1. www.eurofins.com The New EU Fruit Juice Directive & recent Issues seen in Europe The New EU Fruit Juice Directive & recent Issues seen in Europe Dr David A Hammond Fruit Juice and Authenticity Expert Eurofins Analytics France TCJJP Las Vegas October 2012

2. Topics for today 1) New European Fruit Juice Directive  What’s new relative to the old version 2) Issues seen in the lab & detection methods  Water addition to NFC juice  C 4 sugar addition to pineapple juice  Foreign fruit addition to pomegranate juice  Sugar syrup addition to apple juice

3. EU Fruit Juice Directive (FJD) 2012/12/EU  EU Commission wanted to align the FJD closer to the Codex standard for Fruit Juices (Std # 247, 2005)  http://www.codexalimentarius.org/standards/list-of- standards/en/?provide=standards&orderField=fullReference&so rt=asc&num1=CODEX http://www.codexalimentarius.org/standards/list-of- standards/en/?provide=standards&orderField=fullReference&so rt=asc&num1=CODEX  Limit any possible issues with WTO  Wanted to adjust Directive to take into account new production techniques etc  Web reference for the FJD  http://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=OJ:L:2012:115:0001:0011:EN:PDF http://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=OJ:L:2012:115:0001:0011:EN:PDF

4. Major changes to FJD (1) Definitions  Fruit juice (NFC)  Fruit juice from concentrate  Concentrated fruit juice  Dried/powdered fruit juice Addition to definitions - Water extracted fruit juice  This cover juices, which are prepared from dried fruit e.g. plums (prunes), or materials which are too pulpy to press e.g. Acai.  Water extracted prune juice  Although it was not actually legal to call these juices, as they were not prepared by physical means from fresh unpreserved fruit without the addition of water!  Codex YES

5. Major changes to FJD (2) Aroma At present it is compulsory to restore the aroma of a Fruit Juice From Concentrate (FJFC) so that it “shows similar organoleptic and chemical characteristics of an average juice” Aroma restoration to a NFC juice is only permitted from a material recovered from the same batch of juice The restoration of aroma to a NFC & FJFC will be optional. The aroma shall be prepared from the same species of fruit by physical means This solves what has been a very contentious issue in Europe, however, kept the horrible term “average type of juice” Codex YES

6. Major changes to FJD (3) Sugar Previously the addition of sugar to a FJ was permitted:-  Up to 15 g/l for sugar acid correction, provided it was labelled  15 to 150 g/l provided product was labelled as “sweetened” The addition of sugar to FJ, FJFC & FJC will be banned from 4/2015 However, this will mean that it will no longer be possible to make a “No Added Sugar Claim” on retail packs. Codex NO Water “The water (to reconstitute juice concentrate) added must display appropriate characteristics, particularly from the chemical, microbiological and organoleptic viewpoints, in such a way as to guarantee the essential qualities of the juice.” The water for reconstitution should conform to the EU potable water directive (98/3/EC) Codex Yes

7. Major changes to FJD (4) Tomato is now classed as a fruit rather than a vegetable. Under the previous directive this was specifically excluded, as some member states did not allow tomato juice to be prepared from concentrate Codex YES

8. Major changes to FJD (5) Claims It will no longer be possible to make a “sugar free claim” for fruit juices nectars even if they contain added high intensity sweeteners Brix values The Brix of four products:- mango puree, passion fruit, blackcurrant and guava juice were reduced to the values given in the codex standard. These are typically 0.6 to 1.5 Brix lower than the values given in the AIJN reference guides and in the 2010 revision of FJD 112, 2001 AIJN is collecting data to determine if their values or Codex are closer to reality Codex ?

9. 9 What has been happening to juice prices in the last few years?  Orange juice  With short crops, small inventories and strong demand from China the price of OJC has been high and is likely to remain firm  Apple juice  Due to the pressure on the supply of apples available for processing in China the price for AJC is likely to remain firm in the near future  Pineapple juice  The pressure on pineapple has eased, from 2009/2010 when it was like “gold dust” but prices likely to remain firm What do these features mean

10. What does this mean?  Most suppliers are honest and will supply you with “what you want”  However, with the pressure on prices and juices in relatively short supply there are likely to be more issues with extension (adulteration) of juice  So what authenticity issues have we seen recently in our laboratory?

