Liquid chromatography-tandem mass spectrometry method for determining coumoxystrobin residual quantity in vegetable food

A technology of syringstrobin and tandem mass spectrometry, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., and can solve the problems of no detection method for syringstrobin residues, etc.

Inactive Publication Date: 2020-06-16
杭州谱尼检测科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But at present, there is no detection method f

Method used

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  • Liquid chromatography-tandem mass spectrometry method for determining coumoxystrobin residual quantity in vegetable food
  • Liquid chromatography-tandem mass spectrometry method for determining coumoxystrobin residual quantity in vegetable food
  • Liquid chromatography-tandem mass spectrometry method for determining coumoxystrobin residual quantity in vegetable food

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Embodiment 1

[0032] 1. Instruments and reagents

[0033] High performance liquid chromatography-tandem mass spectrometer: American Waters, UPLC-Xevo TQ;

[0034] Standard substance: syringstrobin, purity 98%;

[0035] Methanol: chromatographically pure;

[0036] Acetonitrile: chromatographically pure;

[0037] Formic acid: analytically pure

[0038] Anhydrous magnesium sulfate: analytically pure;

[0039] HLB solid phase extraction cartridge: 6mL, 200mg;

[0040] The water used in this method is primary water.

[0041] 2. Instrument analysis conditions

[0042] The chromatographic column is Waters, BEH C18, 1.7μm, 2.1mm×50mm

[0043] The mobile phase is 0.1% formic acid aqueous solution and 0.1% formic acid acetonitrile solution, gradient elution;

[0044] The flow rate is 0.3mL / min;

[0045] The injection volume is 5.0 μL;

[0046] The column temperature is 40°C;

[0047] Gradient elution: initial mobile phase ratio, 0.1% formic acid aqueous solution; 0.1% formic acid acetonitr...

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Abstract

The invention, which belongs to the technical field of food safety, relates to a method for detecting the residual amount of coumoxystrobin in vegetable food. The method comprises the following steps:weighing a uniform sample; carrying out homogeneous extraction with a methanol solution; carrying out purifying with anhydrous magnesium sulfate and an N-propylethylenediamine solid phase adsorbent;carrying out high-speed refrigerated centrifugation, carrying out supernatant rotary evaporation to be nearly dry, dissolving residues with methanol, carrying out purifying with an HLB purification column; blowing eluted liquid nitrogen to be dry; carrying out dissolving with a mobile phase, fixing the volume, carrying out filtering with a 0.22micron organic filter membrane, and waiting for detection; detecting a to-be-detected substance by using a liquid chromatograph-mass spectrometer, and carrying out quantifying by using an external standard method. The detection method provided by the invention has the advantages of simple and novel pretreatment steps, good impurity removal effect, high sensitivity, high recovery rate and good precision of determination results, 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 method for determining the residual amount of syringstrobin in vegetable food by liquid chromatography tandem mass spectrometry. Background technique [0002] Syringstrobin, chemical name: (E)-2-(2-(3-n-butyl-4methyl-coumarin-7-yloxy)methylphenyl)-3-methoxyacrylic acid Methyl ester, the high-purity technical drug is milky white or light yellow powder, melting point 109-111°C, easily soluble in DMF, acetone, methanol, slightly soluble in petroleum ether, almost insoluble in water. It is not easy to decompose under normal temperature conditions. [0003] It is a high-end fungicide developed by Shenyang Research Institute of Chemical Industry and Jilin Bada Pesticide Co., Ltd., which belongs to methoxyacrylate. It is a protective fungicide and has certain therapeutic effects. It has the characteristics of broad spectrum, low toxicity, high efficiency and safety, ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 李庆熊敏
Owner 杭州谱尼检测科技有限公司
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