5 55 6 SIMCA 13. - 1/4/18 9:3

Whisky samples according cask 1e+6 Marker 1 5e+5 Marker 8e+5 4e+5 6e+5 4e+5 e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 3e+5 e+5 1e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 5 1 15 5 3 35 4 45 5 55 6 5 1 15 5 3 35 4 45 5 55 6 8e+5 Marker 3 SIMCA 13. - 1/4/18 9:4 1.e+6 Marker 4 SIMCA 13. - 1/4/18 9:4 1e+6 6e+5 4e+5 e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 8e+5 6e+5 4e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks e+5 5 1 15 5 3 35 4 45 5 55 6 SIMCA 13. - 1/4/18 9 5 1 15 5 3 35 4 45 5 55 6 SIMCA 13. - 1/4/18 9:3

Whisky samples according cask 1e+6 Marker 1 5e+5 Marker 8e+5 4e+5 6e+5 4e+5 e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 3e+5 e+5 1e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 5 1 15 5 3 35 4 45 5 55 6 5 1 15 5 3 35 4 45 5 55 6 8e+5 Marker 3 SIMCA 13. - 1/4/18 9:4 1.e+6 Marker 4 SIMCA 13. - 1/4/18 9:4 1e+6 6e+5 4e+5 e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 8e+5 6e+5 4e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks e+5 5 1 15 5 3 35 4 45 5 55 6 SIMCA 13. - 1/4/18 9 5 1 15 5 3 35 4 45 5 55 6 SIMCA 13. - 1/4/18 9:3

Whisky samples according cask 1e+6 Marker 1 5e+5 Marker 8e+5 4e+5 6e+5 4e+5 e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 3e+5 e+5 1e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 5 1 15 5 3 35 4 45 5 55 6 5 1 15 5 3 35 4 45 5 55 6 8e+5 Marker 3 SIMCA 13. - 1/4/18 9:4 1.e+6 Marker 4 SIMCA 13. - 1/4/18 9:4 1e+6 6e+5 4e+5 e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks 8e+5 6e+5 4e+5 Bbourbon cask Pbourbon/port wine casks R bourbon/red wine casks Sbourbon/sherry wine casks Wbourbon/white wine casks e+5 5 1 15 5 3 35 4 45 5 55 6 SIMCA 13. - 1/4/18 9 5 1 15 5 3 35 4 45 5 55 6 SIMCA 13. - 1/4/18 9:3

The power of spectral deconvolution 6. TIC x1 1.8 1.6 1.4 1. 1.8.6.4. 14.6 14.68 14.76 14.84 14.9 15. Retention time (min) The role of modern analytical approaches in fighting with food fraud 7

The power of spectral deconvolution 6 x1. 1.8 1.6 1.4 1. 1.8.6.4 1. TIC 14.6 14.68 14.76 14.84 14.9 15. Retention time (min) The role of modern analytical approaches in fighting with food fraud 8

The power of spectral deconvolution 6 x1. 1.8 1.6 1.4 1. 1.8.6.4. 1 TIC x1.8.7.6.5.4.3..1 Spectrum after TIC analysis 17.496 77.388 167.76 138.677 1.89 6 7 8 9 1 11 1 13 14 15 16 17 18 19 1 14.6 14.68 14.76 14.84 14.9 15. Retention time (min) The role of modern analytical approaches in fighting with food fraud 9

The power of spectral deconvolution 6 x1. 1.8 1.6 1.4 1. 1.8.6.4. 1 TIC 14.6 14.68 14.76 14.84 14.9 15. Retention time (min) x1.8.7.6.5.4.3..1 Spectrum after TIC analysis 17.496 77.388 167.76 138.677 1.89 6 7 8 9 1 11 1 13 14 15 16 17 18 19 1 1 deconvoluted spectrum Component RT: 14.7877 x1 8 7 6 5 4 3 1 13.439 167.76 1.887 6 7 8 9 1 11 1 13 14 15 16 17 18 19 1 (m/z) The role of modern analytical approaches in fighting with food fraud 3

