Method of simultaneously measuring amounts of ten kinds of nicotinic medicine residues in royal jelly by liquid chromatography-tandem mass spectrometry

A technology of tandem mass spectrometry and liquid chromatography, which is applied in the field of simultaneous determination of 10 kinds of nicotinic drug residues in royal jelly by liquid chromatography tandem mass spectrometry, can solve the problems that the determination of nicotinic drug residues has not yet been retrieved

Inactive Publication Date: 2017-11-10
THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

However, no research reports on the determination of nicotinic drug residues in royal jelly have been retrieved

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  • Method of simultaneously measuring amounts of ten kinds of nicotinic medicine residues in royal jelly by liquid chromatography-tandem mass spectrometry
  • Method of simultaneously measuring amounts of ten kinds of nicotinic medicine residues in royal jelly by liquid chromatography-tandem mass spectrometry
  • Method of simultaneously measuring amounts of ten kinds of nicotinic medicine residues in royal jelly by liquid chromatography-tandem mass spectrometry

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Embodiment Construction

[0053] Liquid chromatography tandem mass spectrometry is a method for simultaneously determining 10 kinds of nicotinic drug residues in royal jelly, the method comprising the following steps:

[0054] 1. Extraction

[0055] For the detection of royal jelly samples, protein precipitation in the sample is a key step in pretreatment. The present invention compares the extraction methods of trichloroacetic acid precipitation protein and organic solvent precipitation protein extraction. Adding trichloroacetic acid directly to royal jelly for protein precipitation and purification, the extraction solvent is difficult to remove by concentration under reduced pressure, dinotefuran and thiacloprid cannot be effectively extracted, and the extraction recovery rate of acetamiprid is about 30%. Organic solvent precipitation protein test investigated methanol and acetonitrile precipitation protein respectively, the study found that there was no significant difference in the effect of methan...

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Abstract

The invention relates to a measuring method of amounts of multiple nicotinic medicine residues in royal jelly, in particular to a method of simultaneously measuring amounts of ten kinds of nicotinic medicine residues in royal jelly by a liquid chromatography-tandem mass spectrometry. The method comprises the steps of diluting a sample with water and participating protein preliminarily, and further participating and extracting the protein by using methyl alcohol, wherein measurement is carried out by the adoption of the liquid chromatography-tandem mass spectrometry, and quantity determination is performed by the adoption of an external standard method and an isotope internal standard dilution method in a preprocessing process of HLB solid-phase extraction purification. The method of simultaneously measuring the amounts of the ten kinds of nicotinic medicine residues in the royal jelly by the liquid chromatography-tandem mass spectrometry is simple, convenient and fast, small in resource consumption, and low in measuring cost. The preprocessing process, relevant compounds and instruments required by measurement are complementary to those in an existing method, so that the requirements for simultaneously measuring the amounts of the nicotinic medicine residues in the royal jelly are met, and a powerful technical guarantee can be further provided for maintaining food safety and ensuring the royal jelly quality.

Description

technical field [0001] The invention relates to a detection method for the determination of multiple nicotinic drug residues in royal jelly, in particular to a method for simultaneously measuring 10 kinds of nicotinic drug residuals in royal jelly by liquid chromatography tandem mass spectrometry. Background technique [0002] New-type nicotinic drugs belong to a class of new-type broad-spectrum insecticides with high efficiency, low toxicity, strong systemic property, long residual effect and low residue. They occupy a high share in the market and are widely used in rice, corn, etc. , pumpkin and other crops pest control. Since the mid-1980s, the first neonicotinoid insecticide imidacloprid was successfully developed by German Bayer company, and so far more than a dozen products have been commercialized or are about to be commercialized, such as dinotefuran (dinotefuran), thiophene, etc. Clothianidin (clothianidin), imidacloprid (imidacloprid), acetamiprid (acetamiprid, al...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/38
CPCG01N30/88G01N30/38G01N2030/388
Inventor 侯建波谢文张文华洪灯盛涛陆顺李杰
Owner THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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