Advanced analytical methods to test fruit juice authenticity
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17. January 2014
SGF/IRMA Conference in Bangalore (India)
Advanced analytical methods
to test fruit juice authenticity:
Dr. Eric Jamin,
Authenticity Competence Center
Eurofins Analytics France
Presentation by Mrs Navita Pinto
Eurofins Analytical Services India Pvt. Ltd.
www.eurofins.com
AIJN Code of Practice (COP)
Defines typical ranges for the main fruits used in Fruit juices
A criteria = Absolute Quality Requirements
= Brix/density, HMF, ethanol/lactic acid, Toxic
elements, mycotoxins, etc.
COP AIJN
B criteria = Further Authenticity Requirements
= Sugars, organic acids, minerals, etc.
2
Are AIJN parameters equally useful ?NO
Are they sufficient? NO
While most of them are useful, in our experience it is not worth
analysing systematically 100% of AIJN B criteria
(For example we are not using the full amino-acid spectrum but
specific ones + the formol index)
On the other hand some additional tests not covered in the COP
such as the oligosacharides Gc-profile, the anthocyanins HPLC-
profile in red etc. are extremely efficient
Eurofins recommended offer is a tailor-made selection of the
most relevant parameters and validated advanced methods
Eurofins also contributes to the continuous improvement
process of the AIJN COP scope
3
Analytical tools for authenticity testing
Chemical composition methods (e.g. chromatography)
Identification & quantification of defined compounds
Stable isotopes
Molecules origin
Molecular Biology
Identification of species, varieties, etc.
Profiling methods
Whole matrices fingerprint
4
Authenticity issues / analytical solutions
Undeclared addition of other fruit Composition (+ DNA for some fruits)
Undeclared addition of sugar SNIF-NMR & GC oligosacharides profile
Undeclared addition of water (NFC juice/purée) 18O-IRMS of water and ethanol (internal reference)
Undeclared addition of vitamin C Positional C13-IRMS of ascorbic acid
Undeclared addition of Citric acid C13 & 2H-IRMS of citric acid
Undeclared addition of malic acid Positional C13-IRMS of malic acid
Geographical mislabelling 87 Sr-TIMS and multi-isotope testing
Undeclared flavour addition GC-MS profile & chiral analysis of volatiles
5
Isotopic analyses to detect sugar addition:
SNIF-NMR & 13C-IRMS
JUICE
COMPONENTS
Water Sugars
13C/12C
Fermentation
+ Distillation Ethanol
18O/16O 2H/1H
2H/1H
Normalisation to V.SMOW
(International standard)
6
SNIF-NMR applied to Deuterium :
Detection of beet / Corn / Cane sugar
13C -5.0
(‰)
-10.0
Cane, corn
Ethanol
From -15.0
sugars
-20.0
-25.0
Mango (global ranges
-30.0
Beet from AIJN COP)
-35.0
85.0 90.0 95.0 100.0 105.0 110.0 115.0 120.0 125.0 130.0
(D/H)I (ppm) Ethanol from sugars
7
Cap-GC of oligosaccharides:
Detection of sugar syrups
In some cases (e.g. apple) the isotopic values partially overlap
With starch or inulin –derived sugar syrups
Complementary use of sugar syrup marker detected by GC:
- maltose, isomaltose (glucose syrup from cereals starch)
- High Fructose Syrup From Inulin (Chicory, etc.)
- Invert Sugar (from cane or beet sucrose)
8Isotopic analyses in direct fruit juice:
Improved detection of water addition
NFC JUICE
COMPONENTS
Water Sugars
2H/1H
Fermentation Ethanol 18O/16O
18O/16O 2H/1H CH2CH3OH
13C/12C
J. Agric. Food Chem. (2003) 51, 18, 5202-5206
J. Agric. Food Chem. (2006), Vol. 54, No. 2, 279-284
J.AOAC International (2013), Vol. 96, N° 3, 615-
9Practical use: improvement of the existing
method based on water 18O
12
11
10
9
8
7
6 Lab-squeezed
5 samples
O water (‰)
4
3 Market NFC
2
Water addition juices
1
0 Market FC
juices
18
-1
-2
-3 Max (95% c.i.)
-4
-5
-6 Authentic orange from a Min (95% c.i.)
-7 specific origin
-8
-9
AIJN limit
-10
18O ethanol (‰)
J. Agric. Food Chem. (2003) 51, 18, 5202-5206
1018O of ethanol for NFC juice: status
SOP was collaboratively tested:
AIJN guideline for all fruits
Reference data have been published for:
• orange (2003, update in JAOAC 2013)
• pineapple (IFU 2010)
• grape (Revue des œnologues 2010)
11DNA test for mango varieties
Applicable to mango products (juice, concentrate, nectar, purée)
Varieties studied so far :
Itiuba (BRN)
Hilaza (CO)
Chato (PE)
Manila (MEX)
Oro (MEX) The test can detect the presence of a foreign
Criollo (GUA)
Kesar (IND)
variety in Alphonso at > 10%
Sindhura (IND)
Raspuri (IND) In case a mixture is detected, partial
Neelam (IND) quantification can be performed (only
Magdalena River (CO)
regarding the relative %DNA, not the %fruit
Ataulfo (MEX)
Totapuri (IND)
itself).
Alphonso (IND)
Tommy Atkins (MEX) For other varieties, reference material should
Tommy Atkins (BRA)
be provided
Tommy (MEX)
Tommy Haden (MEX)
Petacon (MEX)Mango flavour Organoleptic testing (expert panel) Gc-MS profiles: Totapuri characterised by high terpenes (e.g. Beta myrcene, Ocimene, valencene) Alphonso more complex, characterised by lactons, etc. Keitt, Magdalena: more balanced, less characteric compounds
MANGO:
what are the risks based on past cases?
% non compliance
50%
40%
2% 0%
30%
4% 0%
4%
20% 4%
sugar addition
10% 6% bad quality
citric acid addition
low brix
0%
other fruit
apple orange pineapple mango acerola pomegranate 6%
water addition
untypical flavour profile
58% low fruit content (nectar)
8% labelling
(vide)
8%
Disclaimer:
Non compliance rates presented above are global and may not reflect accurately the market situation in
each country
but they can be used as qualitative indications for major risks for each fruit on a worldwide basis
23/01/2014 Authenticity testing 14More fruit databases are in construction...
Many of them from INDIA
Mango
Apple Cashew apple
Guava
Pomegranate
15Thank you for your attention!
Your contacts:
In Bangalore (India) : In Nantes (France)
Navita Pinto Eric Jamin
Eurofins Analytical Services India Pvt. Ltd., Marcel Dumoulin
#183, Gayathri Tech Park, Julien Chupin
EPIP 2nd Phase, Whitefield, Eurofins Analytics France
Bangalore – 560066 Tel: +33 2 51 83 21 00
Direct- +918030982532
email: eurofinsfr@eurofins.com
Mobile:+9190 1948 8466
www.eurofins.fr
email: navitapinto@eurofins.com
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