Pretreatment purifying method for gas chromatography-mass spectrometry pesticide residue detection

Abstract

The invention discloses a pretreatment purifying method for gas chromatography-mass spectrometry pesticide residue detection. The pretreatment purifying method includes the following steps that an evenly-smashed sample is weighed and put into a centrifugal tube, acetonitrile is added into a centrifugal tube, and then the centrifugal tube is put into a high-speed dispersion machine and subjected tohigh-speed homogenate; sodium chloride and anhydrous magnesium sulfate continue to be added into the centrifugal tube, medium-speed homogenate or violent vibration continues to be carried out, then the centrifugal tube is centrifuged, solution acetonitrile and an aqueous phase in the centrifugal tube are layered, and an extracting solution is obtained; the extracting solution is taken and added into the centrifugal tube, methylbenzene is added for constant volume, then a purifying bag is added, violent vibration and centrifugation are carried out, and supernatant is obtained; the supernatantis taken, an internal standard is added, and the mixture is mixed to be even to be measured; pesticide residues of the to-be-measured supernatant mixed to be even are detected through a gas chromatograph-mass spectrometer. By means of the pretreatment purifying method for gas chromatography-mass spectrometry pesticide residue detection, the stability of measured pesticides can be improved, the peak shape is optimized, the problem that as sample impurities are complex, a response of a target object is reduced, and the peak shape is poor, the tolerance of a liner tube is poor is solved, the replacement frequency of the liner tube is reduced, and the detection cost is reduced.

Description

technical field [0001] The invention relates to the technical field of product detection, in particular to a pretreatment and purification method for detection of pesticide residues by gas chromatography-mass spectrometry. Background technique [0002] GC-MS is an instrument that combines gas chromatograph and mass spectrometer. GC-MS is widely used in the separation and identification of complex components. It has the high resolution of GC and the high sensitivity of mass spectrometry. It is a biological An effective tool for the qualitative and quantitative determination of drugs and metabolites in samples. Among them, the inlet end of the GC / MS instrument mainly includes the supporting capillary and liner. The liner is a common consumable for GC and GCMS, but the price is not cheap. In normal use, the liner needs to be replaced every 30 samples. The detection efficiency is reduced, and the detection cost is also increased. [0003] In the existing techniques for the det...

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Problems solved by technology

[0004] The present invention aims to solve the problems of the existing technique of gas chromatography-mass spectrometry for the determination of pesticide residues, which consume more organic matter in the pretreatment and extraction process, has high requirements for environmental protection, high purification costs, and frequent instrument maintenance, and provides a method for reducing the amount of organic matter used. Environmentally friendly, simple, efficient, high detection stability and precision, and low detection cost pretreatment purification method for detection of pesticide residues by GC

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