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A kind of quantitative method of chloropropanol fatty acid ester

A technology of fatty acid ester and chloropropanol, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of large difference in reaction rate, long time consumption, low detection efficiency, etc., to improve quantitative analysis efficiency and improve quantitative analysis. Efficiency, high sample recovery effect

Active Publication Date: 2021-07-06
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can detect the contents of different forms of 3-MCPD in oils and fats respectively, and obtain the content data of free 3-MCPD, 3-MCPD monoester and 3-MCPD diester, but the acid-catalyzed alcoholysis process is time-consuming Long, low detection efficiency
[0006] CN104237434A discloses a method for detecting the content of 3-chloro-1,2-propanediol ester in edible oil, the method comprising the following steps: sample pretreatment, acid-catalyzed transesterification, salting-out, extraction, purification, derivatization and detection, During the sample pretreatment process, the internal standard substance d5-3-chloro-1,2-propanediol palmitic acid diester is added, and the acid-catalyzed transesterification reaction is carried out at a constant temperature of 40-55°C and closed reaction for 0.5-2h. The method uses acid Catalytic method, but the reaction time is short, and the transesterification reaction is incomplete. The present invention adopts the stable isotope internal standard method to make up for the problem of incomplete reaction caused by insufficient transesterification time. Although the analysis efficiency is improved, the type of ester in edible oil There are many, the reaction rate varies greatly, and the incomplete transesterification reaction causes a large error in the test results
[0007] Therefore, an efficient, accurate and easy-to-promote quantitative method for fatty acid esters of chloropropanol remains to be explored

Method used

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  • A kind of quantitative method of chloropropanol fatty acid ester
  • A kind of quantitative method of chloropropanol fatty acid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] Standard solution preparation: Take 10.00 mg of 3-chloro-1,2-propane dipalmitate and dilute to volume in a 10 mL volumetric flask to obtain a mother solution with a concentration of 1.000 mg / mL. Dilute the mother liquor sequentially into standard solutions with concentrations of 0.50mg / L, 1.000mg / L, 2.000mg / L, 5.000mg / L, and 10.000mg / L, and then add glycidol and sodium chloride solution to it to make glycidol The concentration of ions was 100 μg / L and the concentration of chloride ions was 21.0 μg / L.

[0079] Dilute 10.00mg of d5-3-chloro-1,2-propanedipalmitate to a 10mL volumetric flask to obtain a mother solution with a concentration of 1.0000mg / mL, and dilute the mother solution gradually to a concentration of 2.000mg / L.

[0080] Experimental steps:

[0081] (1) Sample extraction and water washing: Take 0.5mL standard sample (2.00mg / L) in a centrifuge tube, add 45μL of d5-pp-3-MCPD (the concentration is equivalent to 2.000mg / L of d5-3- MCPD standard solution), 7.0m...

Embodiment 2

[0086] The difference from Example 1 is that the ultrasonic power in the acid-catalyzed transesterification step is 240W, the microwave power is 960W, and the rest of the steps are the same. The specific quantitative analysis results are shown in Table 1.

Embodiment 3

[0088] The difference from Example 1 is that the ultrasonic power in the acid-catalyzed transesterification step is 240W, the microwave power is 1440W, and the rest of the steps are the same. The specific quantitative analysis results are shown in Table 1.

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Abstract

The present invention relates to a kind of quantitative method of chloropropanol fatty acid ester, and described method comprises the following steps: (1) carry out acid-catalyzed transesterification reaction under auxiliary condition with test sample, in described test sample The chloropropanol fatty acid ester is converted into chloropropanol; the auxiliary condition is any one or combination of at least two modes in ultrasonic, light wave and microwave; (2) carry out chloropropanol to the product obtained by acid-catalyzed transesterification Alcohol quantitative analysis; (3) calculate the content of chloropropanol fatty acid ester according to the content of chloropropanol. In the quantification method provided by the invention, the transesterification reaction time is short, the sample is extracted cleanly, and the recovery rate is high, which is an efficient, accurate and easy-to-promote quantification method of chloropropanol fatty acid ester.

Description

technical field [0001] The invention relates to the field of component analysis, in particular to a quantitative method for fatty acid esters of chloropropanol. Background technique [0002] Chloropropanol esters are widely found in various heat-processed foods, such as traditional dishes, cooking oil, French fries, bread, etc. In addition to their own toxicity, chloropropanols can also be produced in the human body, and chloropropanols are harmful to the human body. Liver, kidney, nerve, blood system, reproductive system, etc. have toxic effects, and can cause cancer. As early as 1980, in the research on 3-chloropropanol (3-MCPD), it was found that there was a certain amount of 3-MCPD fatty acid monoester and 3-MCPD fatty acid diester in the seasoning of acid hydrolyzed vegetable protein (HVP liquid) , the content of 3-MCPD diester in the hydrolyzate is much higher than that of 3-MCPD monoester. Until 2004, the detection of 3-MCPD esters in different processed foods cause...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/045G01N2030/062G01N2030/067
Inventor 黄明泉张璟琳吴继红孙宝国李贺贺孙金沅孙啸涛郑福平
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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