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Method for enriching and detecting cocaine and metabolin thereof in urine through magnetic dispersed extraction materials

A solid-phase extraction material, cocaine technology, applied in the field of magnetic dispersion extraction material enrichment detection of cocaine and its metabolites in urine, can solve the problems of shortened column life, great influence on operators, cumbersome and time-consuming steps, etc., to achieve Efficient extraction and enrichment, improve efficiency, and avoid low-reproducibility effects

Active Publication Date: 2017-05-24
SHANGHAI CRIMINAL SCI TECH RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the disadvantages of cumbersome and time-consuming steps in the existing cocaine pretreatment method, large consumption of reagents, great influence by operators, or poor reliability, and if the pretreatment is improper, the recovery rate of the whole process will be reduced, There will be problems such as qualitative and quantitative errors and shortened chromatographic column life. A method for the enrichment and detection of cocaine and its metabolites in urine with magnetic dispersion extraction materials is proposed, which can quickly separate and enrich cocaine. Using functionalized magnetic particles and cocaine Combined use of magnetic enrichment and separation, since the pretreated sample is non-damaging, non-polluting, and high in concentration, it can significantly improve the efficiency of pretreatment, reduce the influence of human factors, and greatly improve the accuracy of detection. The accurate inspection provides a more reliable guarantee

Method used

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  • Method for enriching and detecting cocaine and metabolin thereof in urine through magnetic dispersed extraction materials
  • Method for enriching and detecting cocaine and metabolin thereof in urine through magnetic dispersed extraction materials
  • Method for enriching and detecting cocaine and metabolin thereof in urine through magnetic dispersed extraction materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Synthesis of polyvinylpyrrolidone-modified magnetic particles:

[0033] 1) Disperse 1 g of PSA magnetic beads with an average particle size of 500 nm in 500 mL of dimethyl sulfoxide, sonicate at 35 Hz for 10 min, add 0.5 mL of triethylamine solution, stir mechanically at 250 rpm for 10 min, and add 8.2 mL of methacrylic acid glycidyl esters,

[0034] React at 40°C for 16 hours.

[0035] 2) The nanoparticles obtained by magnetic separation were washed with dimethyl sulfoxide and methanol for 3 times, and then dried in vacuum at 60° C. overnight to obtain double bond-modified magnetic nanoparticles;

[0036] 3) Add 0.4 g of double bond-modified magnetic nanoparticles to 180 mL of isopropanol solution, ultrasonicate at 35 Hz for 12 min,

[0037] Add 0.1 g of azobisisobutyronitrile and 0.55 g of vinylpyrrolidone, stir mechanically at 250 rpm, protect with nitrogen, and react at 75 degrees for 12 hours to obtain polyvinylpyrrolidone-modified magnetic particles.

Embodiment 2

[0039] Take 8 normal people's urine samples and divide them into 1mL each. Urine sample 1 is not processed in any way, and it is directly analyzed and tested according to the following method:

[0040] 1) Add a certain amount of cocaine and its metabolites to urine samples 2-8, add 0.004g of PSA magnetic beads and

[0041]0.005 g of the mixture of polyvinylpyrrolidone-modified magnetic particles prepared in Example 1 above was uniformly mixed for 20 minutes, magnetically separated, and urine was removed, and treated in a vacuum drying oven at 60° C. for 2 hours.

[0042] 2) Add 400 μL of elution solution, the elution solvent is acetonitrile:methanol (v / v)=1:4, mix uniformly for 5 minutes, magnetically separate, collect the eluent, and complete the elution of cocaine and its metabolites, The eluate is detected by LC-MS to obtain the analysis result.

[0043] Table 2 is the detection experiment of urine sample and cocaine spiked urine sample

[0044]

[0045]

[0046] Fr...

Embodiment 3

[0055] This embodiment includes the following steps:

[0056] 1) Take 1mL of urine sample (marked as sample A) in a 2mL centrifuge tube, add 0.005g of PSA magnetic beads or 0.002g of polyvinylpyrrolidone modified magnetic particles to mix, mix evenly for 30min, magnetically separate, remove Urine was treated in a vacuum oven at 60°C for 2 hours.

[0057] 2) Add 400 μL of elution solution, the elution solvent is methanol: water (v / v) = 4:1, mix evenly for 5 minutes, magnetically separate, collect the eluate, and complete the elution of cocaine and its metabolites. The eluate was detected by LC-MS, and the analysis showed that cocaine: 0 ng / mL, benzoylecgonine: 0 ng / mL, and methylecgonine: 0 ng / mL were detected in sample A.

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Abstract

The invention discloses a method for enriching and detecting cocaine and metabolin thereof in urine through magnetic dispersed extraction materials. The method comprises the following steps: mixing polyvinylpyrrolidone modified magnetic-particles with PSA magnetic beads, then enriching cocaine and metabolin thereof in urine through the mixture, and detecting and analyzing the contents of the cocaine and the metabolin thereof through an LS-MS method after elution. The method can rapidly separate and enrich cocaine, can effectively combine with, magnetically enrich and separate from cocaine through functional magnetic-particles, can obviously improve the pretreatment efficiency because pretreated samples are not damaged and polluted and high in concentrations, reduces the influence of human factors, improves the detection accuracy to a great extent, and provides a more reliable guarantee for the accurate inspection of micro cocaine.

Description

technical field [0001] The invention relates to a technique in the field of drug detection, in particular to a method for enriching and detecting cocaine and its metabolites in urine with magnetically dispersed extraction materials. Background technique [0002] Cocaine (cocaine, cocaine) is a class of psychotropic drugs strictly controlled by the state (China Food and Drug Administration, State Food and Drug Administration [2005] No. 481 document). Cocaine is a very common drug in our country, and people who use cocaine respond with excitement, self-confidence, increased energy, rapid heartbeat, dilated pupils, fever, shaking and sweating. Continuous smoking of cocaine will form mental and physical dependence, seriously endanger human health and affect social stability. Therefore, the establishment of a rapid and accurate detection method for cocaine-like drugs can provide scientific and accurate criminal evidence. Because cocaine can be ingested through smoking, intraven...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N30/14
CPCG01N30/02G01N30/06G01N30/08G01N30/14G01N2030/027G01N2030/062G01N2030/065
Inventor 杨飞宇倪春芳汪蓉叶海英梁晨张玉荣刘文斌邹芸袁晓亮曹芳琪马克
Owner SHANGHAI CRIMINAL SCI TECH RES INST
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