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Gas chromatography triple quadrupole mass spectrometry method for determining coumoxystrobin residual quantity in vegetable food

A technology of triple quadrupole and syringostrobin is applied in the field of gas chromatography triple quadrupole mass spectrometry, and can solve the problem of no detection method for syringylstrobin residue and the like

Inactive Publication Date: 2020-06-16
SUZHOU PUNI TEST TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at present, there is no detection method for the residual amount of syringstrobin in food

Method used

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  • Gas chromatography triple quadrupole mass spectrometry method for determining coumoxystrobin residual quantity in vegetable food
  • Gas chromatography triple quadrupole mass spectrometry method for determining coumoxystrobin residual quantity in vegetable food
  • Gas chromatography triple quadrupole mass spectrometry method for determining coumoxystrobin residual quantity in vegetable food

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Experimental program
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Effect test

Embodiment 1

[0038] 1. Instruments and reagents

[0039] Gas chromatography triple quadrupole mass spectrometer: Agilent 7000D;

[0040] Standard substance: syringstrobin, purity 98%;

[0041] Toluene: analytically pure;

[0042] Acetonitrile: chromatographically pure;

[0043] n-Hexane: pesticide residue grade

[0044] Sodium chloride: analytically pure;

[0045] pesticarb / NH 2 Solid phase extraction cartridge: 500mg / 500mg / 6mL;

[0046] 2. Instrument analysis conditions

[0047] A. Chromatographic conditions:

[0048] Chromatographic column: HP-5MS, 30m*0.25mm*0.25μm;

[0049] Carrier gas flow rate: 1.0mL / min;

[0050] Injection port temperature: 290°C;

[0051] Injection volume: 1.0μL;

[0052] Injection method: pulse splitless 25psi;

[0053] Heating program: 60°C initial temperature, 40°C / min to 310°C, hold for 10 minutes;

[0054] B: Mass spectrometry conditions:

[0055] Ion source: EI source;

[0056] Detection method: MRM multiple reaction monitoring;

[0057] Colli...

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Abstract

The invention, which belongs to the technical field of food safety, relates to a gas chromatography triple quadrupole mass spectrometry method for determining the coumoxystrobin residual quantity in vegetable food. The method comprises the following steps: weighing a uniform sample; carrying out homogenate extraction with acetonitrile; carrying out salting-out centrifugation; taking half of a supernatant, carrying out concentrating to be nearly dry; dissolving residues in a toluene-acetonitrile mixed solution, carrying out purifying with a solid-phase extraction column, and carrying out eluting with the toluene-acetonitrile mixed solution; carrying out solvent replacement, carrying out machine detection, carrying out qualitative processing of an ion pair and retention time determination; and carrying out quantifying with an external standard method. The detection method has the advantages of simple pretreatment steps, good impurity removal effect, high sensitivity, high recovery rate and good precision of the determination result, and can effectively detect the residual amount of coumoxystrobin in vegetable food.

Description

technical field [0001] The invention belongs to the technical field of food safety, and in particular relates to a gas chromatography triple quadrupole mass spectrometry method for determining the residual amount of syringstrobin in vegetable foods. [0002] technical background [0003] Syringstrobin, the chemical name is methyl N-methoxy-N-{2-[(3,5,6-trichloro-2-pyridyloxy)methyl]phenyl}formate, and the CAS registration number is 850881 -70-8, 96% of the original drug is milky white or light yellow powder, melting point 109 ~ 111 ℃, easily soluble in DMF, acetone, ethyl acetate, methanol, slightly soluble in petroleum ether, almost insoluble in water, not easy at room temperature break down. [0004] Syringostycin was developed by Shenyang Research Institute of Chemical Industry and a methoxyacrylate fungicide developed by Jilin Bada Pesticide Co., Ltd. It is mainly composed of natural product coumarin groups and acrylate groups. Its synthesis process does not use any harm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047G01N2030/062
Inventor 彭剑秋
Owner SUZHOU PUNI TEST TECH CO LTD