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Method of splitting and determining metolachlor enantiomer as chiral pesticide with ultra performance bonded phase chromatography-tandem mass spectrometry technology

A metolachlor and ultra-high-efficiency fusion technology, applied in the field of analytical chemistry, can solve the problems of long separation time, no quantitative analysis method, etc.

Active Publication Date: 2018-08-17
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Abstract
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  • Application Information

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Problems solved by technology

[0005] At present, there are reports on the separation of metolachlor isomers using liquid chromatography chiral stationary phase [Analytical Chemistry Research Bulletin, 2004, 32(2), 191-194; Pesticides, 2008, 47(9), 655- 656], these are all separated by high performance liquid chromatography-chiral chromatographic column, the separation time is long, and there is no quantitative analysis method established for the implementation of product quality control

Method used

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  • Method of splitting and determining metolachlor enantiomer as chiral pesticide with ultra performance bonded phase chromatography-tandem mass spectrometry technology
  • Method of splitting and determining metolachlor enantiomer as chiral pesticide with ultra performance bonded phase chromatography-tandem mass spectrometry technology

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Effect test

example 1

[0026] 1. Instruments and reagents:

[0027] 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.

[0028] Waters TQD quadrupole tandem mass spectrometer; water bath constant temperature oscillator; Swiss Mettler AE 163 electronic balance (sensitivity: 0.0001g).

[0029] 2. Sample handling:

[0030] Accurately weigh 2 g of the ground grain 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 supernatant...

example 2

[0037] As described in Example 1, another dried tobacco sample after milling was selected, and metolachlor was not detected in the sample.

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Abstract

The invention belongs to the analytical chemistry field and the technical field of pesticide residue detection and particularly discloses a method of splitting and determining a metolachlor enantiomeras a chiral pesticide with an ultra performance bonded phase chromatography-tandem mass spectrometry technology. In the method, a QuEChERS method is adopted to extract metolachlor in tobaccos, grainsand dried fruits, an enantiomer of the metolachlor chiral pesticide is detected by combining bonded phase chromatography chiral stationary phase with triple stage quadrupole tandem mass spectrometry,and a method detected limit is 0.0012mg / kg. The method adopts bonded phase chromatography to rapidly perform chiral separation on the metolachlor for the first time; and by taking supercritical CO2 as a mobile phase, use of a great amount of an organic solvent is saved, and the method is green and environmentally friendly. The method uses bonded phase chromatography for rapid analysis, is beneficial to rapid separation and analysis speed of an isomer, consumes 4mins only and is high in sensitivity.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and the technical field of pesticide residue detection, and relates to a method for the resolution and quantification of enantiomers of chiral pesticides. Method for enantiomers of alachlor. Background technique [0002] 25% of the currently used pesticides are chiral, and there are enantiomeric differences in the biological activity of chiral pesticides, and their activity often only exists in one or a few enantiomers, while the enantiomeric 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] Metolachlor is an amide weed control agent, which can be widely used as a weed control agent in more than 70 crop fields because of its broad-spectrum, high efficiency, and strong selectivi...

Claims

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Application Information

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