Method for screening toxic substances in sample by using solid phase support liquid-liquid extraction-GC MS

A solid-phase supported, toxic substance technology, applied in the fields of analytical chemistry and material science, can solve the problem of inability to quickly screen toxic substances, and achieve the effect of eliminating adverse effects, rapid screening, and 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 solid-phase supported liquid-liquid extraction-chromatography-mass spectro

Method used

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  • Method for screening toxic substances in sample by using solid phase support liquid-liquid extraction-GC MS
  • Method for screening toxic substances in sample by using solid phase support liquid-liquid extraction-GC MS
  • Method for screening toxic substances in sample by using solid phase support liquid-liquid extraction-GC MS

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1. Prepare standard samples

[0036] Accurately weigh trichlorfon, parathion, diazinon, methamidophos, phorate, methyl parathion, monocrotophos, dimethoate, malathion, triazophos, Phosphate, isocarbophos, acephate, chlorpyrifos, monosultap, carbofuran, carbafur, methomyl, medicarb, aldicarb, isoprocarb, secbucarb, tetramethrin , cyfluthrin, lambda-cyhalothrin, bifenthrin, fenpropathrin, cypermethrin, fenvalerate, deltamethrin, endosulfan, triadimefon, butachlor, acetochlor, Isobacteria Urea, pentachloronitrobenzene, dicofol, fluroxypyr, fomesafen, tegrafyl, quizalofop, 4-chlorophenoxyacetic acid, hexythiazox, trichlorophenol, endosulfan, chlorothalon Each 25mg of clear, dichlorpyr, fenoxaprop-ethyl, atrazine, alachlor, and buprofezin standard substances was placed in a 10mL volumetric flask, and diluted with methanol to make a 2.5mg / mL standard stock solution .

[0037] Preparation of standard working solution: Accurately measure 100 μL and 50 μL of standard stock so...

Embodiment 2

[0051] Add the standard substances of various toxic substances in Table 1 to methanol respectively, wherein the added concentration of each standard substance is controlled to be 1 μg / mL, and then carry out gas chromatography-mass spectrometry analysis according to the analysis method of Example 1 to obtain the detection of each toxic substance Sensitivity, the results are shown in Table 1. The results in Table 1 show that the gas chromatography-mass spectrometry method of the present invention can simultaneously detect more than 130 toxic substances with different structures, and the detection sensitivity is 0.1-10 ng / μL.

[0052] Table 1 The detection sensitivity of each toxic substance in gas chromatography-mass spectrometry

[0053]

[0054]

[0055]

[0056]

[0057] Note: "-" means not detected.

Embodiment 3

[0059] Add the standard substances of various toxic substances in Table 3 to methanol respectively, and control the addition concentration of each standard substance to be 1 μg / mL, and then use liquid chromatography-mass spectrometry to perform liquid chromatography-mass spectrometry analysis. The analysis conditions are as follows:

[0060] Chromatographic conditions:

[0061] Chromatographic column: ACQUITYUPLC HSS C18 column, 2.1mm×150mm, 1.8μm;

[0062] Mobile phase: A: 0.1% formic acid acetonitrile, B: 5 mM ammonium formate (adjust pH to 3.5 with 0.1% formic acid)

[0063] Elution: Gradient elution, the conditions are shown in Table 2;

[0064] Column temperature: 35°C;

[0065] Flow rate: 0.4mL / min;

[0066] Table 2 Gradient elution conditions used in liquid chromatography-mass spectrometry analysis

[0067] time (min)

A(％)

B(％)

0

13

87

0.5

13

87

10

50

50

10.75

95

5

12.25

95

5...

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Abstract

The invention provides a method for screening toxic substances in a sample by using solid phase support liquid-liquid extraction-GC MC. The method comprises the following steps: extracting the sample by using a mixed solution containing a water-soluble organic solvent and deionized water, centrifuging an extracting solution after extraction, collecting a supernatant and removing the organic solvent in the supernatant, and preparing a sample liquid; adding the sample liquid into an activated solid phase support liquid-liquid extraction column, performing standing, performing eluting by using an eluate, and collecting the eluate; carrying out a chromatogram-mass spectrometry of the eluate. 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 150 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 solid-phase supported liquid-liquid extraction-chromatography-mass coupling method for screening toxic substances in samples. 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] Supported liquid-liquid extraction...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/34G01N30/02
Inventor 常靖王炯栾玉静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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