The power of spectral deconvolution 6 x1. 1.8 1.6 1.4 1. 1.8.6.4. x1.9.8.7.6.5.4.3..1 1 TIC 14.6 14.68 14.76 14.84 14.9 15. Retention time (min) deconvoluted spectrum - Tyrosol 77.386 17.493 138.676 5 55 6 65 7 75 8 85 9 95 1 15 11 115 1 15 13 135 14 (m/z) x1.8.7.6.5.4.3..1 Spectrum after TIC analysis 17.496 77.388 167.76 138.677 1.89 6 7 8 9 1 11 1 13 14 15 16 17 18 19 1 1 deconvoluted spectrum Component RT: 14.7877 x1 8 7 6 5 4 3 1 1 5 13.439 167.76 1.887 6 7 8 9 1 11 1 13 14 15 16 17 18 19 1 (m/z) NIST spectrum Tyrosol 51 53 55 57 59 63 65 67 69 74 76 (mainlib) Benzeneethanol, 4-hydroxy- 77 78 81 83 86 89 91 94 96 11 13 15 (m/z) 55 6 65 7 75 8 85 9 95 1 15 11 115 1 15 13 135 14 17 18 19 115 117 119 11 13 135 137 The role of modern analytical approaches in fighting with food fraud 31 OH OH 138 139

The power of spectral deconvolution 6 x1. 1.8 1.6 1.4 1. 1.8.6.4. x1.9.8.7.6.5.4.3..1 1.e+6 1e+6 8e+5 6e+5 4e+5 1 TIC 14.6 14.68 14.76 14.84 14.9 15. Retention time (min) deconvoluted e+5 spectrum - Tyrosol Tyrosol 77.386 17.493 138.676 5 55 6 65 7 75 8 85 9 95 1 15 11 115 1 15 13 135 14 (m/z) x1.8.7.6.5.4.3..1 Spectrum after TIC analysis 17.496 77.388 167.76 138.677 1.89 6 7 8 9 1 11 1 13 14 15 16 17 18 19 1 1 deconvoluted spectrum Component RT: 14.7877 x1 8 7 6 5 4 3 1 5 13.439 167.76 1.887 6 7 8 9 1 11 1 13 14 15 16 17 18 19 1 (m/z) NIST spectrum Tyrosol 5 1 15 5 3 35 17 1 4 45 5 55 6 SIMCA 13. - 1/4/18 9:3 51 53 55 57 59 63 65 67 69 74 76 (mainlib) Benzeneethanol, 4-hydroxy- 77 78 81 83 86 89 91 94 96 11 13 15 (m/z) 55 6 65 7 75 8 85 9 95 1 15 11 115 1 15 13 135 14 18 19 115 117 119 11 13 135 137 The role of modern analytical approaches in fighting with food fraud 3 OH OH 138 139

Malt or blended whisky?? The role of modern analytical approaches in fighting with food fraud 33

Malt or blended whisky? Blended Scotch Whiskies represent the largest product category by volume of sales Malt Scotch Whiskies are premium product on the market The role of modern analytical approaches in fighting with food fraud 34

Malt or blended whisky? Blended Scotch Whiskies represent the largest product category by volume of sales Malt Scotch Whiskies are premium product on the market PCA peated malt whiskies B blended whiskies M malt whiskies SIMCA 13. - 1/17/18 The role of modern analytical approaches in fighting with food fraud 35

Malt or blended whisky? On the market are blended whiskies at different quality Extra blended whiskies contain more malt content and they are matured longer time period PCA the youngest single malt whisky (8 years) Bblended whiskies B premium blended whiskies Mmalt whiskies 1 years No. 5 SIMCA 13. - 1/17/18 The role of modern analytical approaches in fighting with food fraud 36

