Tackling Food Fraud, International Approaches

Lemon PMF Update AOAC Virtual Annual Meeting & Exposition 2020

Ramin Jahromi Eurofins Nutrition Analysis Center Des Moines, IA E-mail: [email protected] +1 5152651461

[email protected] www.eurofins.com Please Note

Most suppliers are honest and will supply you with what you ordered, however, not ALL are!

Through testing you cannot prove authenticity – you can only look for indicators of adulteration.

[email protected] 2 What legally is a Fruit Juice? Codex Alimentarius Fruit Juice Standard 247/2005

Legal definition Fruit juice is the unfermented but fermentable liquid obtained from the edible part of sound, appropriately mature and fresh fruit or of fruit maintained in sound condition by suitable means including post harvest surface treatments applied in accordance with the applicable provisions of the Codex Alimentarius Commission. Some may be processed with pips, seeds and peel, which are not usually incorporated in the juice, but some parts or components of pips, seeds and peel, which cannot be removed by Good Manufacturing Practices (GMP) will be acceptable. The juice is prepared by suitable processes, which maintain the essential physical, chemical, organoleptical and nutritional characteristics of the juices of the fruit from which it comes. The juice may be cloudy or clear and may have restored aromatic substances and volatile flavour components, all of which must be obtained by suitable physical means, and all of which must be recovered from the same kind of fruit. Pulp and cells obtained by suitable physical means from the same kind of fruit may be added.

[email protected] 21CFR146.114

[email protected] 4 What types of adulteration occur?

1) Addition of sugars to juice e.g. the addition of sucrose and/or syrups to , addition of a high fructose syrup to 2) Addition of undeclared acids to juice e.g. the extension of juice with synthetic citric acid or apple juice with malic acid 3) Extension of an expensive juice with a cheaper one e.g. extension of juice with apple juice, pomegranate with cherry, , apple ………… 4) Accidental contamination e.g. adventitious mixing of different juices due to poor GMP

[email protected] When is it detected?

When you test! Now and again at any time Generally more of a problem when prices are high When a “new juice” is popular and in short supply When a new method is introduced 1991 UK’s MAFF used SNIF-NMR® to detect sugar addition in OJ (16 out of 21 samples failed) 1995/6 Cap-GC introduced detected adulteration of apple juice (major problem) 2007 Isotopic & conventional analysis of (MAJOR problems highlighted) 2015/16 Polymethoxylated flavones to detect addition of to lemon -IFU Rec No. 11 (2020)

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[email protected] 10 PMF Method IFU Rec No.11 (2020)

 Sample (20 ml) is passed through activated C18 SPE cartridge.  The sugars and acids are then eluted from the cartridge with 5 mL water.  The more polar materials are then eluted with 5 mL 28% acetonitrile in water.  Traces of solvent are “blown” out of the SPE cartridge with air, prior to the final elution of the PMFs using 5 mL 1:1 methanol/chloroform.  The solvent is collected in a small flask and removed from the extract by evaporation under vacuum at 35°C.  The residue is taken up in methanol (1 ml) prior to LC analysis.

[email protected] 11 Pure Lemon & Lime Juice

[email protected] 12 Brazilian Lime & Lemon

[email protected] 13 Brazilian Lime & Lemon

[email protected] 14 Brazilian Lime & Lemon

DAD 313.8 nm vs. 7-Methoxy 322.2 nm

[email protected] 15 Mexican Lime & Lemon

[email protected] 16 Florida Unripe Lemon

Research by Danielle Pringle-EurofinsUS

[email protected] 17 Florida Unripe Lemon

[email protected] 18 Detection of lime in lemon Lemon Juice Citropten

Labelled as 7-Methoxycoumarin* lemon juice?? Lime juice! Bergapten$ Isopimpinellin$

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*Lehnert & Ara Fruit processing 2014, 242 – 248, $Jahromi et al Poster @ AOAC annual meeting 2015 Questions

Any Questions?

[email protected] +1 515 265 1461