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Method for separating and measuring enantiomers of chiral pesticides metalaxyl and dimethomorph with UPCC-MS/MS (ultraperformance convergence chromatography-tandem mass spectrometry)

An ultra-efficient fusion and dimorpholine technology, applied in the field of analytical chemistry, can solve the problems of cumbersome chiral column synthesis and long separation time.

Active Publication Date: 2018-09-07
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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Problems solved by technology

Hou Jingguo et al [Analytical Chemistry, 2003, 31(3), 307-310] separated a group of enantiomers of metalaxyl 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

Method used

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  • Method for separating and measuring enantiomers of chiral pesticides metalaxyl and dimethomorph with UPCC-MS/MS (ultraperformance convergence chromatography-tandem mass spectrometry)
  • Method for separating and measuring enantiomers of chiral pesticides metalaxyl and dimethomorph with UPCC-MS/MS (ultraperformance convergence chromatography-tandem mass spectrometry)
  • Method for separating and measuring enantiomers of chiral pesticides metalaxyl and dimethomorph with UPCC-MS/MS (ultraperformance convergence chromatography-tandem mass spectrometry)

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0036] 1. Instruments and reagents:

[0037] Acetonitrile, methanol, and ethanol are all chromatographic grade reagents, and sodium citrate and sodium chloride are all 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 processing:

[0040] Accurately weigh 2 g of the ground grain sample into a 50 mL centrifuge tube with a lid, add 10 mL of water, add 10 mL of acetonitrile after soaking, and then place the centrifuge tube on a vortex mixer and shake at 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 place it on the vortex mixer and shake at 2000 rpm for 5 min, then centrifuge at 6000 rpm for 3 min; pipette 1.0 mL of the s...

example 2

[0047] As described in Example 1, another tobacco sample was selected, and the contents of S-metalaxyl and R-metalaxyl in the sample were 1.42 and 0.88 mg / kg, respectively.

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Abstract

The invention belongs to the field of analytical chemistry and the technical field of pesticide residue detection, particularly provides a method for separating and measuring enantiomers of chiral pesticides metalaxyl and dimethomorph with UPCC-MS / MS (ultraperformance convergence chromatography-tandem mass spectrometry) and relates to a separating and quantitating method for raceme of multiple chiral pesticides. According to the method, metalaxyl and dimethomorph in tobacco and dried fruits are extracted with a QuEChERS method, and the enantiomers of the two chiral pesticides metalaxyl and dimethomorph are synchronously detected through combination of chiral stationary phase of bonded phase chromatography and triple quadrupole MS. The convergence chromatography is adopted for the first time for rapid chiral separation of metalaxyl and dimethomorph, and sensitivity is high; supercritical CO2 is taken as a moving phase, so that a large quantity of organic solvents are saved, and the method is environmentally friendly.

Description

Technical field [0001] The invention belongs to the field of analytical chemistry and the technical field of pesticide residue detection, in particular to a method for separating and determining the enantiomers of chiral pesticides metalaxyl and dimethomorph by ultra-efficient convergence chromatography-tandem mass spectrometry technology, involving multiple Resolution and quantification methods of racemates of chiral pesticides. Background technique [0002] 25% of the pesticides currently in use are chiral. The biological activity of chiral pesticides is different in enantiomers, and its activity is usually only in one or a few enantiomers, while the enantiomers of chiral pesticides 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] Pesticide metalaxyl, chemical n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
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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