SIMCA 13. - 1/17/18 Malt or blended whisky? PLS-DA Bblended whiskies B premium blended whiskies M malt whiskies Recognition ability 99% Prediction ability 94% The role of modern analytical approaches in fighting with food fraud 37

.5..15.1.5.8.6.4. 1 3 4 5 6 7 8 9 1 11 1 13 14 1 3 4 5 6 7 8 9 1 11 1 13 14 SIMCA 13. - 1/17/18 SIMCA 13. - 4/18/18 SIMCA 13. - 1/19/18.4.35.3.5..15.1.4.35.3.5..15.1.35.3.5..15.1.5.15.1.5 1 3 4 5 6 7 8 9 1 11 1 13 14 1 3 4 5 6 7 8 9 1 11 1 13 14 1 3 4 5 6 7 8 9 1 11 1 13 14 1 3 4 5 6 7 8 9 1 11 1 13 14 SIMCA 13. - 1/19/ SIMCA 13. - 1/19/ SIMCA 13. - 4/18/1 SIMCA 13. - 4/18/18 Malt or blended whisky? PLS-DA Bblended whiskies B premium blended whiskies M malt whiskies Vanillin,4-diterbutylphenol Recognition ability 99% Prediction ability 94% Ethyl vanillate Benzylalcohol Damascenone 1-propanone-1-(4-hydroxy-3-methoxyphenyl The role of modern analytical approaches in fighting with food fraud 38

.5..15.1.5.8.6.4. 1 3 4 5 6 7 8 9 1 11 1 13 14 1 3 4 5 6 7 8 9 1 11 1 13 14 SIMCA 13. - 1/17/18 SIMCA 13. - 4/18/18 SIMCA 13. - 1/19/18.4.35.3.5..15.1.4.35.3.5..15.1.35.3.5..15.1.5.15.1.5 1 3 4 5 6 7 8 9 1 11 1 13 14 1 3 4 5 6 7 8 9 1 11 1 13 14 1 3 4 5 6 7 8 9 1 11 1 13 14 1 3 4 5 6 7 8 9 1 11 1 13 14 SIMCA 13. - 1/19/ SIMCA 13. - 1/19/ SIMCA 13. - 4/18/1 SIMCA 13. - 4/18/18 Malt or blended whisky? PLS-DA Bblended whiskies B premium blended whiskies M malt whiskies Vanillin,4-diterbutylphenol Recognition ability 99% Prediction ability 94% Ethyl vanillate Benzylalcohol Damascenone 1-propanone-1-(4-hydroxy-3-methoxyphenyl The role of modern analytical approaches in fighting with food fraud 39

Fake or authentic whisky?? The role of modern analytical approaches in fighting with food fraud 4

6e+6 4e+6 e+6 3e+6 e+6 1e+6 5e+6 4e+6 3e+6 e+6 1e+6 1 3 4 5 6 7 8 9 1 11 1 13 14 15 16 SIMCA 13. - 5/8/18 1 3 4 5 6 7 8 9 1 11 1 13 14 15 16 SIMCA 13. - 5/8/ 1 3 4 5 6 7 8 9 1 11 1 13 14 15 16 SIMCA 13. - 5/8/18 Fake or authentic whisky? PCA Fake samples Authentic samples g MMalt whiskies Blended whiskies Premium blended whiskies ffake whiskies Syringaldehyde Ethyl dodecanoate SIMCA 13. - 1/1/18 1:49 g 1,3-Diacetylbenzene The role of modern analytical approaches in fighting with food fraud 41

