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1 SYMPOSIUM ON FOOD CHEMISTRY AND QUALITY ASSURANCE.

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Presentation on theme: "1 SYMPOSIUM ON FOOD CHEMISTRY AND QUALITY ASSURANCE."— Presentation transcript:

1 1 SYMPOSIUM ON FOOD CHEMISTRY AND QUALITY ASSURANCE

2 2 Alan Richards Head of Scientific Services Public Analyst (2m population) Official Agricultural Analyst President Association Public Analysts

3 3 Summary History of Food Adulteration in UK History of Food Adulteration in UK Public Analyst Links to Enforcement Public Analyst Links to Enforcement Legal Qualification (MChemA) Legal Qualification (MChemA) MChemA Examination MChemA Examination Certificates of Analysis Certificates of Analysis EU Methods and UK Analysis EU Methods and UK Analysis Test Methods Test Methods Food Complaints Food Complaints Other work of Public Analysts Other work of Public Analysts

4 4 UNITED KINGDOM

5 5 DURHAM

6 6 HISTORY OF FOOD ADULTERATION 1200 AD – KING HENRY II “GARBLE” 1200 AD – KING HENRY II “GARBLE” 1700 AD – STEADY INCREASE 1700 AD – STEADY INCREASE 1800 AD – INDUSTRIAL REVOLUTION 1800 AD – INDUSTRIAL REVOLUTION

7 7 In 1820 A TREATISE ON ADULTERATIONS OF FOOD, AND CULINARY POISONS. EXHIBITING The Fraudulent Sophistications of BREAD, BEER, WINE, SPIRITOUS LIQUORS, TEA, COFFEE, CREAM, CONFECTIONERY, VINEGAR, MUSTARD, PEPPER, CHEESE, OLIVE OIL, PICKLES, AND OTHER ARTICLES EMPLOYED IN DOMESTIC ECONOMY. AND METHODS OF DETECTING THEM. By Fredrick Accum, OPERATIVE CHEMIST, AND MEMBER OF THE PRINCIPAL ACADEMIES AND SOCIETIES OF ARTS AND SCIENCES IN EUROPE. Philadelphia: PRINTED AND PUBLISHED BY AB'M SMALL 1820.

8 8 Frederick Accum

9 ARTHUR HILL HASSALL ARTHUR HILL HASSALL Purchased and analysed 2500 articles of food and produced reports in the medical journal The Lancet identifying many examples of adulteration of foods. Information Link: ar/Thefightagainstfoodadulteration.asp ar/Thefightagainstfoodadulteration.asp

10 10 Origin of UK Food Law  1860ADULTERATION OF FOOD AND DRINKS ACT  1872ADULTERATION OF FOOD AND DRUGS ACT  1875SALE OF FOOD AND DRUGS ACT  1899SALE OF FOOD AND DRUGS ACT  1928FOOD AND DRUGS ADULTERATION ACT  1938FOOD AND DRUGS ACT  1955FOOD AND DRUGS ACT  1980FOOD ACT  1990FOOD SAFETY ACT 1999FOOD STANDARDS AGENCY

11 11 Modern Public Analysts Public Analyst Industry Food Standards Agency Government Chemist Environmenta l Health Consumers Trading Standards Central Science Lab English Law Courts

12 12 QUOTATION “The duties of the Public Analyst are daily increasing in complexity and difficulty. Higher qualifications than formerly are required of him, owing not only to the general advance in science as applied to the analysis of food, but also the exacting character of the numerous regulations of government departments concerned.... “ “The duties of the Public Analyst are daily increasing in complexity and difficulty. Higher qualifications than formerly are required of him, owing not only to the general advance in science as applied to the analysis of food, but also the exacting character of the numerous regulations of government departments concerned.... “ September 1923 September 1923

13 13 Mastership in Chemical Analysis

14 14 Food Safety Act Certificate

15 15 The MChemA Examination Theory of analytical instrumentation, Theory of analytical instrumentation, QA and statistics, QA and statistics, Methods of testing, Methods of testing, Laws relating to food, water and animal feeds Laws relating to food, water and animal feeds Practical application of skills Practical application of skills Ability to write certificates of analysis Ability to write certificates of analysis

16 16 MChemA Questions Day 1 Day 1  Theory of Analytical Chemistry, 3 hours,  Methods of analysis food, drugs & water 3 hours Day 2 Day 2  law related to food, drugs and water, lab administration  identify the six unknown substances using the microscope Day 3, 4 and 5 Day 3, 4 and 5  Practical Demonstration of Skills

17 17 Certificates of Analysis Food Safety Act  The FACTS  The STANDARD  The INTERPRETATION

18 18 Certificates of Analysis Food Complaint Certificate Food Complaint Certificate  Full History  Photographs  Results of Analysis  Interpretation  None Technical Report

19 19 Other Certificates Agriculture Act Certificates Agriculture Act Certificates Statements of Witness Statements of Witness UKAS UKAS

20 20 Official Food Labs

21 21 Other Work

22 22 Other Work

23 23 UK Food Laws Pre 1980 – mostly set by UK Pre 1980 – mostly set by UK EU Influence EU Influence EU Methods of Analysis EU Methods of Analysis  Contaminants in Food Regulation 2007  Commission Regulation (EC) No 1881/2006 of 19 December 2006  Commission Directive 2001/22/EC

