Method for simultaneously determining residual quantities of amitraz and metabolites in royal jelly through dispersive solid phase extraction-liquid chromatography-mass spectrometry/mass spectrometry method

A liquid chromatography and disperse solid-phase technology, which is applied in the field of determination of amitraz and its metabolite residues in royal jelly, can solve the problems of large liver damage, toxic side effects, mutagenicity, etc., and achieve low resource consumption and food maintenance. Safety and low detection cost

Inactive Publication Date: 2018-12-14
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, but studies have shown that 2,4-Dimethylaniline has toxic side effects and mutagenicity, and is harmful to the liver. Larger damage
However, the patent still needs to be improved in terms of detection speed, green detection and cost saving

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  • Method for simultaneously determining residual quantities of amitraz and metabolites in royal jelly through dispersive solid phase extraction-liquid chromatography-mass spectrometry/mass spectrometry method
  • Method for simultaneously determining residual quantities of amitraz and metabolites in royal jelly through dispersive solid phase extraction-liquid chromatography-mass spectrometry/mass spectrometry method
  • Method for simultaneously determining residual quantities of amitraz and metabolites in royal jelly through dispersive solid phase extraction-liquid chromatography-mass spectrometry/mass spectrometry method

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Embodiment Construction

[0037] Dispersive solid phase extraction-liquid chromatography-mass spectrometry / mass spectrometry is a method for simultaneous determination of bisformamidine and its metabolites in royal jelly. The method includes the following steps:

[0038] One, extraction

[0039] Due to the instability of amitraz, it is necessary to first investigate the stability of the compound under the extraction conditions. Due to the particularity of royal jelly samples, protein precipitation is a key step of pretreatment. Therefore, it is necessary to determine the drug residues in royal jelly samples. Remove protein treatment from the sample to reduce the influence of protein on the determination. The experiment comprehensively investigated the effect of organic solvent precipitation and extraction of protein in acidic solution, neutral solution and alkaline solution environment. The study found that acid solution (pH=5) bisformamidine is prone to hydrolysis, and the recovery rate is less than 30%, a...

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Abstract

The invention relates to a method for determining residual quantities of amitraz and three metabolites thereof in royal jelly, in particular to a method for simultaneously determining the residual quantities of the amitraz and the metabolites in royal jelly through a dispersive solid phase extraction-liquid chromatography-mass spectrometry / mass spectrometry method. The method includes the steps that after a buffer solution with pH being 9 is added into a sample to conduct diluting, and protein precipitation, extraction, and salt precipitation are carried out through acetonitrile and sodium chloride; dispersive solid phase extraction is conducted through an adsorbent containing N-propyl ethylenediamine (PSA), anhydrous magnesium sulfate and C18 powder to purify an extraction solution, detection is carried out through a liquid chromatography-mass spectrometry / mass spectrometer, and quantifying is carried out through an isotope internal standard dilution method. The method is environmentally friendly, easy, convenient and quick, small in resource consumption, and low in detection cost, and the sensitivity of the method can meet the requirements of detection and confirmation of the residual quantities of the amitraz and the metabolites thereof in the royal jelly.

Description

Technical field [0001] The invention relates to a method for determining the residual amount of bisformamidine and its metabolites in royal jelly, in particular to a dispersive solid phase extraction-liquid chromatography-mass spectrometry / mass spectrometry method for the simultaneous determination of bisformamidine and monoformamidine in royal jelly 2,4- Method for residual amounts of dimethylphenylformamide and 2,4-dimethylaniline. Background technique [0002] Royal jelly (royal jelly) is the secretion of the pharyngeal glands of young worker bees that nurture larvae in the bee nest. It is also the food for the larvae that will become queen bees and the queen bee's lifelong food. Studies have found that 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 ye...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 侯建波谢文洪灯张文华钱艳江鹏盛涛韩超
Owner ZHEJIANG ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE
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