Fake or authentic whisky? PCA Fake samples Authentic samples 15 Vanillin 8 6 Anysladehyde 1 4 5 3 SD = 61.387 SD = 43.996 3 SD = 19.917 SD = 13.678 15 Average = 9.33137 1 3 4 5 6 7 8 9 1 11 1 13 14 15 16 17 18 SIMCA 13. - 5/3/17 11:1 Styralyl acetate 1 Average = 1.169 1 3 4 5 6 7 8 9 1 11 1 13 14 15 16 17 18 SIMCA 13. - 5/3/17 11: Triacetin 8 1 6 5 4 3 SD = 43.7396 3 SD = 31.684 SD = 9.637 SD =.3519 Average = 4.91886 Average = 1.41887 1 3 4 5 6 7 8 9 1 11 1 13 14 15 16 17 18 1 3 4 5 6 7 8 9 1 11 1 13 14 15 16 17 18 SIMCA 13. - 5/3/17 11:13 SIMCA 13. - 5/3/17 11:5 SD = 1 5141.8 SIMCA 13. - 1/1/18 1:49.6 Anysaldehyde, triacetin, benzaldehyde, syringol, styraryl acetate, vanillin, 1,,3-propanetriol,1- acetate, dimethyl succinate were detected in fake samples Some of them are food additives.4. -. -.4 -.6 -.8 -.6 -.4 -...4.6 p[1] RX[1] =.17 RX[] =.11 SIMCA 13. - 4/18/18 4:48:1 PM (UTC+) The role of modern analytical approaches in fighting with food fraud 4

Conclusion Non target screening strategy based on GC-Q-TOF for the whisky authentication has been developed Agilent 7b GC-QTOF The role of modern analytical approaches in fighting with food fraud 43

Conclusion Non target screening strategy based on GC-Q-TOF for the whisky authentication has been developed This new method provides additional information to classical methods used until now Agilent 7b GC-QTOF The role of modern analytical approaches in fighting with food fraud 44

Conclusion Non target screening strategy based on GC-Q-TOF for the whisky authentication has been developed This new method provides additional information to classical methods used until now Identified markers for: Different cask used for maturation N-(3-methylbutyl)Acetamide, -furancarboxylic acid, ethyl 5-oxoprolinate, tyrosol Malt (ethyl vanillate, damascenone, 1-propanone-1-(4-hydroxy-3- methoxy)phenyl) and blended (vanillin,,4-diterbutylphenol, benzylalcohol) whiskies Authentic samples Syringaldehyde, Ethyl dodecanoate, 1,3-Diacetylbenzene Agilent 7b GC-QTOF The role of modern analytical approaches in fighting with food fraud 45

Conclusion Non target screening strategy based on GC-Q-TOF for the whisky authentication has been developed This new method provides additional information to classical methods used until now Identified markers for: Different cask used for maturation N-(3-methylbutyl)Acetamide, -furancarboxylic acid, ethyl 5-oxoprolinate, tyrosol Malt (ethyl vanillate, damascenone, 1-propanone-1-(4-hydroxy-3- methoxy)phenyl) and blended (vanillin,,4-diterbutylphenol, benzylalcohol) whiskies Authentic samples Syringaldehyde, Ethyl dodecanoate, 1,3-Diacetylbenzene In fake samples, food additives were detected Agilent 7b GC-QTOF The role of modern analytical approaches in fighting with food fraud 46

Conclusion Non target screening strategy based on GC-Q-TOF for the whisky authentication has been developed This new method provides additional information to classical methods used until now Identified markers for: Different cask used for maturation N-(3-methylbutyl)Acetamide, -furancarboxylic acid, ethyl 5-oxoprolinate, tyrosol Malt (ethyl vanillate, damascenone, 1-propanone-1-(4-hydroxy-3- methoxy)phenyl) and blended (vanillin,,4-diterbutylphenol, benzylalcohol) whiskies Authentic samples Syringaldehyde, Ethyl dodecanoate, 1,3-Diacetylbenzene In fake samples, food additives were detected Agilent 7b GC-QTOF The role of modern analytical approaches in fighting with food fraud 47

www.foodintegrity.eu The project has received funding from the European Union s Seventh Framework Programme for research, technological development and demonstration under grant agreement No. 613688. Disclaimer: The information expressed in this presentation reflects the authors views; the European Commission is not liable for the information contained therein.

2024 © cuisinedocbox.com Privacy Policy | Terms of Service | Feedback