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HPLC-MS/MS determination method of fluridone residue

A technology for the determination of chlorpyrifos and its method, which is applied in the field of liquid mass spectrometry detection of herbicide chlorpyridone residues, can solve the problems of cumbersome operation and low sensitivity, achieve good repeatability, high sensitivity, and avoid matrix interference effect

Inactive Publication Date: 2018-12-07
SHANDONG ACADEMY OF PESTICIDE SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is cumbersome to operate and has low sensitivity

Method used

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  • HPLC-MS/MS determination method of fluridone residue
  • HPLC-MS/MS determination method of fluridone residue
  • HPLC-MS/MS determination method of fluridone residue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: Detection of chlorpyrazone residues in cottonseeds and cotton plants

[0040] (1) extraction

[0041] The cottonseed sample was crushed and sieved with a food conditioner to obtain a crushed sample with a particle size of about 100 μm. Accurately weighed 5 g of the crushed sample (accurate to 0.01 g) into a 50 mL plastic centrifuge tube with a stopper, and added 10 mL of acetonitrile and 5 mL to Ionized water, vortex for 10min; add 4g sodium chloride, vortex for 1min; centrifuge at 3800r / min for 5min, to be purified.

[0042] (2) purification

[0043]Take the supernatant directly into a 2mL centrifuge tube filled with 100mg C18 filler, vortex for 1min, and after standing still, pass the supernatant through a 0.22μm organic filter membrane to obtain a sample solution for HPLC-MS / MS determination.

[0044] (3) Make a standard curve

[0045] Preparation of standard working solution

[0046] Accurately weigh 50±0.1mg of chlorpyrifos standard product in a 50mL...

Embodiment 2

[0062] Example 2: Detection of chlorpyrazone residues in soil

[0063] (1) extraction

[0064] Weigh 10g of soil sample (accurate to 0.01g) into a 50mL stoppered plastic centrifuge tube, add 10mL of acetonitrile, vortex for 10min; add 2g of sodium chloride, vortex for 1min; centrifuge at 3800r / min for 5min to be purified.

[0065] (2) purification

[0066] Take about 1 mL of the supernatant, pass through a 0.22 μm organic filter membrane, and obtain a sample solution for detection.

[0067] (3) Make a standard curve

[0068] Preparation of standard working solution

[0069] 10, 5, 0.5, 0.1, 0.05 μg / mL standard solutions of chlorpyrazone with soil as the substrate were prepared according to step (3) of Example 1. Treat the soil blank sample without chlorpyrizone according to the above pretreatment steps (1) and (2) to obtain the soil blank sample solution, take 5 parts of 900 μL blank sample solution, and add Add 100 μL of the above-mentioned standard solutions of differen...

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Abstract

The invention discloses an HPLC-MS / MS determination method of fluridone residue, belonging to the technical field of determining pesticide residue. According to the specific scheme, the determinationmethod comprises the following steps: (1) extraction: grinding a sample, adding a solvent, performing vortex extraction, and centrifuging; (2) purification: purifying supernant, to obtain a sample liquor; (3) establishing a standard curve; and (4) determining and calculating fluridone residue in the sample. By utilizing the dispersive solid-phase extraction technology, a sample pretreatment methodwhich can simply and conveniently as well as quickly and effectively avoid matrix interface in the sample, by combining HPLC-MS / MS, the pretreatment method, is applied to qualitative confirmation andquantitative detection of fluridone in cotton seeds, cotton plants and soil, the average recovery rate is 74.0%-108.8%, the average relative standard deviation (RSD) is 0.9%-7.1%, the detection limitis 1.5mug / kg, and the determination method has the advantages of being simple and convenient, quick, accurate to operate, high in sensitivity, and good in repeatability.

Description

technical field [0001] The invention belongs to the technical field of determination of pesticide residues, and in particular relates to a liquid mass spectrometry detection method for the herbicide chlorpyrifos residues. Background technique [0002] Fluidone, a pyrrolidone herbicide, can be used to control most water or water surface weeds, and can also be used as a pre-emergence selective herbicide to control annual narrow-leaved and broad-leaved cotton weeds and Certain perennial weeds. The chemical name is: 1-methyl-3-phenyl-5-(3-trifluoromethylphenyl)-4-pyridone, the English chemical name is: l-methyl-3-phenyl-5-[3- (trifluoromethyl)-phenyl]-4pyridinone. The CAS registration number is 59756-60-4, the molecular weight is 329.3, the appearance is white to light yellow solid, the refractive index is 1.567, the flash point is 222.6°C, the melting point is 154-155°C, the density is 1.274g / cm3, and the boiling point is 444.4°C (760mmHg). for: [0003] [0004] Fluoxet...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/724G01N2030/027
Inventor 冯义志梁林张爱娟潘金菊齐晓雪任玉鹏金杰李文平马新刚韩济峰
Owner SHANDONG ACADEMY OF PESTICIDE SCI
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