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UPLC-MS/MS method for analyzing residues of meconazole and pyraclostrobin in grapes

A technology for pyraclostrobin and pyraclostrobin is applied in the field of pesticide residue determination, can solve the problems of high cost, low recovery rate, time-consuming and the like, and achieves the effects of low cost, simple operation and good purification effect

Inactive Publication Date: 2022-01-18
TIANJIN INSTITUE OF QUALITY STANDARD & TESTING OF AGRICULTUAL PRODS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solid-phase extraction method is time-consuming and costly, and the QuEChERS method is simple to operate. However, due to the structure containing Cl and F atoms in the structure of chloroflufeconazole, it is easily absorbed by PSA and NH. 2 Adsorption, resulting in lower recovery

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  • UPLC-MS/MS method for analyzing residues of meconazole and pyraclostrobin in grapes
  • UPLC-MS/MS method for analyzing residues of meconazole and pyraclostrobin in grapes
  • UPLC-MS/MS method for analyzing residues of meconazole and pyraclostrobin in grapes

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Experimental program
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Embodiment 1

[0033] 400 g / L chlorofluoroconazole · pyraclostrobin suspension concentrate, the preparation was diluted 1500 times, applied 3 times, with an interval of 7 days between applications, and the grape sample collected 7 days after the last application was used as the sample. The inventive method carries out sample pretreatment and ultra-high performance liquid chromatography-tandem mass spectrometry determination. The preparation method is as follows:

[0034] 1. Instruments and reagents:

[0035] Waters Acquity, USA TM UPLC I-Class ultra-high performance liquid chromatography, Xevo TQ-S triple quadrupole mass spectrometer; Swiss Mettler electronic balance (sensitivity 0.00001g and 0.01g); Tormorgen high-throughput tissue grinder; Vortex mixer; Benchtop High-speed centrifuge; American Milli-Q ultrapure water instrument.

[0036] The purity of the standard product of flufeconazole is 99.7%, and the purity of the standard product of pyraclostrobin is 99.9%. Acetonitrile and form...

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Abstract

A UPLC-MS / MS method for analyzing residues of meconazole and pyraclostrobin in grapes is characterized in that a QuEChERS method is replaced with a dilution method for purification, the matrix effect is eliminated, the problem that the recovery rate of meconazole is low due to QuEChERS purification is solved, a sample is extracted through acetonitrile, an extracting solution is salted out, an upper-layer organic phase is taken and diluted with 0.1% formic acid, and ultra-high performance liquid chromatography-tandem mass spectrometer (UPLC-MS / MS) detection is conducted. The method disclosed by the invention can be used for residue analysis of the meconazole and the pyraclostrobin in the grapes, has the advantages of simplicity, rapidness, low cost and the like, and is good in purification effect and high in sensitivity, and both the accuracy and the precision meet the requirements of a multi-residue analysis method.

Description

Technical field: [0001] The invention belongs to the technical field of determination of pesticide residues in agricultural products, and relates to a determination method for the residues of chlorofluconazole and pyraclostrobin in grapes. Background technique: [0002] Mefentrifluconazole is a new triazole fungicide developed by BASF with the development code BAS750F. This species is the first triazole fungicide on the market for more than 10 years after prothioconazole. The unique isopropanol group in the molecule enables it to freely rotate from a free state to a combined state with a target. It can well inhibit the transfer of Septoria sp., reduce the mutation of pathogens, and delay the emergence and development of resistance. It has systemic conductivity and has both protective and therapeutic effects. Compared with other azole fungicides, chlorofluconazole not only has higher activity; but also has better environmental characteristics, and its toxicity to mammals, be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72
CPCG01N30/02G01N30/72
Inventor 李娜马颖郭永泽张玉婷邵辉刘磊李辉李晋津卢娜张圆圆
Owner TIANJIN INSTITUE OF QUALITY STANDARD & TESTING OF AGRICULTUAL PRODS