Method for extracting pyrethroid pesticide residue in liquid sample

A technology for pyrethroids and pyrethroids, which is applied in the field of pesticide residue detection, can solve the problems that extraction and purification of pyrethroid pesticides is not a simple or effective method, consumes a lot of organic solvents, and has limited application scope, and reduces detection steps. and manpower, high recovery rate, and the effect of improving detection efficiency

Inactive Publication Date: 2017-06-20
HAINAN MEDICAL COLLEGE
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Problems solved by technology

These pretreatment methods have disadvantages such as high consumption of organic solvents, small sample throughput, limited application range, c...

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  • Method for extracting pyrethroid pesticide residue in liquid sample
  • Method for extracting pyrethroid pesticide residue in liquid sample
  • Method for extracting pyrethroid pesticide residue in liquid sample

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specific Embodiment approach

[0025] DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be further described below in combination with examples.

[0026] The instruments, reagents, materials, etc. involved in the following examples, unless otherwise specified, are conventional instruments, reagents, materials, etc. in the prior art, and can be obtained through formal commercial channels. The experimental methods, detection methods, etc. involved in the following examples, unless otherwise specified, are conventional experimental methods, detection methods, etc. in the prior art.

[0027] Experimental Screening of Optimal Extraction Conditions

[0028] The extraction method is as follows: take 2mL samples (4 kinds of pyrethroid pesticide mixed standard solutions), place them in a 10mL glass centrifuge tube, adjust the pH value to the design value (use 5% phosphoric acid solution or 0.5mol / L sodium hydroxide solution to adjust ; see Table 1), add 2mL of acetonitrile, and mix to o...

Embodiment 1

[0034] Example 1: Extraction and detection of pyrethroid pesticide residues in urine, wastewater and seawater samples

[0035] 1. Extraction and detection method

[0036]The extraction method steps are as follows: each get 2mL urine sample, waste water and seawater sample, place respectively in 10mL glass centrifuge tube, adjust pH value to 3 (adjust with 5% phosphoric acid solution or 0.5mol / L sodium hydroxide solution), each Add 2mL of acetonitrile and mix well to obtain a homogeneous solution. Add 4 mL of salting-out solution (pH=4) to the homogeneous solution, and the solution is divided into two layers, the upper layer is an acetonitrile phase, and the lower layer is an aqueous phase. Get the upper acetonitrile phase, carry out gas chromatography-mass spectrometry detection after filtering through 0.45 μm microporous membrane (flow process is as follows: figure 1 shown).

[0037] The salting-out solution is prepared by the following method: prepare 100mmol / L phosph...

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Abstract

The invention discloses a method for extracting pyrethroid pesticide residue in a liquid sample. The method comprises the following steps: (1) taking the liquid sample to be detected, adjusting the pH value of the liquid sample to be 3, adding acetonitrile, and evenly mixing to obtain a uniform solution; (2) adding salting-out liquid into the uniform solution, and standing until layering; (3) after layering, taking the acetonitrile phase at the upper layer, filtering the acetonitrile phase by using a microporous filter membrane with the thickness of 0.45mu m, and then directly carrying out gas chromatography-mass spectrometry determination, wherein the liquid sample is preferably a high-salt or/and high-protein sample. The method for extracting the pyrethroid pesticide residue can be used for extracting and purifying pyrethroid pesticides such as bifenthrin, permethrin, beta-cyfluthrin and fenvalerate, thus reducing the consumption of organic reagents; furthermore, a centrifuge device, an ultrasonic device, a shaking device and the like do not need to be used in the method, so that the method is simple, rapid and high in recovery rate, and can be predicted; the method has good application prospect in the technical field of pesticide residue determination.

Description

technical field [0001] The invention relates to an extraction method for pyrethroid pesticide residues in liquid samples, in particular to an extraction method for pyrethroid pesticide residues in high-salt or / and high-protein samples, and belongs to the technical field of pesticide residue detection. Background technique [0002] Pyrethroid pesticides are broad-spectrum insecticides that have good control effects on various pests in agriculture, forestry, horticulture, warehouses, animal husbandry, and sanitation. Due to the advantages of low price, high efficacy and low toxicity, pyrethroid pesticides are widely used in the growth process of fruits and vegetables, and are used in indoor and outdoor insect removal processes. Pyrethroid pesticides are easily spread by surface water infiltration and soil erosion. However, such pesticides are neurotoxic, can produce neurotoxic effects on insects and mammals, and they are fat-soluble compounds that are not sensitive to light a...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/02
Inventor 温莹莹牛宗亮于春伟张军文少白季玉祥李娜蹇丽
Owner HAINAN MEDICAL COLLEGE
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