Method for detecting 43 types of medicines in blood by liquid chromatogram tandem mass spectrum

A technology of tandem mass spectrometry and liquid chromatography, which is applied in the field of detection of 43 kinds of drugs in blood by liquid chromatography tandem mass spectrometry, can solve the problems of long time consumption, difficulty in purchasing ether, and high toxicity of the test, so as to save processing time, improve sensitivity, meet The effect of timeliness requirements

Inactive Publication Date: 2019-12-03
成都民用航空医学中心
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Problems solved by technology

[0006] In 2016, the Judicial Authentication Technical Specification "Detection of 238 Toxins (Drugs) in Blood and Urine by Liquid Chromatography-Tandem Mass Spectrometry" (SF / Z JD0107005-2016) issued by the Judicial Authentication Administration of the Ministry of Justice of the People's Republic of China, It introduces a detection method for simultaneous detection of multiple toxic drugs such as opioids, amphetamines, antidepressants, and antiepileptics. The sample pretreatment is extracted with the precursor reagent ether, which is not easy to buy, and the test is more toxic. And a large blood volume (1ml) is required, and the types of drugs tested cannot meet the requirements of AP-67FS-003
[0007] The patent with the publication number CN 104133006 A discloses an ultra-high performance liquid chromatography-mass spectrometry method, which can simultaneously detect 11 kinds of hypoglycemic drugs, 19 kinds of blood pressure drugs and 1 kind of blood lipid-lowering drugs commonly used in clinical practice. Drugs do not involve psychotropic drugs and common drugs, nor can they fully meet the needs of civil aviation crews for safe drug use supervision
[0008] The patent with the publication number CN 107807178 A discloses a method for detecting drugs and antipsychotic drugs in blood by ultra-high performance liquid chromatography mass spectrometry. Although the method can detect 9 common drugs and 14 common psychotropic drugs Testing, but does not involve antihypertensive drugs and hypoglycemic drugs, which cannot fully meet the needs of civil aviation crew safety medication supervision
[0009] If the drugs specified in AP-67FS-003 are screened according to the patents with publication numbers CN 104133006 A and CN 107807178 A, the medical examiners need to complete 2 blood draws and 2 different experiments to complete all drug screening , requires a large amount of biological samples and takes a long time
[0010] At present, there is no accurate and effective method for simultaneous detection of hypoglycemic, hypotensive, psychotropic drugs and common drugs specified in AP-67FS-003, which needs to be developed urgently

Method used

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  • Method for detecting 43 types of medicines in blood by liquid chromatogram tandem mass spectrum
  • Method for detecting 43 types of medicines in blood by liquid chromatogram tandem mass spectrum
  • Method for detecting 43 types of medicines in blood by liquid chromatogram tandem mass spectrum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1 blood collection tube screening test

[0037] Under the same concentration and chromatographic conditions, two anticoagulant tubes of sodium fluoride and sodium heparin were used to collect blank blood respectively, and a comparative test was carried out by adding blank (100ng / ml). higher. Three kinds of narcotics, seven kinds of hypoglycemic drugs, and seven kinds of antihypertensive drugs in blood samples collected by sodium fluoride could not be effectively detected. The test results are shown in Table 1-4.

[0038] Table 1 Statistical table of blood collection tube screening comparison test results - drugs

[0039]

[0040]

[0041] Table 2 Statistical table of blood collection tube screening comparison test results - hypoglycemic drugs

[0042]

[0043]

[0044] Table 3 Statistical table of blood collection tube screening comparison test results - antihypertensive drugs

[0045]

[0046]

[0047] Table 4 Statistical table of blood...

Embodiment 2

[0051] Embodiment 2 pretreatment method screening test

[0052] Under the same chromatographic conditions and the same concentration, 2 times the volume of acetonitrile was used to precipitate protein and organic solvent to extract the sample, the method is as follows.

[0053] a: Take an appropriate amount of each substance, blow dry with nitrogen at 60°C, add 1ml of blank blood to the residue, add 3ml of ethyl acetate, vortex and mix for 1min, centrifuge at 5000r / min for 5min, take the supernatant and blow dry with nitrogen, add 50μl of reconstitution solvent to the residue Reconstitute, vortex for 1min, centrifuge at 13000r / min for 5min, inject sample for detection.

[0054] b: Take an appropriate amount of each substance, blow dry with nitrogen at 60°C, add 1ml of blank blood to the residue, add 3ml of acetonitrile, vortex and mix for 1min, centrifuge at 5000r / min for 5min, take the supernatant and blow dry with nitrogen, add 50μl of reconstitution solvent to the residue t...

Embodiment 3

[0069] Embodiment 3 mobile phase screening test

[0070] Carry out the following screening experiments to the detection conditions of liquid chromatography. The experimental example adopts 5mM ammonium formate aqueous solution-methanol (95:5) containing 0.1% formic acid as the mobile phase, and the comparative example adopts the following liquid phase conditions of A-F, with gradient elution 43 substances were detected.

[0071] Table 9 Experimental example Gradient elution ratio

[0072]

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Abstract

The invention belongs to the technical field of medicine detection, and particularly relates to a method for detecting 43 types of medicines in blood by liquid chromatogram tandem mass spectrum. Aiming at the problem of lack of a method capable of simultaneously detecting seven types of common poisons, eleven types of antihypertensive drugs, eleven types of hypoglycemic agents and fourteen types of psychiatric drugs in the prior art, the invention provides the method. The method comprises the following steps of (a) performing protein precipitation on a to-be-detected sample with acetonitrile;and (b) detecting a selected drug by a multi-reaction monitoring (MRM) mode of high performance liquid chromatography-tandem mass spectrometry, and mass spectrum screening analysis is performed in a segmented way according to compound retention time and by two or three pairs of parent ions/daughter ions. By the method, the screening analysis of 43 types of drugs such as common antihypertensive drugs, common hypoglycemic agents, psychiatric drugs and poisons can be rapidly and accurately completed within 25 minutes in one time, the detection efficiency is high, and the method is good in sensitivity and is suitable for promotion and application.

Description

technical field [0001] The invention belongs to the technical field of drug detection, and in particular relates to a method for detecting 43 kinds of drugs in blood by liquid chromatography tandem mass spectrometry. Background technique [0002] With the rapid development of the civil aviation industry, flight safety has always been the purpose of civil aviation services and the prerequisite for the development of civil aviation. As a special occupation group, pilots' physical and mental health directly affect flight safety. With the continuous increase of the number of aviation personnel, the aviation health security work has gradually entered a difficult situation. Aviation personnel self-seeking medical treatment and taking medicines occur from time to time. Many of these medicines have side effects that affect flight activities, greatly increasing the probability of flight accidents. According to the "Civil Aviation Crew, Air Traffic Controllers Drugs and Drugs Testing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/065
Inventor 席彰周亚兰
Owner 成都民用航空医学中心
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