稳定同位素技术在果汁真实性鉴别研究与应用

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Method for 18O/16O Isotope Ratio Determination of Water
Manual Preparation Homogeneity of gas introduce
Test 1 2 Positon number 6 9 δ18O(ave) SD 0.07 0.06
Time 1992 1993 1995 1997 1997 1998 2004 Methods AOAC 992.09 CEN (TC174 N108, ENV 12140) AOAC Official method 995.17 CEN (TC174 N109, ENV 12141) CEN (TC174 N109, ENV 12142) BS DD ENV 13070-1998 AOAC method 2004.01 Component Water Cane sugar Ethanol Water Water Pulp Ethanol Instrument IRMS IRMS SNIF-NMR IRMS IRMS IRMS IRMS Isotope
What is NFC/FC orange juice?
National Standard：Orange juice and orange juice beverages
NFC- orange juice: Juice obtained directly from orange fruit, just processing by squeeze. FC-orange juice: Concentrated orange juice returned to its original state by the addition of water and other ingredients lost during the process of concentrated orange juice, to make sure the juice has the same color, flavor and soluble solid according to orange.
What is NFC/FC orange juice?
More fresh More natural More healthy More safe Better quality
No additives... No treatments... "NFC" juice: juice obtained by physical press
779 715
794 854 906 1054
Mainly are fresh fruits; •Lower deep processing rate; 75% of concentrated orange juices are imported.
The main fruit production since 2000(10,000 tons)
Repeatability of gas introduce
Pos. 1# No. 1 No. 2 No. 3 No. 4 -26.93 -27.22 -27.03 -27.36 Pos. 14# -27.03 -27.08 -27.19 -27.22
-27.29
-27.27
No. 5
-27.33
-27.20
7
Presented Orange juice standards GB/T 21731
physical &chemical paramenters
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Analytical Methods
NFC orange juice and FC orange juice
International Standards of Juice
QB/Twk.baidu.com855-2015
QB/T4854-2015
China National Determination of 13C/12C Isotope Ratio Standardization of pulp and total Center of Food sugar & Fermentation
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NFC fruit industry significance
•Great Market Potential •Resources Advantages •Improve fruit added value
•counterfeit products
•Lack of standards for authenticity assessment
Method for 18O/16O Isotope Ratio Determination of Water
Ion current of δ18O of CO2 measured by GC-IRMS
No. Intensity（mv） δ18O（‰）
1 4415 -9.29
2 4651 -9.40
1064 567 1132 579 1198 627
2007 2786 2008 2984
2009 3168 2010 3326 2011 3598 2012 3849
2058 2331
2521 2645 2944 3168
1289 669 1353 785
1426 883 1565 956 1579 1040 1707 1156
Determination of 18O/16O Isotope Ratio of Ethanol derived from juice sugar
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Method for 18O/16O Isotope Ratio Determination of Water
Type 1. （On-line equilibrium-IRMS）
Outline
1.Background 2.Methods Standards for Juice Analysis
3.Development of Stable Isotope Analytical Methods 4.Authenticity Assessment of Juices by IRMS 5.Food Analysis using Isotopic Technology Lab(FAIT)
18O/16O 13C/12C
(D/H)I , (D/H)II ,R
18O/16O
D/H
13C/12C
13C/12C
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Standards of Juice in China
Plan number of standards project name Method for 18O/16O Isotope Ratio Determination of Water in orange juice Technical focal China National Standardization Center of Food & Fermentation Drafting unit China National Research of Food &Fermentation Industries China National Research of Food &Fermentation Industries
Tangerine
878 1160
Pear Grapes 842 328 879 368
Banana 494 527
2002 1924
2003 2110 2004 2367 2005 2401 2006 2606
1199
1345 1495 1591 1689
930
979
447
517
555
590 605 651 690
Off-line equilibrium Separation and DI-IRMS purification of CO2 Gas tight syringes Separated by GC Eight-way valve CF-IRMS Classic method
On-line equilibrium
Commercialization CO2- water balancing device
Isotope ratio mass spectrometer
Method for 18O/16O Isotope Ratio Determination of Water
Type 2. New method (GC-IRMS)
3 4761 -9.38
4 4677 -9.30
5 4688 -9.33
6 4722 -9.29
7 4703 -9.28
8 4689 -9.31
9 4692 -9.30
10 4687 -9.27
Ave
SD
-9.31
0.04
The intensities of 10 injections are similar. the SD of 10 measurement is only 0.4‰, which reached the inter-precision of GasBench II-IRMS （SD≤0.08‰，n=10）.
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Fruit and juice industry situation in China
Annual production: 120 million tons; The outputs of apple and orange lead the world.
Yeas Apple 2000 2043 2001 2001
Just like GasBench -IRMS
Method for 18O/16O Isotope Ratio Determination of Water
Aerated
CO2- water Isotope exchange equilibrium
Injection
pretreatment device
Research & Application of Stable Isotopic Techniques In Juices Authenticity Assessment
钟其顶 博士
Dr. Zhong Qiding
China National Research Institute of Food &S Fermentation Industries National Standard Center of food & Fermentation Industries
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Method Development
Method for 18O/16O Isotope Ratio Determination of Water in orange juice Determination of 13C/12C Isotope Ratio of pulp and total sugar
Outline
1.Background 2.Methods Standards for Juice Analysis
3.Development of Stable Isotope Analytical Methods 4.Authenticity Assessment of Juices by IRMS 5.Food Analysis using Isotopic Technology Lab(FAIT)
Max Min the range Ave SD
-26.93 -27.36 0.43
-27.03 -27.22 0.19
-27.17
0.19
-27.14
0.08
Precision of δ18O determination
No. 1 2 3 4 5 6
Beijing 2015.11
Outline
1.Background 2.Methods Standards for Juice Analysis
3.Development of Stable Isotope Analytical Methods 4.Authenticity Assessment of Juices by IRMS 5.Food Analysis using Isotopic Technology Lab(FAIT)