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Column switching LC-MS/MS analysis method for detecting soporific and sedative drugs and metabolins thereof in urine

A technology of LC-MS and analysis method, applied in the direction of analyzing materials, measuring devices, material separation, etc., can solve the problems of heavy workload, time-consuming, etc., achieve high precision and reproducibility, improve analytical sensitivity, and simple pre-treatment Effect

Active Publication Date: 2011-02-02
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

[0003] Sample pretreatment is a very important step in the analysis method of biological samples, and it is also a relatively time-consuming and labor-intensive process.

Method used

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  • Column switching LC-MS/MS analysis method for detecting soporific and sedative drugs and metabolins thereof in urine
  • Column switching LC-MS/MS analysis method for detecting soporific and sedative drugs and metabolins thereof in urine
  • Column switching LC-MS/MS analysis method for detecting soporific and sedative drugs and metabolins thereof in urine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Equipped with double-pump infusion system and high-pressure flow path selection valve system

[0073] 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

[0075] Hypnotic and sedative drugs and their metabolites: 7-aminonitroazepam, prazosin, 7-aminoclonazepam, zolpitant, tetrahydropalmatine, clozapine, flurazepam, midazolam, diphenhydramine Doxepin, α-hydroxymidazolam, trihexyphenidyl, amitriptyline, chlorpromazine, α-hydroxytriazolam, α-hydroxyalprazolam, carbamazepine, estazolam , oxazepam, nitrazepam, alprazolam, lorazepam, triazolam, clonazepam, methaqualone, flunitrazepam, desazepam, oxyazepam, isoazepam, formazan Detection of diazepam, diazepam, and prazepam.

[0076] 1. Liquid chromatography conditions

[0077] a. Pretreatment column model: HLB 25μm 2.1×20mm (Waters Company)

[0078] Pretreatment column column temperature: room temperature

[0079] Pretreatment mobile phase: water

[0080] Flow rate: 1.0mL·min -1

[0081] Preprocessing time: 36s

[0082] Switching time: 36s-3.00min

[0083] b. Analytical column model: MS C18 3.5μm 2.1mm×150mm (Waters Company)

[0084] Analytical column column temperature: 35...

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Abstract

The invention discloses an column-switching LC-MS / MS analytical method for detecting soporific and sedative drugs and metabolins thereof in urine. The method comprises the following steps of: 1, configuring a double-pump infusion system and a high pressure flow channel selection valve system; 2, analyzing a sample according to a set LC-MS / MS condition; and 3, analyzing a result. The detection limit of soporific and sedative drugs or metabolins thereof in urine in the method is 0.01-10ng.Ml; the linear range is 2-3orders of magnitude, and related coefficients gamma are above 0.001, which showsa good linear relation. The urine sample to be tested in the method can be sampled after simple treatment, thereby simplifying experimental procedures, saving analysis time and reducing costs. The column switching LC-MS / MS analysis method of the invention is fast, sensitive and reliable, can be used for analyzing 32 kinds of common soporific and sedative drugs and metabolins thereof in urine, canbe widely used in analysis of actual cases.

Description

technical field [0001] The invention relates to a column switching LC-MS / MS analysis method for detecting hypnotic and sedative drugs and their metabolites in urine, in particular to a column switching LC-MS / MS method for detecting 32 kinds of hypnotic and sedative drugs and their metabolites in urine samples MS analysis method. Background technique [0002] Hypnotic and sedative drugs can inhibit the central nervous system, causing sedation, hypnosis and anticonvulsions. They are mainly used to treat anxiety, insomnia and convulsions. Since then, its usage has been increasing. However, hypnotic and sedative drugs can lead to dependence and abuse, which has become a global drug dependence problem. Due to the wide variety of hypnotic and sedative drugs, their easy availability and wide application, they are more harmful than opioids. At present, the common hypnotic and sedative drugs are taken orally in a safe range, and sharing them with alcoholic beverages can enhance th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08G01N30/20G01N30/02G01N30/72G01N30/28
Inventor 张玉荣梁晨汪蓉叶海英张润生丁敏菊
Owner 上海市公安局刑事侦查总队
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