24 24 Commission Directive 2001/22/EC  Specific methods for the determination of lead, cadmium and mercury  Specific methods for the determination of lead, cadmium and mercury  contents are not prescribed.  Laboratories shall use a validated method that fulfils the performance  Laboratories shall use a validated method that fulfils the performance  criteria indicated in Table 3.  Where possible, the validation shall include a certified reference material in  Where possible, the validation shall include a certified reference material in  the collaborative trial test materials.  LOD - No more than one tenth of the value of the specification in  LOD - No more than one tenth of the value of the specification in  Regulation (EC) No 466/2001, except if the value of the specification for lead is less than 0,1 mg/kg. For the latter, no more than one fifth of the value of the specification  LOQ - No more than one fifth of the value of the specification in Regulation  LOQ - No more than one fifth of the value of the specification in Regulation  (EC) No 466/2001, except if the value of the specification for lead is less than 0,1 mg/kg. For the latter, no more than two fifths of the value of the specification.  Precision HORRAT r or HORRAT R values of less than 1,5 in the validation  Precision HORRAT r or HORRAT R values of less than 1,5 in the validation  collaborative trial  Recovery %  Recovery % Specificity - Free from matrix or spectral interferences Specificity - Free from matrix or spectral interferences

25 25 UK and EU Laws When searching for UK regulations I need the date of the regulation and the statutory instrument (SI) number. All current regulations are available on the internet on the website: EC regulations can be found on the website: EC regulations can be found on the website: The public analyst website offers a list of current regulations on their website at: The public analyst website offers a list of current regulations on their website at:

26 26 Sampling Formal Sampling – passing on Formal Sampling – passing on Informal Sampling Informal Sampling Complaints Complaints Regulation sampling Regulation sampling Projects Projects Surveillance Surveillance

27 27 Glass Contamination

28 28 Fibres Human Hair Mouse Hair

29 29 Faecal Contamination

30 30 Moulds

31 31 Infestation

32 32 Authenticity Cod Haddock Salmon Coley

33 33 Modes of Adulteration Mislabelling of age ‘Stretching’ with neutral spirit (cereal or non–cereal derived) Geographic mislabelling Addition of flavourings Addition of sweetening

34 34 Methanol Propanol Isobutanol 2-methyl-1-butanol Isoamyl alcohol Ethyl acetate Isoamyl acetate Methanol Propanol Isobutanol 2-methyl-1-butanol Isoamyl alcohol Ethyl acetate Isoamyl acetate polar polar ? polar polar ? – – – – – – – – – – – – Polarity Compound BP (°C) Concentration range Chromatographic Analysis of Distilled Spirits Major Volatile Congeners (Mostly alcohols and esters)

35 35 Modes of Adulteration

36 36 Cask Extractives

37 37 Stable isotope analysis in food authentication Simon Kelly 1 & Alison Bateman 2 1 Institute of Food Research, Norwich, UK, NR4 7UA 2 University of East Anglia, Norwich, UK, NR4 7JT Detecting the substitution of Organic crops with conventional produce

38 38 Stable Isotopes of Nitrogen P 7 N P 7 N 8 ‘light’ isotope ‘heavy’ isotope 14 N 7 15 N %0.37 %

39 39 Tomatoes – normal dist n

40 40 Tomato Data - 3-D Scatter Plot for variables  15 N‰, Mn (ppm), Cu (ppm) & Rb (ppm)

41 41 A METHOD FOR THE SIMULTANEOUS DETERMINATION OF SWEETENERS IN FOODS Steve Appleton Steve Appleton Durham Scientific Services Durham Scientific Services

42 42 Evaporative Light Scattering Detector (ELSD) Gaining popularity as a universal detector. Simple three step process Nebulisation – column effluent forms a dispersion of droplets Nebulisation – column effluent forms a dispersion of droplets Evaporation – mobile phase is evaporated, leaving a fine mist of dried sample. Evaporation – mobile phase is evaporated, leaving a fine mist of dried sample. Detection – laser light scattered by sample particles is detected, generating an electrical signal. Detection – laser light scattered by sample particles is detected, generating an electrical signal.

43 43 Evaporative Light Scattering Detector (ELSD) Pro since all particles scatter light, all sample components are detected, regardless of their structure or optical properties. since all particles scatter light, all sample components are detected, regardless of their structure or optical properties.Con method limitations as it can only be used with volatile mobile phases and mobile phase modifiers method limitations as it can only be used with volatile mobile phases and mobile phase modifiers

44 44 ELSD

45 45 ELSD plus UV

46 46 Elisa and DNA Protein Protein  Heat labile  Cross reactivity  Batch variation DNA DNA  Cooked foods  Specific  Simplified “lab on a chip”

47 47 Lab on a Chip

48 48 DNA Analysis Applications Applications  Fish & meat speciation  Basmati rice authenticity  Detection of bushmeat  GMO testing  Fruit juices  Durum wheat

49 49 Fish Speciation Method uses PCR-RFLP Method uses PCR-RFLP A region of a specific gene is amplified by PCR using universal primers A region of a specific gene is amplified by PCR using universal primers  Produces a single PCR product of the same size from all samples Can be done on raw, cooked and some canned fish (not tuna) Can be done on raw, cooked and some canned fish (not tuna) No need for a reference specimen No need for a reference specimen

50 50 DNA Results

51 51 Reminder A WRONG RESULT IS WORSE THAN NO RESULT AT ALL !

52 52 THANK YOU


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