Column switching LC-MS/MS (Liquid Chromatography-Mass Spectrometry/Mass Spectrometry) analytical method for detecting morphine alkaloid in urine

A technology of LC-MS and analysis method, applied in the direction of analysis materials, measurement devices, material separation, etc., can solve the problems of cumbersome sample processing, heavy workload, low sensitivity, etc., and achieve improved analysis sensitivity, high precision and reproducibility Sexuality, simple effect of pre-processing

Active Publication Date: 2010-12-22
上海市公安局刑事侦查总队
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When cracking drug cases, anti-drug departments often use monoclonal antibody immunoassay kits in order to qualitatively detect drugs in the body fluids of drug suspects. However, monoclonal antibody immunoassay kits are prone to false positives due to the interference of certain drugs and cannot be used alone As a qualitative basis for drug abuse cases, it is particularly important to qualitatively test drugs in the body fluids of such people to determine whether they are taking heroin
After heroin enters the human body, it metabolizes very quickly in the body, and the original heroin is almost undetectable, and heroin is quickly metabolized into morphine and monoacetylmorphine in the human body, and morphine is a water-soluble drug with high polarity, which can be directly detected by gas chromatography. Difficult to analyze and low sensitivity
At present, there have been many reports on the analysis of morphine in urine by gas chromatography-mass spectrometry (GC-MS). Qualitative analysis, sample processing is cumbersome, and it is difficult to meet the needs of rapid inspection of actual cases
[0003] Sample pretreatment is a very important step in biological sample analysis methods, and it is also a time-consuming and labor-intensive process.

Method used

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  • Column switching LC-MS/MS (Liquid Chromatography-Mass Spectrometry/Mass Spectrometry) analytical method for detecting morphine alkaloid in urine
  • Column switching LC-MS/MS (Liquid Chromatography-Mass Spectrometry/Mass Spectrometry) analytical method for detecting morphine alkaloid in urine
  • Column switching LC-MS/MS (Liquid Chromatography-Mass Spectrometry/Mass Spectrometry) analytical method for detecting morphine alkaloid in urine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Equipped with double-pump infusion system and high-pressure flow path selection valve system

[0062] Connect the interface ⑤ of the ten-way switching valve 1 with the quaternary gradient pump 2 (Waters Alliance 2695); connect the interface ⑩ of the ten-way switching valve 1 with the high-pressure binary pump 3 (Waters 1525) through the sampler 4; Ports ④ and ⑨ of valve 1 are connected with pretreatment column 5 ( The two ends of HLB) are connected respectively, and the analytical column 6 ( One end of MS C18) is connected to port ⑧ of ten-way switching valve 1, and the other end is connected to detector 7 (Quattro Premier XE series quadrupole mass spectrometer).

Embodiment 2

[0064] Morphine, O 6 - Detection of monoacetylmorphine, codeine, acetylcodeine

[0065] 1. Liquid chromatography conditions

[0066] a. Pretreatment column model: HLB 25μm 2.1×20mm (Waters Company)

[0067] Pretreatment column column temperature: room temperature

[0068] Pretreatment mobile phase: water

[0069] Flow rate: 1.0mL·min -1

[0070] Preprocessing time: 36s

[0071] Switching time: 36s-3.00min

[0072] b. Analytical column model: MS C18 3.5μm 2.1mm×150mm (Waters Company)

[0073] Analytical column column temperature: 35°C

[0074] The analytical mobile phase includes A and B, wherein A is an aqueous solution of 2 mM ammonium formate and 0.05% (v / v) formic acid (0.126 g of ammonium formate and 500 μL formic acid, add water to 1000 mL), and B is 2 mM ammonium formate and 0.05% (v / v) v) Acetonitrile of formic acid (dissolve 0.126 g of ammonium formate and 500 μL of formic acid in 40 mL of water, add 960 mL of acetonitrile).

[0075] Flow rate: 0.2mL·min ...

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Abstract

The invention discloses a column switching LC-MS / MS (Liquid Chromatography-Mass Spectrometry / Mass Spectrometry) analytical method for detecting morphine alkaloid in urine, comprising the following steps of: (1) configuring a double-pump transfusion system and a high-pressure flow path selecting valve system; (2) analyzing a sample according to the set LC-MS / MS condition; and (3) analyzing a result. The limit of detection of the method for morphine, O6-monoacetylmorphine, codeine and acetylcodeine in the urine sample is 0.3-1ng.mL-1, the related coefficient gamma is above 0.9991, and the linear relation is favorable. Meanwhile, the urine sample can be directly injected and analyzed without pretreatment so that the experimental step is simplified, and the cost is saved. The method has the advantages of rapidity, sensitivity, simplicity and reliability and can be widely applied to actual case analysis.

Description

technical field [0001] The invention relates to a column switching LC-MS / MS analysis method for detecting morphine alkaloids in urine, in particular to a method for detecting morphine, O 6 - Column switching LC-MS / MS analysis method for monoacetylmorphine, codeine or acetylcodeine. Background technique [0002] In recent years, as the international drug epidemic continues to spread, the invasion of foreign drugs to our country has intensified, and more and more people are taking or injecting heroin. In order to crack down on drug criminals and maintain justice, the anti-drug department has increased its investigation of drug cases year by year. When cracking drug cases, anti-drug departments often use monoclonal antibody immunoassay kits for the qualitative detection of drugs in the body fluids of drug suspects. However, monoclonal antibody immunoassay kits are prone to false positives due to the interference of certain drugs and cannot be used alone As a qualitative basis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/72G01N30/60
Inventor 梁晨张玉荣叶海英汪蓉丁敏菊张润生
Owner 上海市公安局刑事侦查总队
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