11. Issues seen in various juices in our lab

12. Issues seen with orange

13. 13 13 C/ 12 C NFC JUICE Sugars COMPONENTS Fermentation  Ethanol 2 H/ 1 H CH 2 CH 3 OH 18 O/ 16 O 2 H/ 1 H Water 18 O/ 16 O Isotopic analyses in direct fruit juice: Improved detection of water addition J. Agric. Food Chem. (2003) 51, 18, 5202-5206 ; J. Agric. Food Chem. (2006), Vol. 54, No. 2, 279-284 Given in AIJN COP

14. 14 Seasonal & regional effects: similar impact on water and ethanol Precipitations (San Jose):

15. Water addition to NFC juice 1. The best way to detect water added to NFC juice is by using isotopic methods 2. The single parameter method δ 18 O or δD given in the AIJN COP is not very sensitive to ground water addition and may lead to false positive results (as shown by Costa Rica) 3. Eurofins published the original paper on this approach in 2003 4. Eurofins has working with the isotopic group of the Association with German Food Chemist & conducted a ring test of the method which was completely recently

16. Pineapple problems

17. 17 Advantage of 13 C SNIF-NMR of ethanol : discrimination between CAM and C 4 plants C3C3 C4C4 CAM Similar global 13 C NEW ! CH 2 OH CH 3 CH 2 OH CH 3 CH 2 OH CH 3 Sugars ethanol

18. 18 New application of 13 C SNIF-NMR to pineapple: improved detection of C 4 sugar addition J. Agric. Food Chem. 2010, 58, 11580–11585 Corn (C 4 ) Cane (C 4 ) Pineapples (CAM) Beet (C 3 ) Cane sugar addition

19. Pomegranate issues

20. Traditional methods Addition of cheaper juices to pomegranate  Anthocyanin profile (IFU 71)  Sorbitol by HPLC (IFU 67) or electrochemical detection  Tartaric acid by HPLC (IFU 65)  Cap-GC profile (IFU rec 4) Addition of sugars to apple juice  Cap-GC profile (IFU rec 4)

21. Normal Anthocyanin profile for pomegranate juice Delpin-3,5-digluc Cyan-3,5-digluc Delpin-3-gluc Cyn-3-gluc Unknown

22. Anthocyanin profile for adulterated pomegranate juice Acylated “cyanidins” Pomegranate juice plus black carrot extract Small peaks are pom.

23. Rapid Screening methods For years juice chemists have been on a mission to find the ultimate method that is :- Quick to apply Cheap to utilise Able to detect all adulterations Tried:- FT mid range Infra red spectroscopy (FT-IR) Near Infra Red Spectroscopy (NIR) Pyrolysis mass spectrometry (Py-MS) All have failed in time to deliver early promise

24. 1 H-NMR Screening Work conducted by SGF in association with Bruker & independently at Eurofins suggests that “we” are getting there. Both teams have shown that from the pattern of peaks in the NMR spectrum you can:-  Estimate, with good accuracy, the concentrations of a range of juice components sugars, acids, sorbitol etc  Detect the presence of some foreign components in a juice  Use statistical techniques to identify abnormal juices  The technique is used by many of the national and regional schemes within EQCS as a screening method

25. Typical report from this method showing abnormal results for an orange juice blend

26. Statistical assessment into OJ, MJ & Blood OJ

27. Country of origin

28. NFC or FC

29. Sample does not fit expected juice model 1) Could be due to adulteration 2) Or unusual properties

30. Conclusions (1) 1) Know the regulations of the country you are exporting to 2) Ensure any practices that you are using are legal in that country e.g. Use of cellulases in the EU are not permitted so you can not use total liquefaction of the fruit to extract juice and sell it to EU countries Ensure any agrochemcicals that are permitted on your fruit are approved in the importing country or allow a sufficiently large “wash out” period so there are no residues. Most countries have an action level of 10 ppb for unapproved materials, “which is not a lot”. 3) Due to crop shortages and high fruit prices there have been more issues with juice adulteration in the last two years than normal

31. Conclusions (2) 4) Most suppliers are honest, however, there are always a few that take a “flexible view” on what is allowed 5) New methods have shown up old problems 6) Old methods have shown up old issues 7) This would suggest a higher level of testing should be employed to ensure quality material at present 8) It takes a long time and a lot on money to build a good reputation but this can be lost very quickly if you are caught with adulterated or “sub-standard” products

32. 32 Thank you for your attention. Any questions? davidfruitjuice@aol.com