HPLC-MSMS method for measuring glyphosate, glufosinate-ammonium and metabolites

Abstract

The invention belongs to the technical field of compound detection, and discloses an HPLC-MSMS (High Performance Liquid Chromatography-Mass Spectrometry Mass Spectrometry) method for measuring glyphosate, glufosinate-ammonium and metabolites, which comprises the following steps: pretreating a to-be-measured actual sample: adding frozen fruits and vegetables and dry ice into a mortar, and grinding into a fine powder state; accurately weighing 5.0 g of sample powder, and adding the sample powder into a 50mL centrifugal tube; adding 10.0 mL of methanol containing 1.0% of formic acid into the centrifugal tube; after shaking the centrifugal tube for 1 minute by hand, violently shaking the centrifugal tube for 5 minutes by adopting a mechanical mode, carrying out centrifugal treatment for 5 minutes at the speed of 8000 rpm, and finally filtering supernate by using a 0.22 mu m filter; a chromatography-mass spectrometry method is developed according to the structural characteristics of the compound; and analyzing the target compound by using a detector. Technical breakthrough is achieved, the key technical problem of a direct method is basically solved, the detection efficiency and the sensitivity of the method are improved, and determination can be completed within 3 minutes.

Description

technical field [0001] The invention belongs to the technical field of compound detection, in particular to an HPLC-MSMS method for determining glyphosate, glufosinate and metabolites. Background technique [0002] At present, the detection of glyphosate, glufosinate and their metabolites has always been a difficult problem. At present, two kinds of derivatization method and LC / MS direct method are mostly reported. The derivatization method has simple technology and low equipment requirements, but its biggest problem is that the derivatization efficiency is not high, the derivatization reaction time is too long, and the detection efficiency is low. The advantages of direct LC / MS determination are convenient pretreatment and high sensitivity, but the biggest technical difficulties are the low ionization efficiency and the problem that glyphosate is easily combined with the metal active site of the chromatography pipeline. Therefore, there is an urgent need to design a novel,...

AI Technical Summary

Problems solved by technology

[0004] (1) In the current derivatization-based method for detecting glyphosate, glufosinate-ammonium and their metabolites, there are problems such as low derivatization efficiency, cumbersome operation, long time, and poor reproducibility

[0005] (2) In the current method for detecting glyphosate, glufosinate-ammonium and their metabolites based on direct liquid chromatography-mass spectrometry, there are problems of low ionization efficiency and easy fusion of glyphosate with the metal active sites of the chromatographic pipeline

[0007] (1) If the sample to be tested is injected directly, the response of glyphosate, glufosinate and its metabolites in mass spectrometry is very low, and a large volume of sample is required, which will lead to tailing of the response peak and inaccurate data

[0008] (2) Glyphosate and its metabolites are highly polar compounds with multiple active sites, which are condensed in the metal pipeline of the liquid chromatography column, which affects the detection results and easily damages the column

[0009] The significance of solving the above problems and defects is: by selecting Raptor Polar X chromatographic column and passivating the pipelines of liquid chromatography and mass spectrometry, a direct and rapid determination of glyphosate, glufosinate and ammonium by HPLC-MSMS is established. The method of its metabolites has high response and good reproducibility, and a single sample detection can be completed in 3 minutes, which overcomes the problem of low response of the direct injection method and solves the problem of low efficiency and poor reproducibility of the pre-column derivatization HPLC-MSMS method question

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