Method for splitting and measuring enantiomer of chiral pesticide benalaxyl through ultra-performance convergence chromatography-tandem mass-spectrometric technique

An ultra-efficient phase convergence and tandem mass spectrometry technology, which is applied in the resolution and quantification of racemates, can solve the problems of cumbersome synthesis of chiral columns, long separation time, and consumption of organic solvents, etc., to achieve separation and fast analysis speed , the effect of high sensitivity

Active Publication Date: 2018-08-21
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Abstract
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Problems solved by technology

Hou Jingguo et al [Analytical Chemistry, 2006, 11(34), 1424-1528] separated a group of enantiomers of benalaxyl by high performance liquid chromatography using a chiral chromatographic column, but the synthesis of the chiral column is cumbersome and the separation time is cumbersome. Long, consumes a lot of organic solvent
Feng Shuoli et al [Zhejiang University of Technology, master's thesis] and others adopted a chromatographic column to separate a group of enantiomers of benalaxyl by supercritical fluid chromatography, but the separation time was long

Method used

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  • Method for splitting and measuring enantiomer of chiral pesticide benalaxyl through ultra-performance convergence chromatography-tandem mass-spectrometric technique

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example 1

[0031] 1. Instruments and reagents:

[0032] Tert-butyl methyl ether, methanol and isopropanol are chromatographic grade reagents, sodium citrate and sodium chloride are analytical reagents; distilled water meets the requirements of first-grade water in GB / T 6682.

[0033] Waters TQD quadrupole tandem mass spectrometer; water bath constant temperature oscillator; Swiss Mettler AE 163 electronic balance (sensitivity: 0.0001g).

[0034] 2. Sample handling:

[0035] Accurately weigh 2 g of the ground grain 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 2000 rpm for 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 supernatant into...

example 2

[0042] As described in Example 1, another tobacco sample was selected, and the contents of S-benalaxyl and R-benalaxyl in the sample were 0.85 and 0.74 mg / kg, respectively.

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Abstract

The invention belongs to the field of analytical chemistry and the technical field of determination of pesticide residues, particularly relates to a method for splitting and measuring enantiomer of achiral pesticide benalaxyl through the ultra-performance convergence chromatography-tandem mass-spectrometric technique, and relates to a method for splitting and quantifying raceme of the chiral pesticide. The method uses a QuEChERs method to extract benalaxyl in tobacco, cereals and dried fruits, and the enantiomer of the chiral pesticide benalaxyl is detected through the combination of convergence chromatographic chiral stationary phase and triple quadrupole tandem mass spectrum. The convergence chromatography is used for the first time to rapidly chirally separate the benalaxyl, and the sensitivity is high. The supercritical CO2 is taken as a mobile phase, a large number of organic solvents are saved in use, and the method is green and environmentally friendly.

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 the chiral pesticide benalaxyl by ultra-high-efficiency convergence chromatography-tandem mass spectrometry, and relates to the racemization of the chiral pesticide Body separation and quantification methods. Background technique [0002] The enantiomers of chiral pesticides often have significantly different digestion and fate in the environment. That is, the enantiomers of chiral pesticides may have huge differences in many aspects such as activity, toxicity, absorption, metabolism, and degradation in the natural environment and organisms. [0003] Chiral analysis is a powerful tool that can help people detect and deeply understand the biochemical impact process of chiral pesticides on the environment. A comprehensive and in-depth understanding of chiral...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 杨飞唐纲岭邓惠敏边照阳李中皓王颖范子彦刘珊珊
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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