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Method for simultaneous detection of 3-chloropropanol ester and glycidyl ester in food

A technology of glycidyl ester and chloropropanol ester, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of inability to meet the detection requirements of a wide variety of food substrates, long detection cycles, and low detection efficiency, and achieves short The effect of processing cycle, high accuracy and sensitive method

Inactive Publication Date: 2017-03-15
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, in the draft ISO international standard and the DGF standard of the German Oil Industry Association, the detection method for the content of 3-chloropropanol fatty acid ester and glycidol has the defect that the detection method is aimed at a single matrix, which cannot meet the requirements of a wide variety of food products. Matrix testing requirements
In addition, most of the existing detection methods are only for oil samples, and can only detect 3-chloropropanol fatty acid esters or glycidyl esters in samples, which have problems such as low detection efficiency and long detection cycle.

Method used

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  • Method for simultaneous detection of 3-chloropropanol ester and glycidyl ester in food
  • Method for simultaneous detection of 3-chloropropanol ester and glycidyl ester in food
  • Method for simultaneous detection of 3-chloropropanol ester and glycidyl ester in food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Example 1 Simultaneous detection of 3-chloropropanol esters and glycidyl esters in edible oil matrix samples

[0080] 1.1 Solution preparation

[0081] 0.5mol / L sodium methoxide-methanol solution: Weigh 2.701g of solid sodium methoxide into a 100mL volumetric flask, dilute to 100mL with methanol, and mix well.

[0082] 10% sodium sulfate-acetic acid solution: Weigh 10 g of anhydrous sodium sulfate solid, dissolve it in 100 mL of water, and then add 4 mL of glacial acetic acid to the solution.

[0083] 20% sodium chloride-acetic acid solution: Weigh 20 g of sodium chloride solid, dissolve it in 100 mL of water, and then add 4 mL of glacial acetic acid to the solution.

[0084] Acetone-water solution (19:1, V / V): Measure 190mL of acetone and 10mL of water, and mix well.

[0085] PBA solution: Weigh 2.5g of phenylboronic acid (PBA) and dissolve it in 20ml of acetone-water (19:1, V / V), and mix well.

[0086] Tert-butyl methyl ether-ethyl acetate solution (8:2, V / V): Meas...

Embodiment 2

[0133] Example 2 Simultaneous detection of 3-chloropropanol ester and glycidyl ester in milk powder food matrix samples

[0134] 2.1 Make standard curve

[0135] Refer to the preparation method of the standard curve in 1.2 in Example 1, and no more details are given. The 3-chloropropanol ester and glycidyl ester total amount standard curve equation that present embodiment makes is Y=0.5134X+0.03946 (R=0.9992, linear range is 0.05~2.0mg / kg); The 3-chloropropanol of making The equation of the ester content standard curve is Y=0.5X+0.08215 (R=0.9995, the linear range is 0.025~1.0mg / kg).

[0136] 2.2 Food sample testing

[0137] 1) Sample pretreatment: the sample of this embodiment is milk powder, get 2g sample in the polytetrafluoroethylene centrifuge tube of 50mL tool stopper, establish two such samples, and respectively as sample experiment group A, sample experiment group B, Add 50 μL of internal standard solution to the samples of sample experimental groups A and B respect...

Embodiment 3

[0141] Example 3 Simultaneous detection of 3-chloropropanol ester and glycidyl ester in fried puffed food matrix samples

[0142] 3.1 Make standard curve

[0143] Refer to the preparation method of the standard curve in 1.2 in Example 1, and no more details are given. The 3-chloropropanol ester and glycidyl ester total amount standard curve equation that present embodiment makes is Y=0.6185X-0.005332 (R=0.9993, linear range is 0.1~5.0mg / kg); The 3-chloropropanol of making The equation of the ester content standard curve is Y=0.6120X-0.01025 (R=0.9998, the linear range is 0.05-2.5 mg / kg).

[0144] 3.2 Food sample testing

[0145] All steps of food sample detection in this embodiment are carried out with reference to the corresponding steps in 2.2 in Example 2, and will not be repeated here.

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Abstract

The invention provides a method for simultaneous detection of 3-chloropropanol ester and glycidyl ester in food. The method comprises the following steps: 1) pretreatment of a sample: dividing a food sample into two equal parts which are respectively used as food samples for a sample testing group A and a sample testing group B, and separately adding an internal standard solution into the food samples for ultrasonic extraction; 2) an ester interchange reaction: subjecting to-be-reacted solutions of the sample testing groups A and B to a hydrolysis reaction, then respectively adding a sodium chloride-acetic acid solution and a sodium sulfate-acetic acid solution into the reaction systems of the sample testing groups A and B to terminate the hydrolysis reaction, and then separately carrying out de-esterification with n-hexane; 3) a derivative reaction: adding a phenylboronic acid solution into residues obtained after de-esterification of the sample testing groups A and B for the derivative reaction;and 4) GC-MS detection and analysis. The method provided by the invention can simultaneously detect 3-chloropropanol ester and glycidyl ester in food, has high detection efficiency and is applicable to detection of a plurality of food samples.

Description

technical field [0001] The invention belongs to the field of food safety, in particular to a method for simultaneously detecting 3-chloropropanol ester and glycidyl ester in food. Background technique [0002] Chloropropanol esters (chloropropanol esters) and glycidol esters (GE) are new pollutants discovered in recent years. It has been detected in infant milk powder. Chloropropanol esters are the esterification products of chloropropanol and fatty acids. Glycidyl esters in oils coexist with chloride ions, and can also form chloropropanol esters when heated. Glycidyl esters and chloropropanol esters It can be hydrolyzed in internal organs and converted into carcinogenic glycidol and chloropropanol compounds, among which 3-chloropropanol (3-MCPD) is the most toxic. Most of 3-chloropropanols in food exist in the form of fatty acid esters, and the free form is rare. At present, the research on 3-MCPD esters mainly focuses on 3-MCPD esters. [0003] In 1995, the Food Science...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/067
Inventor 刘青曾广丰王志元邹志飞陈文锐黄瑾韦晓群庞世琦
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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