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用液相色谱-热喷雾质谱法测定人血浆中血小板活化因子拮抗剂6-(2-氯苯基)-9-[(4-甲氧基苯基)硫代氨基甲酰基]-1-甲基-7,8,9,10-四氢-4H-吡啶并[4',3'-4,5]-噻吩并[3,2-f][1,2,4]三唑并[4,3-a][1,4]二氮杂卓

Determination of the platelet activating factor antagonist 6-(2- chlorophenyl)-9-[(4-methoxyphenyl)thiocarbamoyl]-1-methyl-7,8,9,10- tetrahydro-4H-pyrido[4',3'-4,5]-thieno[3,2-f][1,2,4]triazolo[4, 3-a][1,4] diazepine in human plasma by liquid chromatography-thermospray mass spectrometry.

作者信息

Celma C

机构信息

Mass Spectrometry Department, S.A. LASA Laboratorios, Sant Feliu de Llobregat, Barcelona, Spain.

出版信息

J Chromatogr B Biomed Appl. 1994 Jul 1;657(1):214-8. doi: 10.1016/0378-4347(94)80090-1.

DOI:10.1016/0378-4347(94)80090-1
PMID:7952071
Abstract

A sensitive and specific method for the determination of the platelet activating factor (PAF) antagonist 6-(2-chlorophenyl)-9-[(4-methoxyphenyl)-thiocarbamoyl]-1-methyl-7,8,9,10- tetrahydro-4H-pyrido[4',3'-4,5]thieno-[3,2-f][1, 2, 4]triazolo [4, 3-a][1, 4] diazepine (I) in human plasma is described. The target molecule was analyzed by high-performance liquid chromatography (HPLC) coupled to mass spectrometry (MS) after extraction by ion-exchange chromatography. HPLC was carried out using a C18 column and the coupling to the MS was done by a thermospray (TSP) interface working in the direct ion-evaporation ionization mode in presence of 0.1 M ammonium acetate. Selected-ion monitoring (SIM) was carried out for the ion m/z 370 and its [M + 2]+ isotopic peak. Evaluation of the intensity matching of such ions has been used in the validation results. The method gives good accuracy and precision over the concentration range 1-200 ng/ml in human plasma.

摘要

描述了一种测定人血浆中血小板活化因子(PAF)拮抗剂6-(2-氯苯基)-9-[(4-甲氧基苯基)-硫代氨基甲酰基]-1-甲基-7,8,9,10-四氢-4H-吡啶并[4',3'-4,5]噻吩并[3,2-f][1,2,4]三唑并[4,3-a][1,4]二氮杂卓(I)的灵敏且特异的方法。通过离子交换色谱萃取后,采用高效液相色谱(HPLC)与质谱(MS)联用对目标分子进行分析。HPLC使用C18柱进行,与MS的联用通过在0.1M乙酸铵存在下以直接离子蒸发电离模式工作的热喷雾(TSP)接口完成。对离子m/z 370及其[M + 2]+同位素峰进行选择离子监测(SIM)。在验证结果中使用了对此类离子强度匹配的评估。该方法在人血浆1 - 200 ng/ml的浓度范围内具有良好的准确度和精密度。

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