Method for detecting diphenoxylate in biological sample by liquid chromatography-tandem mass spectrometry for criminal investigation

A technology of liquid chromatography and tandem mass spectrometry, which is applied in the field of detection of diphenoxylate in biological samples by liquid chromatography-tandem mass spectrometry, can solve the problems of complex operation, low detection sensitivity, and increased detection difficulty, and achieve simple operation and improved Effects of detection sensitivity and shortened detection time

Active Publication Date: 2013-10-09
INST OF FORENSIC SCI OF MIN OF PUBLIC SECURITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the detection of diphenoxylate in the prior art, the detection sensitivity is low and the operation is more complicated, which makes the detection more difficult; while in the criminal inve

Method used

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  • Method for detecting diphenoxylate in biological sample by liquid chromatography-tandem mass spectrometry for criminal investigation
  • Method for detecting diphenoxylate in biological sample by liquid chromatography-tandem mass spectrometry for criminal investigation
  • Method for detecting diphenoxylate in biological sample by liquid chromatography-tandem mass spectrometry for criminal investigation

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Experimental program
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Effect test

Embodiment 1 and Embodiment 2

[0026] In embodiment 1 and embodiment 2:

[0027] 1. Main instruments and equipment

[0028] UPLC-XevoTM TQ MS liquid chromatography-mass spectrometry instrument from Waters, USA, including Mass Lynx data processing system;

[0029] Gel permeation chromatography device: AccuPurep automatic gel chromatography system and Accu-Vap online concentration system, equipped with a 5.0mL quantitative loop and a 190-760nm variable wavelength ultraviolet detector and C0785 gel permeation chromatography purification column (gel column Filling phase is Bio-Beads SX-3) (U.S. J2-Scientific company);

[0030] EYELA CUTE MIXER CM100 oscillator (Jingdong, Japan);

[0031] Thermo Biofuge Primo R high-speed centrifuge (Thermo Electric);

[0032] BP210s electronic balance (Germany Sartorius company);

[0033] Millipore Simlicity Pure Water Purification System (France)

[0034] Scientific Industries Vortex Shaker (USA);

[0035] DSY-II automatic fast concentrator (Beijing Jingjingyuan Techno...

Embodiment 1

[0052] The method for using liquid chromatography-tandem mass spectrometry to detect diphenoxylate in biological samples for criminal investigation purposes in this embodiment includes the following steps:

[0053] (1) extract diphenoxylate from biological sample; Biological sample in the present embodiment is blood, urine and liver, and extracting diphenoxylate from blood, urine and liver comprises the following steps:

[0054] (1) Biological sample pretreatment: 1mL of blood, 1mL of urine or 1g of liver was cut into pieces, then added 600μl of acetonitrile, vortexed on a vortex for more than 5 minutes, then added 4mL of formic acid aqueous solution with a volume fraction of 2% formic acid, and vortexed Mix and rotate on the device for more than 5 minutes, centrifuge, and pass the supernatant through the column;

[0055] (2) Column activation: Take a mixed cation exchange extraction column, activate it with 2mL methanol and 2mL water in turn; (3) Pass through the column: pass...

Embodiment 2

[0086] The method for using liquid chromatography-tandem mass spectrometry to detect diphenoxylate in biological samples for criminal investigation purposes in this embodiment includes the following steps:

[0087] (1) extracting diphenoxylate from biological samples, the biological samples in the present embodiment are blood, urine and liver, extracting diphenoxylate from blood, urine and liver comprises the following steps: 1mL blood, 1mL urine or 1g After the liver is chopped, add 0.5mL acetonitrile, vortex on the vortex shaker, add 0.08mol / L potassium hydroxide solution to adjust the pH to 8, oscillate and mix, add 5mL dichloromethane to vortex, oscillate for 10min, and centrifuge at 8000rpm for 10min , after separating the organic phase, add 5 mL of dichloromethane for the second extraction, combine the two organic phases, purify by gel permeation chromatography, concentrate the leachate to dryness, dissolve the residue with 1 mL of acetonitrile, and use liquid chromatogra...

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Abstract

The invention relates to a method for detecting diphenoxylate in a biological sample by liquid chromatography-tandem mass spectrometry for criminal investigation. The method comprises the following steps: (I) extracting diphenoxylate from the biological sample; and (II) detecting diphenoxylate extracted in the step (I) by a liquid chromatography-tandem mass spectrometry instrument. The method provided by the invention improves the sensitivity of the detection of diphenoxylate in the biological sample to be detected, and reduces the degree of detection difficulty of diphenoxylate in the biological sample to be detected.

Description

technical field [0001] The invention belongs to the field of analysis and detection of chemical substances in criminal investigation, in particular to a method for detecting diphenoxylate in biological samples using liquid chromatography-tandem mass spectrometry for the purpose of criminal investigation. Background technique [0002] Diphenoxylate is a common antidiarrheal drug in clinical practice. In recent years, it is often poisoned due to improper use of drugs, especially among children under 10 years old. In addition, diphenoxylate is often used by drug addicts as a substitute for heroin, causing abuse and poisoning. Therefore, the detection of diphenoxylate is very necessary. In the detection of diphenoxylate in the prior art, the detection sensitivity is low and the operation is more complicated, which makes the detection more difficult; while in the criminal investigation for the detection of urine samples or blood samples of drug suspects, high detection sensitivit...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 栾玉静董颖杜鸿雁王瑞花张蕾萍常靖王炯张云峰于忠山何毅王芳琳侯小平崔冠峰
Owner INST OF FORENSIC SCI OF MIN OF PUBLIC SECURITY
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