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Detection method for simultaneously measuring residue of chlordimeform and 4-chloro-2-methylaniline as metabolite thereof in royal jelly

A technology for metabolites and detection methods, applied in the detection field of simultaneous determination of chlordimeform and its metabolite 4-chloro-o-toluidine in royal jelly, capable of solving the problem of chlordimeform and its metabolite 4-chloro-o-toluidine Problems such as the residue cannot be detected at the same time

Inactive Publication Date: 2009-11-04
THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

[0006] In order to solve the difficult problem that the residual amount of dimeform and its metabolite 4-chloro-o-toluidine in the existing royal jelly cannot be detected simultaneously, the object of the present invention is to provide a gas chromatography-mass spectrometry method for the simultaneous determination of dimeform and its metabolism in royal jelly. The detection method for the residue of 4-chloro-o-toluidine, which does not need to be converted, can simultaneously measure the residue of chlordimeform and its metabolite 4-chloro-o-toluidine, which is accurate, sensitive and simple

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  • Detection method for simultaneously measuring residue of chlordimeform and 4-chloro-2-methylaniline as metabolite thereof in royal jelly
  • Detection method for simultaneously measuring residue of chlordimeform and 4-chloro-2-methylaniline as metabolite thereof in royal jelly

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Embodiment Construction

[0024] A detailed description will be given below of specific embodiments of the present invention.

[0025] The present invention simultaneously measures the detection method of chlordimeform and its metabolite 4-chloro-o-toluidine residue in royal jelly, the method comprises the following steps:

[0026] 1. Extraction

[0027] Weigh 2 g of the sample (accurate to 0.01 g) into a 50 mL centrifuge tube, add 10 mL of trichloroacetic acid solution (3.8), vortex and mix for 1 min, and centrifuge at 8000 r / min for 3 min. Transfer the upper aqueous phase to another 50mL centrifuge tube, add about 4mL of sodium hydroxide solution (3.9) to adjust the pH to greater than 12. Add 5 g of sodium chloride and 20 mL of n-hexane-acetone (1+1, v / v) mixed solvent, vortex and mix for 1 min, and transfer the upper organic phase into a concentrating bottle. Then add 20 mL of n-hexane-acetone (1+1, v / v) mixed solvent to the water phase, repeat the extraction once, combine the upper organic phase,...

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Abstract

The invention relates to a detection method for simultaneously measuring the residue of chlordimeform and 4-chloro-2-methylaniline as the metabolite thereof in royal jelly, in particular to a detection method for measuring the residue of chlordimeform and 4-chloro-2-methylaniline as the metabolite thereof in the royal jelly by the gas chromatography-mass spectrometry (GC-MS). The method comprises the following steps: precipitating protein by a trichloroacetic acid solution; then, adjusting the pH value until the solution is alkaline; further purifying the solution by the liquid-liquid partition using acetonitrile / n-hexane; and measuring the residue by the GC-MS. The residue of chlordimeform and 4-chloro-2-methylaniline as the metabolite thereof in the solution to be measured can be measured in a way that chlordimeform and 4-chloro-2-methylaniline as the metabolite thereof coexist without conversion, therefore, the invention has the characteristics that the method is accurate, sensitive and simple.

Description

technical field [0001] The invention relates to a detection method for simultaneously determining the residues of chlordimeform and its metabolite 4-chloro-o-toluidine in royal jelly, in particular to the gas chromatography-mass spectrometry method for determining the residues of chlordimeform and its metabolite 4-chloro-o-toluidine in royal jelly Quantitative detection method. Background technique [0002] Dimeform is a formamidine insecticide and acaricide. Due to its potential carcinogenicity to humans, it is listed as a highly toxic insecticide. Most countries and regions in the world have set strict maximum residue limits for dimeform in food. Since the European Union and Japan have not stipulated the maximum residue limit of dimeform in royal jelly, the uniform standard (0.01mg / kg) is used as the maximum residue limit. The United Nations Codex Committee (CAC) stipulates that the residual amount of chlordimeform should be the sum of its metabolites. [0003] Most of ...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N1/28G01N30/28
Inventor 丁慧瑛谢文陈笑梅蒋晓英周召千
Owner THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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