Method for screening toxic substances in sample by using solid phase microextraction-GC-MS

A toxic substance and GC-MS technology, applied in the fields of analytical chemistry and material science, can solve the problems of inability to quickly screen toxic substances, achieve good practical application value, eliminate adverse effects, and achieve high detection efficiency

Inactive Publication Date: 2015-10-07
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

[0005] The invention provides a method for screening toxic substances in samples by using solid-phase microextraction-gas chromatography, which is used to solve technical defects such as the inability to quickly screen toxic substances of various structures in samples in prior art methods

Method used

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  • Method for screening toxic substances in sample by using solid phase microextraction-GC-MS
  • Method for screening toxic substances in sample by using solid phase microextraction-GC-MS
  • Method for screening toxic substances in sample by using solid phase microextraction-GC-MS

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Prepare samples

[0034] Take three identical blood samples of 100 mL each, and set the first blood sample as a blank sample.

[0035] Add isoprocarb, methomyl, secbucarb, phorate, carbofuran, pentachloronitrobenzene, diazinon, chlorothalonil, teclozole, and acetochlor to 100 mL of the second blood sample , propanil, alachlor, methyl parathion, carbaryl, malathion, chlorpyrifos, parathion, isocarbophos, dicofol, methapon, butachlor, endosulfan, buprofezin , triazophos, fluroxypyr, tetramethrin, bifenthrin, fenpropathrin, cyfluthrin, cypermethrin, quialofop, fenvalerate, tetramine and dichlorvos standard substances, The added concentration of each standard was controlled to be 100ng / mL, and then placed at room temperature for 3 weeks to make it highly corrupted, and sample 1-1 was obtained.

[0036] Add fenfluramine, barbiturate, ibuprofen, phenacetin, amobarbital, pentobarbital, pethalin, secobarbital, and dika to 100 mL of the third blood sample, respectively Ket...

Embodiment 2

[0052] Take six identical blood samples, and add various toxic substance standard substances in Table 1 to each blood sample, wherein the added concentration of each toxic substance standard substance in the first to sixth blood samples is controlled to be 500ng / mL, 200ng / mL, 100ng / mL, 50ng / mL, 5ng / mL, 1ng / mL, each sample was placed at room temperature for 3 weeks, after making it highly corrupt, the extraction of toxic substances according to Example 1 GC-MS analysis was carried out with the analytical method, and the detection limit and linear relationship of each toxic substance were obtained. The results are shown in Table 1.

[0053] Table 1 The detection limit and linear relationship of each toxic substance in blood samples

[0054]

[0055]

[0056]

[0057] It can be seen from Table 1 that:

[0058] The method of the present invention can simultaneously detect the above-mentioned more than 60 toxic substances with different structures in blood, and the detect...

Embodiment 3

[0060] Take three identical blood samples, and add the standard substances of various toxic substances in Table 2 to each blood sample, wherein the added concentrations of the standard substances of toxic substances in the first to third blood samples are controlled to be 200ng / mL, 100ng / mL, 50ng / mL, each sample is placed at room temperature for 3 weeks, after making it highly corrupt, carry out GC-MS analysis according to the extraction and analysis method of toxic substances in Example 1, and calculate each The recovery rate of toxic substances, the results are shown in Table 2.

[0061] Table 2 The recovery rate of each toxic substance in blood samples

[0062]

[0063]

[0064]

[0065] It can be seen from Table 2:

[0066] The method of the present invention can detect more than 60 kinds of toxic substances in the blood, and the recovery rate of the toxic substances in the blood is basically over 60%, especially the recovery rate of some toxic substances can rea...

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Abstract

The invention provides a method for screening toxic substances in a sample by using solid phase microextraction-GC-MS. The method comprises the following steps: extracting the sample by using a mixed solution containing a water-soluble organic solvent and deionized water, and producing an extract; centrifuging the extract, collecting a supernatant and removing organic solvents in the supernatant, performing centrifuging again, collecting a supernatant, and producing a sample liquid; inserting a PDMS extraction head into the sample liquid for carrying out solid phase microextraction, after extraction, fetching out the PDMS extraction head, inserting the extraction head into the GC-MS for desorption, and analyzing the desorbed sample which enters into a chromatographic column by using a GC-MS method. According to the invention, different toxic substances of a plurality of structures in a sample can be rapidly and effectively detected, especially screening of more than 60 kinds of toxic substances can be realized by single determination with high detection efficiency; the method provided by the invention is especially suitable for fields such as forensic science and has a good praticical value.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and material science, and in particular relates to a method for screening toxic substances in samples by using solid-phase microextraction-gas chromatography. Background technique [0002] In the field of forensic science, it is usually necessary to detect many toxic substances in various samples such as fresh organ tissues, blood, body fluids, carrion, and putrid mud. analgesics, narcotics, antibiotics, etc.), narcotics, food additives, Chinese herbal medicines, etc. However, the composition of these samples is relatively complex, especially the impurities contained in oils, pigments, proteins, enzymes, etc. are likely to interfere with the detection of toxic substances. Therefore, how to effectively remove impurities in samples and efficiently extract target poisons in samples has become a need for research one of the subjects. [0003] In addition, due to the complexity of the sample, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 常靖张云峰王瑞花郭震崔冠峰侯小平王芳琳于忠山何毅
Owner INST OF FORENSIC SCI OF MIN OF PUBLIC SECURITY
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