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Method for measuring residual quantities of amitraz in royal jelly and metabolites of amitraz by liquid chromatography-mass spectrography/mass spectrometry

A technology of metabolites and liquid chromatography, which is applied in the field of liquid chromatography-mass spectrometry/mass spectrometry to determine the residues of amitraz and its metabolites in royal jelly, which can solve the problems of mutagenicity, large liver damage, toxic and side effects, etc.

Active Publication Date: 2017-08-29
ZHEJIANG ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE
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Problems solved by technology

2,4-Dimethylaniline is usually used as a raw material for the synthesis of monoformamidine and amitraz in chemical synthesis, which has toxic side effects and mutagenicity. Studies have shown that 2,4-Dimethylaniline is harmful to the liver Larger damage
[0020] There are no standard methods and research reports on the determination of amitraz and its metabolite residues in royal jelly by liquid chromatography-mass spectrometry / mass spectrometry

Method used

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  • Method for measuring residual quantities of amitraz in royal jelly and metabolites of amitraz by liquid chromatography-mass spectrography/mass spectrometry
  • Method for measuring residual quantities of amitraz in royal jelly and metabolites of amitraz by liquid chromatography-mass spectrography/mass spectrometry
  • Method for measuring residual quantities of amitraz in royal jelly and metabolites of amitraz by liquid chromatography-mass spectrography/mass spectrometry

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Embodiment Construction

[0070] The specific embodiments of the present invention will be described in detail below in conjunction with the drawings.

[0071] 1 Extraction:

[0072] Weigh 2.0g (accurate to 0.01g) of royal jelly sample into two 50mL poly-plug centrifuge tubes, add isotope internal standard, add 8mL 5% ammonia solution, 2,000 rpm, vortex and mix for 5 minutes, let stand for 5 Add 10 mL of 5% ammonia acetonitrile solution, 2000 rpm, vortex and mix, let stand for 5 minutes, dilute to 20 mL, vortex and mix for 5 minutes, centrifuge at 8,500 rpm, and transfer 2.0 mL of the supernatant , Add 2mL 5% ammonia acetonitrile solution and mix, vortex to mix, centrifuge at 8,500 rpm, take the supernatant to be purified.

[0073] Due to the instability of amitraz, the stability of the compound is first investigated. In addition, due to the particularity of royal jelly samples, it is usually necessary to remove protein from the sample to reduce protein pair determination when determining drug residues in ro...

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Abstract

The invention relates to a detecting method for measuring residual quantities of amitraz in royal jelly and metabolites of the amitraz, in particular to a method for measuring the amitraz, N-(2,4-dimethylphenyl)-N'-methylfomamidine, N-(2,4-dimethylphenyl) formamide and 2,4-dimethylaniline in the royal jelly by liquid chromatography-mass spectrography / mass spectrometry. The method for measuring the residual quantities of the amitraz in the royal jelly and the metabolites of the amitraz by the liquid chromatography-mass spectrography / mass spectrometry comprises the following steps: adding ammoniation water in a test specimen for diluting; then precipitating protein by using ammoniac acetonitrile and extracting the protein; purifying an extracting solution by using a neutral alumina solid phase extraction column; adopting a liquid chromatography-mass spectrography / mass spectrometer for detecting; quantifying the amitraz and the 2,4-dimethylaniline by an internal standard method; quantifying the N-(2,4-dimethylphenyl)-N'-methylfomamidine and the N-(2,4-dimethylphenyl) formamide by an external standard method. The sensitivity of the method can meet detection and verification requirements of the residual quantities of the amitraz in the royal jelly and the metabolites of the amitraz.

Description

Technical field [0001] The invention relates to a detection method for bisformamidine and its metabolite residues in royal jelly, in particular to a liquid chromatography-tandem mass spectrometry method for simultaneous determination of bisformamidine and monoformamidine 2,4-dimethylphenylformamide in royal jelly And 2,4-dimethylaniline. Background technique [0002] Royal jelly (royal jelly), also known as royal jelly, royal jelly, royal jelly, and bee jelly, is the secretion of the pharyngeal glands of young worker bees that nurture larvae in the bee nest. It is the food for the larvae that will become queen bees. The queen bee's lifelong food. Royal jelly is like mammalian milk with great nutritional value and immune function, and contains extremely high longevity factors. Nutritionists believe that royal jelly is a super nutritious food with high active ingredients that can be taken directly by humans. In recent years, studies have shown that royal jelly has medical and he...

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72
Inventor 侯建波谢文张文华李杰张兴涛姚滨滨洪灯
Owner ZHEJIANG ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE
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