Method for simultaneously measuring residue amounts of various neonicotine type drugs in royal jelly and metabolites thereof

A new technology of nicotine and metabolites, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of long pretreatment time, high price, high equipment cost and time cost, and achieve simple, low cost and easy purification process. effect of operation

Inactive Publication Date: 2018-12-28
ZHEJIANG ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, the price of the HLB solid-phase extraction column used in the solid-phase extraction technology is relatively high, and the price on the general market is about 70 yuan/piece (and it is f...

Method used

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  • Method for simultaneously measuring residue amounts of various neonicotine type drugs in royal jelly and metabolites thereof
  • Method for simultaneously measuring residue amounts of various neonicotine type drugs in royal jelly and metabolites thereof
  • Method for simultaneously measuring residue amounts of various neonicotine type drugs in royal jelly and metabolites thereof

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Experimental program
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Embodiment 1

[0098] This embodiment is a method for simultaneously determining the residues of multiple new-type nicotinoids and their metabolites in royal jelly. This embodiment can simultaneously detect the residues of 10 new-type nicotinoids and two metabolites in royal jelly , the basic information of these 10 new nicotinic drugs and 2 metabolites are shown in Table 1.

[0099] Table 1 Basic information of various compounds

[0100]

[0101] The method includes the following steps:

[0102] (1) Add a protein remover to the sample to be tested, vortex, and centrifuge to get the supernatant to obtain an extract;

[0103] When detecting neonicotinoid drug residues in royal jelly samples, protein precipitation in samples is a key step in pretreatment. In this example, trichloroacetic acid-precipitated proteins and organic solvent-precipitated proteins were compared to determine the optimal protein precipitation method , the comparison results are as follows:

[0104] When trichloroac...

Embodiment 2

[0123] Embodiment 2 recovery test

[0124] Add known amounts of novel nicotinoids and metabolites to royal jelly that does not contain the above-mentioned 10 novel nicotinoids and 2 metabolites, and perform pretreatment on royal jelly according to the method of Example 1 to obtain the liquid; according to the standard curve of embodiment 1, adopt the liquid chromatography tandem mass spectrometry condition of embodiment 1 to detect the content of each novel nicotinic drug and metabolite in the liquid to be tested, carry out recovery rate experiment:

[0125] Recovery rate (%)=(recovery amount-content in blank sample) / scaling amount×100%;

[0126] Each test was repeated six times in parallel, and the recovery test results are shown in Table 4.

[0127] The total ion chromatogram is as figure 1 As shown, the selective ion chromatogram of each compound is as follows Figures 2a-2z and Figures 3a-3d shown.

[0128] Table 4 Addition levels, recoveries and precision of 10 ne...

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Abstract

The invention discloses a method for simultaneously measuring residue amounts of various neonicotine type drugs in royal jelly and metabolites thereof. The method comprises the following steps of: (1)removing protein in a to-be-measured sample to obtain extract; (2) carrying out purification on the extract by adopting an absorbent to obtain purified solution, and after drying the purified solution, making up to volume with a loading solvent to obtain to-be-measured solution, wherein the absorbent is formed by mixing anhydrous magnesium sulfate, N-primary secondary amine and C18 powder in a mass ratio of 10:6:3; (3) drawing a standard curve; and (4) carrying out sample injection on the to-be-measured solution under a preset liquid chromatography tandem mass spectrometry condition, and according to the standard curve and a detection result of the to-be-measured solution, calculating content of the corresponding neonicotine type drugs or metabolites in the to-be-measured solution. According to the invention, a dispersive solid-phase extraction purification technology is adopted to carry out purification on the extract; the method is simple and convenient in step, easy to operate, green and friendly; purification only requires 5 to 10 minutes; extraction efficiency is high; cost of consumables is only 5 to 7 yuan each time; and cost is low.

Description

technical field [0001] The invention belongs to the technical field of bee product quality detection and safety monitoring, and in particular relates to a method for simultaneously measuring the residues of various new-type nicotinic drugs and their metabolites in royal jelly. Background technique [0002] New neonicotinoid insecticides occupy a high share in the global market, and they are widely used in the pest control of rice, corn, pumpkin and other crops. Since the first neonicotinoid insecticide imidacloprid came out in the 1980s, more than a dozen products have been commercialized or will be commercialized so far, such as dinotefuran (dinotefuran), clothianidin (clothianidin), imidacloprid ( imidacloprid), acetamiprid (also known as acetamiprid), etc. [0003] Because the use of new neonicotinoid insecticides will pollute the nectar source plants, and then be enriched in the body of bees, which will cause harm to the body functions of bees. Studies have found that w...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/54
CPCG01N30/02G01N30/06G01N30/54G01N2030/027G01N2030/062
Inventor 侯建波谢文钱艳洪灯盛涛毛壬熠韩超张文华
Owner ZHEJIANG ACAD OF SCI & TECH FOR INSPECTION & QUARANTINE
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