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Method for detecting a plurality of pyrazoles bactericides in wine by solid phase extraction, liquid chromatogram and tandem mass spectrum

A technology of liquid chromatography and tandem mass spectrometry, which is applied in the field of food testing and can solve problems such as threats to human health and high residues

Active Publication Date: 2015-06-17
韩超
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  • Abstract
  • Description
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Problems solved by technology

Although these pyrazole fungicides are relatively friendly to the environment, if they are not used properly in agricultural products, they will cause high residues in food and threaten human health

Method used

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  • Method for detecting a plurality of pyrazoles bactericides in wine by solid phase extraction, liquid chromatogram and tandem mass spectrum
  • Method for detecting a plurality of pyrazoles bactericides in wine by solid phase extraction, liquid chromatogram and tandem mass spectrum
  • Method for detecting a plurality of pyrazoles bactericides in wine by solid phase extraction, liquid chromatogram and tandem mass spectrum

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Embodiment 1

[0037] Include the following steps:

[0038] (1) Preparation of samples to be tested: Weigh 5.0 g of wine samples, add 3 mL of ultrapure water and mix to obtain the solution to be tested;

[0039](2) Solid-phase extraction purification: Take the HLB SPE column, activate the SPE column with methanol and water in sequence, take all the liquid to be tested to the SPE column, and then use 4-6mL water and 4-6mL methanol / water mixed solution (v / v, 2 / 3) Rinse the SPE column, vacuum the SPE column to dryness, elute the SPE column with 6-8mL of methanol to obtain the eluate, concentrate the eluate, and dilute it with 2 mL of methanol The sample solution to be tested is obtained after the pore filter membrane;

[0040] (3) Configuration of standard solution: take penflufen, flufenapyramide, pyraclostrobin, pyrimazole, bixen, and furamet standard products, and prepare them with methanol at a mass concentration of 200 mg / L single-standard stock solution, when used for determination, di...

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Abstract

The invention discloses a method for detecting a plurality of pyrazoles bactericides in wine by solid phase extraction, liquid chromatogram and tandem mass spectrum. The method is capable of simultaneously detecting six pyrazoles bactericides of penflufen, fluxapyroxad, isopyrazam, rabenzazole, bixafen and furametpyr in a wine sample. According to the invention, a liquid to be detected which is obtained by diluting the wine sample through addition of ultrapure water, the liquid to be detected is purified by a HLB solid phase extraction column, a C18 reversed-phase column is used for separating; a target analysis object and ions perform qualitative analysis on information comparison in a multi-reaction monitoring mode by using reservation time; and an internal standard method is used for quantification. The method has the advantages of fast analysis speed, high sensitivity, good reappearance and accuracy, and provides the novel detection method for wine sample quality.

Description

technical field [0001] The invention belongs to the field of food detection, relates to solid-phase extraction-liquid chromatography-tandem mass spectrometry (LC-MS / MS), specifically refers to a kind of penflufen, flufenapyramide and pyraclostrobin in wine , pyrimazole, bixafen, furamet and other six kinds of pyrazole fungicide detection method, especially for wine. Background technique [0002] During the field management of grapes, the main raw material for wine production, a certain amount of pesticides are usually sprayed to prevent the occurrence of diseases and insect pests. Potential health hazard. There are also the above-mentioned problems in fruit juices or other crop processed wines. [0003] Fungicides are a class of low-toxic pesticides used to prevent and control plant diseases caused by various pathogenic microorganisms, mainly referring to fungicides. At present, pyrazole compounds have become one of the hotspots in the development of new fungicides becaus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
Inventor 韩超陈祥准夏碧琪周永芳刘滨刘翠平
Owner 韩超
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