Centre Interfacultaire de Recherche du Médicament, ULg, Centre Hospitalier Universitaire Sart Tilman, Liege, Belgium.
J Anal Toxicol. 2010 Jun;34(5):280-6. doi: 10.1093/jat/34.5.280.
A selective and sensitive ultra-performance liquid chromatography (UPLC)-electrospray ionization-tandem mass spectrometry (MS) method for simultaneous determination of bupropion and its main metabolites, hydroxybupropion, erythrohydrobupropion, and threohydrobupropion, in human whole blood is presented. The sample preparation consists of cleanup protein precipitation with methanol combined with a solid-phase extraction on Oasis HLB cartridges. Analytes were separated on a Waters Acquity UPLC((R)) BEH phenyl column using a binary mobile phase consisting of ammonium formate buffer (2 mM, pH 4) and acetonitrile. Detection was performed on a Waters Acquity UPLC system coupled to a Quattro Premier triple-quadrupole MS in positive ion selected reaction monitoring. Internal standards were bupropion-d(9) and hydroxybupropion-d(6). Linearity was from 5 to 1000 ng/mL for bupropion and from 10 to 2000 ng/mL for metabolites. Accuracy profiles (80-120%), precision (< 15%), and limits of detection (1 ng/mL for bupropion and 2 ng/mL for metabolites) were also evaluated and responded to all criteria of validation. The aim of this study was to compare this presented method with a previously described method developed on a classic liquid chromatography-tandem MS system.
一种选择性和灵敏的超高效液相色谱（UPLC）-电喷雾串联质谱（MS）方法，用于同时测定人全血中的丁丙诺啡及其主要代谢物羟丁丙诺啡、赤型羟丁丙诺啡和苏型羟丁丙诺啡。样品制备包括使用甲醇进行蛋白质沉淀净化，然后用 Oasis HLB 固相萃取小柱进行固相萃取。分析物在 Waters Acquity UPLC((R)) BEH 苯基柱上用包含甲酸铵缓冲液（2 mM，pH 4）和乙腈的二元流动相分离。检测在 Waters Acquity UPLC 系统上进行，该系统与 Quattro Premier 三重四极杆 MS 联用，采用正离子选择反应监测。内标物为丁丙诺啡-d(9)和羟丁丙诺啡-d(6)。丁丙诺啡的线性范围为 5 至 1000 ng/mL，代谢物的线性范围为 10 至 2000 ng/mL。还评估了准确度（80-120%）、精密度（<15%）和检测限（丁丙诺啡为 1 ng/mL，代谢物为 2 ng/mL），并满足了所有验证标准。本研究的目的是将该方法与之前在经典液相色谱-串联 MS 系统上开发的方法进行比较。
