Callejas S L, Biddlecombe R A, Jones A E, Joyce K B, Pereira A I, Pleasance S
Department of International Bioanalysis, GlaxoWellcome Research and Development, Ware, Herts, UK.
J Chromatogr B Biomed Sci Appl. 1998 Nov 6;718(2):243-50. doi: 10.1016/s0378-4347(98)00374-0.
A sensitive, robust and high throughput mass spectrometry based method is described for the determination of the glucocorticoid fluticasone propionate in plasma. The method employs solid-phase extraction in 96 well microtitre plate format which has been automated by means of a custom built Zymark robotic system. The extracts are analysed by liquid chromatography-tandem mass spectrometry using thermally and pneumatically assisted electrospray ionisation and selected reaction monitoring. The method is both accurate and precise with both intra- and inter-assay precision (C.V.) of less than <6%. The method provides a lower limit of quantification of 20 pg/ml from 0.5 ml of human plasma, sufficient to monitor systemic concentrations of inhaled fluticasone propionate at therapeutic doses.
描述了一种灵敏、稳健且高通量的基于质谱法的血浆中丙酸氟替卡松糖皮质激素测定方法。该方法采用96孔微量滴定板形式的固相萃取,并通过定制的Zymark机器人系统实现了自动化。提取物通过液相色谱-串联质谱法进行分析,采用热辅助和气动辅助电喷雾电离以及选择反应监测。该方法准确且精密,批内和批间精密度(变异系数)均小于6%。该方法从0.5 ml人血浆中提供了20 pg/ml的定量下限,足以监测治疗剂量下吸入丙酸氟替卡松的全身浓度。