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Method for detecting content of oral anticoagulant drug in biological sample based on high performance liquid chromatography and triple quadrupole tandem mass spectrometry

A high-performance liquid chromatography, triple quadrupole technology, applied in the field of oral anticoagulant drug content, can solve the problems of difficulty and complicated interpretation of test results, and achieve the effects of easy automation, fast and stable detection, and convenient clinical promotion.

Pending Publication Date: 2021-07-09
FUWAI HOSPITAL CHINESE ACAD OF MEDICAL SCI & PEKING UNION MEDICAL COLLEGE +2
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Problems solved by technology

Not only is the interpretation of test results from the same laboratory very complex, but comparisons between different laboratories are also difficult

Method used

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  • Method for detecting content of oral anticoagulant drug in biological sample based on high performance liquid chromatography and triple quadrupole tandem mass spectrometry
  • Method for detecting content of oral anticoagulant drug in biological sample based on high performance liquid chromatography and triple quadrupole tandem mass spectrometry
  • Method for detecting content of oral anticoagulant drug in biological sample based on high performance liquid chromatography and triple quadrupole tandem mass spectrometry

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Embodiment

[0052] Dabigatran, rivaroxaban, apixaban and edoxaban standard products of the present invention and internal standards dabigatran-d3, rivaroxaban-d4, apixaban-d3 and apixaban Doshaban-d6 was purchased from TRC.

[0053] An analytical method for detecting dabigatran, rivaroxaban, apixaban and edoxaban in biological samples using high performance liquid chromatography triple quadrupole tandem mass spectrometer (LC-MS / MS), comprising the following steps :

[0054] 1. Preparation of standard stock solution and standard solution

[0055]Use an analytical balance to accurately weigh appropriate amounts of dabigatran, rivaroxaban, apixaban, and edoxaban standard substances, dissolve them in DMSO solution, and prepare standard stock solutions;

[0056] Use 50% methanol aqueous solution to dilute standard stock solution to prepare mixed standard working solution;

[0057] Use 50% aqueous methanol to dilute the mixed standard working solution, prepare the mixed standard working solu...

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Abstract

The invention provides a method for detecting the content of an oral anticoagulant drug in a biological sample based on high performance liquid chromatography and triple quadrupole tandem mass spectrometry, and relates to the technical field of clinical biological sample detection. The method comprises the following steps: (a) preparing a standard substance solution; (b) preparing an internal standard solution; (c) pretreating a biological sample; (d) respectively adding the biological sample, the standard substance solution and the quality control substance working solution into the mixed internal standard working solution, mixing, centrifuging, taking supernate, and carrying out high performance liquid chromatography triple quadrupole tandem mass spectrometry; wherein a used analysis chromatographic column is a C18 chromatographic column, and a mobile phase A and a mobile phase B are mixed for gradient elution; the mobile phase A is an aqueous solution containing 0.1-0.5% of formic acid; and the mobile phase B is 0-0.5% formic acid methanol solution. The method provided by the invention realizes one-time detection of the content of various oral anticoagulant drugs in the biological sample, and is simple and efficient.

Description

technical field [0001] The invention relates to the technical field of clinical biological sample detection, in particular to a method for detecting the content of oral anticoagulants in biological samples based on high-performance liquid chromatography triple quadrupole tandem mass spectrometry. Background technique [0002] Oral anticoagulant drugs (NOACs) such as dabigatran, rivaroxaban, apixaban, edoxaban, etc. are usually fixed doses, and there is no routine monitoring of coagulation function. Existing clinical studies have confirmed that the efficacy of NOACs is at least equivalent to that of vitamin K antagonists, but there are fewer serious bleeding events, especially significantly less intracranial hemorrhage. This simplifies anticoagulant therapy by eliminating the need for monitoring for bleeding events. This advantage of NOACs, together with their proven efficacy and safety, may explain why guidelines prefer NOACs over vitamin K antagonists in stroke prevention ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/04G01N30/06G01N30/14G01N30/34G01N30/86G01N30/88
CPCG01N30/02G01N30/72G01N30/04G01N30/06G01N30/14G01N30/34G01N30/8634G01N30/8679G01N30/88G01N2030/045G01N2030/884
Inventor 周洲王恺隽赵丽平肖滋兰栗琳丁亮何启鑫
Owner FUWAI HOSPITAL CHINESE ACAD OF MEDICAL SCI & PEKING UNION MEDICAL COLLEGE
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