The New EU Fruit Juice Directive & recent Issues seen in Europe TCJJP Las Vegas October 2012 Dr David A Hammond Fruit Juice and Authenticity Expert Eurofins Analytics France www.eurofins.com 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 C4 sugar addition to pineapple juice Foreign fruit addition to pomegranate juice Sugar syrup addition to apple juice 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-ofstandards/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 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 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 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 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 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 ? 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 9 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? Issues seen in various juices in our lab Issues seen with orange Isotopic analyses in direct fruit juice: Improved detection of water addition NFC JUICE COMPONENTS Water Sugars 2H/1H Fermentation Ethanol 18O/16O 2H/1H 18O/16O CH2CH3OH 13C/12C Given in AIJN COP J. Agric. Food Chem. (2003) 51, 18, 5202-5206 ; J. Agric. Food Chem. (2006), Vol. 54, No. 2, 279-284 13 Seasonal & regional effects: similar impact on water and ethanol 5 4 Authentic pineapple 3 2 1 AIJN guideline 18 d O water 0 -1 -2 -3 Costa Rican fruits -4 -5 -6 Costa Rican juices -7 -8 -9 -10 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 d18O ethanol (‰) 14 Precipitations (San Jose): 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 δ18O 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 Pineapple problems Advantage of 13C SNIF-NMR of ethanol : discrimination between CAM and C4 plants Sugars ethanol C4 C3 CH2OH CH2OH CH3 CAM CH2OH NEW ! CH3 17 CH3 New application of 13C SNIF-NMR to pineapple: improved detection of C4 sugar addition -5 Corn (C4) Pineapple CANE Cane (C4) -15 50% 30% 15% -20 Cane sugar addition MAIZE 20% 10% 0% BEET d 13 C of ethanol CH 3 (‰) -10 Pineapples (CAM) -25 Spiked samples Beet (C3) -30 -30 -25 -20 -15 -10 -5 d 13C of ethanol CH2 (‰ ) J. Agric. Food Chem. 2010, 58, 11580–11585 18 0 Pomegranate issues 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) Normal Anthocyanin profile for pomegranate juice Delpin-3,5-digluc Cyan-3,5-digluc Delpin-3-gluc Cyn-3-gluc Unknown Anthocyanin profile for adulterated pomegranate juice Acylated “cyanidins” Small peaks are pom. Pomegranate juice plus black carrot extract 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 1H-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 Typical report from this method showing abnormal results for an orange juice blend Statistical assessment into OJ, MJ & Blood OJ Country of origin NFC or FC Sample does not fit expected juice model 1) Could be due to adulteration 2) Or unusual properties 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 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 Thank you for your attention. Any questions? davidfruitjuice@aol.com 32