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Method for detecting content of fatty acid-chlorine-propylene glycol monoester and diester in food

A chloropropanol mono-diester, fatty acid technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of few separate detection studies, large elution solvent ratios, and complex solvent ratios, etc. The effect of less consumption, accurate qualitative analysis results and strong separation ability

Active Publication Date: 2013-08-14
FUJIAN CENT FOR DISEASE CONTROL & PREVENTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many research reports on the indirect determination of the total amount of fatty acid chloropropanol esters by hydrolysis method in the world, but there are few researches on the detection of fatty acid chloropropanol mono / diester content in food. People such as Seefelder use aminopropyl ( aminopropyl) solid-phase extraction method, eluting with a mixture of n-hexane, diethyl ether, dichloromethane and ethyl acetate in different proportions, separating 3-MCPD monoester and diester, and then detecting their respective contents by GC-MS , due to the variety of solvents used and the complex ratio of solvents, the operation is very cumbersome (Janis C , Owen W P , Ray H L , et al. Jr. J. Agric. Food Chem. 1984, 32(3), 474-476.); Zelinková et al. used silica gel solid-phase extraction method to elute and separate MCPD mono / diester with mixed solvents of petroleum ether and ether in different proportions, and then analyze it in combination with GC-MS, but its disadvantage is that the proportion of elution solvent required is large, and The volume of solvent consumed is as high as 850 ml, the operation is cumbersome, the sensitivity is low, and the instrument is seriously polluted (Zuzana Z , Doleqal M, Jan V. Eur Food Res Technol . 2009, 228:571–578.)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Sample handling

[0030] Accurately weigh the appropriate amount d 5 - 3-Chloro-1,2-propanediol monopalmitate, d 5 - 3-chloro-1,2-propanediol palmitate, d 5 - 2-Chloro-1,3-propanediol monostearate, d 5 - Dissolve 2-chloro-1,3-propanediol diester of stearic acid in a 10ml volumetric flask, dissolve it with ethyl acetate, adjust the volume to the mark, mix well to obtain a standard stock solution, and store it in a refrigerator at -24°C; Take an appropriate amount of stock solution and dilute it with n-hexane to 2.0 μg / ml mixed internal standard solution. Weigh 0.1 g of edible oil sample into a 1.5 ml plastic centrifuge tube, add 25 μl of mixed internal standard solution, and ultrasonically mix at 45 °C for 5 min.

[0031] (2) Extraction and separation

[0032] Column loading: transfer the well-mixed sample and internal standard solution into a 6.0 ml amino solid-phase extraction column activated by 4.0 ml of n-hexane (the weight of the amino filler is 0.5 g, the...

Embodiment 2

[0047] (1) Sample handling

[0048] Accurately weigh the appropriate amount d 5 - 3-Chloro-1,2-propanediol monopalmitate, d 5 - 3-chloro-1,2-propanediol palmitate, d 5 - 2-Chloro-1,3-propanediol monostearate, d 5 - Dissolve 2-chloro-1,3-propanediol diester of stearic acid in a 10ml volumetric flask, dissolve it with ethyl acetate, adjust the volume to the mark, mix well to obtain a standard stock solution, and store it in a refrigerator at -24°C; Take an appropriate amount of stock solution and dilute it with n-hexane to 2.0 μg / ml mixed internal standard solution. Weigh 1g of the mixed milk powder, extract the fat according to the first method in the national standard GB / T5413.3-2010 "Determination of fat in infant food and dairy products", and then take the fat extract of 0.1g milk powder Into a 1.5ml plastic centrifuge tube, add 25μl mixed internal standard solution, and ultrasonically mix at 45°C for 5 minutes;

[0049] (2) Extraction and separation

[0050] Column lo...

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Abstract

The invention relates to a method for detecting content of a fatty acid in food, and particularly relates to a method for detecting the contents of a fatty acid 3-chlorine-1,2-propylene glycol monoester, a fatty acid 3-chlorine-1,2-propylene glycol diester, a fatty acid 2-chlorine-1,3-propylene glycol monoester and a fatty acid 2-chlorine-1,3-propylene glycol diester in food by a gas chromatograph-mass spectrometer. According to the method, an amino solid-phase extraction column is adopted, a normal hexane-ethyl acetate mixed solvent is utilized for implementing elution, a GC-MS approach of alkaline hydrolysis-phenylboronic acid derivatization is utilized for determination; the method comprises seven steps of: sample treatment, extraction separation, alkaline hydrolysis treatment, derivatization treatment, analysis by the gas chromatograph-mass spectrometer, preparation of a standard curve, and quantification; and the method only needs few types of solvents and is low in solvent consumption, easy to operate, high in sensitivity, strong in analysis capability, correct in quantitive analysis result, low in detection limit and short in analysis time.

Description

technical field [0001] The invention relates to a method for detecting oil in food, in particular to a method for detecting fatty acid 3-chloro-1,2-propanediol monoester and fatty acid 3-chloro-1,2-propanediol in food by using gas chromatography-mass spectrometry Diester, fatty acid 2-chloro-1,3-propanediol monoester, fatty acid 2-chloro-1,3-propanediol diester four types of ester content method. Background technique [0002] Chloropropanols are well-known contaminants in food processing, especially 3-chloro-1,2-propanediol (3-MCPD for short), which is widely recognized for its nephrotoxicity, reproductive toxicity, immunosuppressive and potential carcinogenicity. attention, and fatty acid chloropropanol ester (chloropropyl ester) is a kind of substance formed by the esterification of chloropropanol and fatty acid, which is a new food safety problem in the world in recent years, especially fatty acid 3- Chloro-1,2-propanediol esters (3-MCPD esters for short) are the most po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 傅武胜吴少明郑奎城
Owner FUJIAN CENT FOR DISEASE CONTROL & PREVENTION
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