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Pyrethroid pesticide inspection method for treating biological detection material by using gel permeation chromatography

A technology of pyrethroids and gel permeation chromatography, which is applied in the field of criminal investigation, can solve the problems of lack of effective and feasible methods, no systematic inspection methods, etc., and achieve shortened pretreatment time, reduced analysis cost, high sensitivity and recovery rate Effect

Active Publication Date: 2015-07-01
INST OF FORENSIC SCI OF MIN OF PUBLIC SECURITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since it is difficult to remove macromolecular impurities such as proteins and oils contained in biological samples such as blood, urine, and liver tissue, there is no systematic test method for certain types of toxic substances in biological samples such as blood, urine, and liver tissue.
In the analysis and detection of toxicants in the domestic public security system, the application of gel permeation chromatography is still in its infancy, and there is still a lack of effective and feasible methods.

Method used

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  • Pyrethroid pesticide inspection method for treating biological detection material by using gel permeation chromatography
  • Pyrethroid pesticide inspection method for treating biological detection material by using gel permeation chromatography
  • Pyrethroid pesticide inspection method for treating biological detection material by using gel permeation chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Biological sample preparation

[0027] Blank blood and blank urine were collected from healthy volunteers who did not take any drugs within a week; blank liver tissues were collected from pigs that did not take any drugs within a week. Cypermethrin, deltamethrin, fenpropathrin, fenvalerate and lambda-cyhalothrin were all purchased from the National Standard Materials Research Center.

[0028] 2. Experimental conditions

[0029] 2.1 Preparation of standard solution

[0030] Preparation of standard stock solution: Weigh 10 mg each of cypermethrin, deltamethrin, fenpropathrin, fenvalerate and lambda-cyhalothrin, respectively, place them in 10 mL volumetric flasks, add a small amount of methanol to dissolve And dilute to the mark, and prepare 1 mg / mL standard stock solutions of cypermethrin, deltamethrin, fenpropathrin, esfenvalerate and lambda-cyhalothrin respectively, and store them in a refrigerator at 4°C for use.

[0031] Pipette a certain amount of single standa...

Embodiment 2

[0105] The difference between this embodiment and Example 1 is that the extraction solvent (i.e. organic solvent A) is a mixed solution of isoamyl ether and cyclohexanone, and the volume ratio of isoamyl ether and cyclohexanone in the mixed solution is 1:8; The rest of the experimental conditions are the same; using the mixed solution of isoamyl ether and cyclohexanone as the extraction solvent, the recovery and precision of the five pyrethroid pesticides are shown in Table 2-11~2-13.

[0106] Table 2-11 Addition recovery and precision of 5 pyrethroid pesticides in blood after GPC purification

[0107]

[0108]

[0109] Table 2-12 Addition recovery and precision of 5 pyrethroid pesticides in urine after GPC purification

[0110]

[0111] Table 2-13 Addition recovery and precision of five pyrethroid pesticides in liver after GPC purification

[0112]

[0113] It can be seen from Tables 2-11 to 2-13 that the recoveries of biological samples containing five pyrethroi...

Embodiment 3

[0115] The difference between this embodiment and Example 1 is that the extraction solvent (i.e. organic solvent A) is a mixed solution of cycloheptane and propyl butyrate, and the volume ratio of cycloheptane and propyl butyrate in the mixed solution is 1:3; The rest of the experimental conditions were the same; using the mixed solution of cycloheptane and propyl butyrate as the extraction solvent, the recovery and precision of the five pyrethroid pesticides were shown in Table 2-14~2-16.

[0116] Table 2-14 Addition recovery and precision of 5 pyrethroid pesticides in blood after GPC purification

[0117]

[0118] Table 2-15 Addition recovery and precision of 5 pyrethroid pesticides in urine after GPC purification

[0119]

[0120] Table 2-16 Addition recovery and precision of five pyrethroid pesticides in liver after GPC purification

[0121]

[0122] It can be seen from Tables 2-14 to 2-16 that the recoveries of biological samples containing 5 kinds of pyrethroid...

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Abstract

The present invention discloses a pyrethroid pesticide g inspection method for treating a biological detection material by using a gel permeation chromatography. The method comprises the following steps: (1) adding an organic solvent to a biological detection material, carrying out centrifugation, separating the organic phase, concentrating the obtained organic phase until drying, dissolving, and filtering with an organic microporous filtration membrane to obtain the extraction solution; (2) adding the extraction solution to a gel permeation chromatography purification column, carrying out elution, collecting the eluent, carrying out blowing drying through a concentrator, and dissolving to obtain a solution requiring detection; and (3) detecting the solution requiring detection by using a gas chromatography. According to the present invention, the gel permeation chromatography technology is applied in the field of toxicant analysis, the biological detection material pretreatment technology with characteristics of simpleness, rapidness, high sensitivity and high recovery rate is established based on the pyrethroid pesticide, advantages of pretreatment time shortening, analysis cost reduction and detection result reliability increase are provided, problems of various detection material types and complex components in the toxicant analysis are solved, and assurance is provided for improvement of efficiency of the toxicant analysis inspection work in the public security industry.

Description

technical field [0001] The invention relates to a method for detecting drugs and poisons in the field of criminal investigation, in particular to a method for detecting pyrethroid pesticides by using gel permeation chromatography to process biological inspection materials. Background technique [0002] With the advancement of technology, the requirements for drug and toxicant analysis and testing are getting higher and higher, including high reproducibility, high recovery rate, low detection limit and simple operation, etc., so it is urgent to establish a simple, fast and sensitive and a pretreatment method with a high recovery rate. At present, the existing pretreatment technologies mainly include liquid-liquid extraction, solid-phase extraction, and solid-phase microextraction. Check the situation. In the sample pretreatment technology, gel permeation chromatography technology, as a new type of analysis technology, has shown its potential application prospects due to its...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 栾玉静董颖王瑞花杜鸿雁张蕾萍常靖何毅王炯张云峰侯小平于忠山王芳琳崔冠峰
Owner INST OF FORENSIC SCI OF MIN OF PUBLIC SECURITY