Method for splitting and determining chiral pesticide quizalofop-ethyl and fluazifop-butyl enantiomers by super high performance combined chromatography-tandem mass spectrometry

A technology of fluazifop-pyr and ultra-high-efficiency phase combination, which is applied in the field of analytical chemistry and can solve problems such as poor separation of fluazifop-pyr and long analysis time

Active Publication Date: 2018-08-14
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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AI Technical Summary

Problems solved by technology

[Pesticides, 2012, 51(3), 193-196] used supercritical fluid chromatography to separate these two types of pesticides, but the analysis time was as long as 50 minutes, and the separation of fluazifop-methyl was not good

Method used

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  • Method for splitting and determining chiral pesticide quizalofop-ethyl and fluazifop-butyl enantiomers by super high performance combined chromatography-tandem mass spectrometry
  • Method for splitting and determining chiral pesticide quizalofop-ethyl and fluazifop-butyl enantiomers by super high performance combined chromatography-tandem mass spectrometry
  • Method for splitting and determining chiral pesticide quizalofop-ethyl and fluazifop-butyl enantiomers by super high performance combined chromatography-tandem mass spectrometry

Examples

Experimental program
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Effect test

example 1

[0036] 1. Instruments and reagents:

[0037] Acetonitrile, ethanol, and methanol are chromatographic grade reagents, and sodium citrate and sodium chloride are analytical reagents; distilled water meets the requirements of first-grade water in GB / T 6682.

[0038] Waters TQD quadrupole tandem mass spectrometer; water bath constant temperature oscillator; Swiss Mettler AE 163 electronic balance (sensitivity: 0.0001g).

[0039] 2. Sample handling:

[0040] Accurately weigh 2 g of the ground tobacco powder sample into a 50 mL capped centrifuge tube, add 10 mL of water, add 10 mL of acetonitrile after soaking, then place the centrifuge tube on a vortex mixer and vibrate at a rate of 2000 rpm 5 min. Then add 5 g of anhydrous magnesium sulfate, 1 g of sodium chloride, 1 g of sodium citrate and 0.5 g of disodium hydrogen citrate to the centrifuge tube, and immediately oscillate at a rate of 2000 rpm for 5 min, then centrifuge at 6000 rpm for 3 min; pipette 1.0 mL of the supernata...

example 2

[0049] Grain samples were selected as described in Example 1, and fluazifop-p-p and quizalofop-p-p were not detected in the samples.

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PUM

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Abstract

The invention belongs to the field of analytical chemistry and the technical field of pesticide residue detection, particularly discloses a method for splitting and determining chiral pesticide quizalofop-ethyl and fluazifop-butyl enantiomers by super high performance combined chromatography-tandem mass spectrometry, and relates to a splitting and quantifying method for enantiomers of chiral pesticides. According to the method, quizalofop-ethyl and fluazifop-butyl in tobacco and dried fruit are extracted by adopting a QuEChERS method; enantiomers of two chiral pesticides of the quizalofop-ethyl and the fluazifop-butyl are simultaneously detected by combining combined chromatography chiral stationary phase with triple quadrupole tandem mass spectrometry; the detection limits of the method are respectively 0.0018 and 0.0016 mg/kg. By the method, the quizalofop-ethyl and the fluazifop-butyl are chirally separated rapidly by adopting combined chromatography for the first time; the use of alarge number of organic solvents is reduced by taking supercritical CO2 as a moving phase, so that the method is green and environmentally friendly. The method provided by the invention is high in analysis speed by adopting the combined chromatography; the time consumption is only five minutes; the sensitivity is high; the separation degree between chiral isomers is high.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and the technical field of pesticide residue detection, and specifically relates to a method for splitting and measuring the enantiomers of quizalofop-p-p and fluazifop-p-p-methyl in an ultra-high-efficiency convergence chromatography-tandem mass spectrometry technology, involving many A method for the resolution and quantification of the enantiomers of a chiral pesticide. Background technique [0002] 25% of the currently used pesticides are chiral, and there are enantiomeric differences in the biological activities of chiral pesticides, and their activity often exists in only one or a few enantiomers, while the enantiomers Dissolution and fate in the environment are often also significantly different. That is, there may be huge differences in the activity, toxicity, absorption, metabolism, and degradation of chiral pesticide enantiomers in the natural environment and organisms. [0003] Flu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 杨飞唐纲岭邓惠敏边照阳李中皓范子彦王颖刘珊珊
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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