LC／MS法测定人血浆中的卡维地洛浓度

目的：建立测定人血浆中卡维地洛浓度的LC／MS方法。方法：以盐酸氨溴索为内标，待测血浆样品经乙腈沉淀，高速离心后取上清液进样，色谱柱为SHIMADZU VP-ODS柱（250mm×2．0mm，5μm），甲醇-0．1％甲酸水溶液：64：36（含10mmol·L^-1乙酸铵）为流动相。ESI离子源；CDL Tempe 250℃，Heat Block Tempe 200℃，Detector Voltage 1．7Kv；正离子方式检测，扫描方式为选择离子扫描（SIM），用于定量的离子分别为卡维地洛m／z：407；内标（氨溴索）m／z：379；扫描时间：0．2s。结果：内源性物质不干扰卡维地洛的检测，每个样品分析时间约4．4min，卡维地洛的线性范围为0．3—120ng·ml^-1，批内、批间RSD均小于10％，低、中、高浓度的（0．6，5，60ng·ml^-1）平均提取回收率分别为92．43％、85．08％、88．32％。结论：该法操作快速、简单、准确，介质用量少，可用于，临床药物动力学研究中大批量血样的处理。

Determination of Carvedilol in Human Serum by LC/MS

Objective： To develop a rapid, simple and specific high performance liquid chromatography-mass spectrography （HPLC- MS） method for determination of carvedilol in human serum. Method： The ambroxol hydrochloride was used as the internal standard, SHIMADZU VP-ODS column（250mm x 2.0mm,51xm） was used, mobile phase was consisted of methanol/0.1% formic acid （64：36 v/v, containing 10 mmol·L^-1 ammonium acetate） flow rate was 0.2 ml· min^-1. Result： Each analysis was completed within 4.4 minute. The assay was linear over the concentration range 0.3 - 120 ng·ml^-1 excluded from endogenous substance effect. The intra- and inter-day precision over the entire concentration range were less than 10%. The mean extraction recoveries of carvedilol were 92.43, 85.08 and 88.32% at concentrations of 0.6,5 and 60 ng· ml^-1, respectively. Conclusion： A simple, rapid and specific HPLC-MS method for clinical pharmacokinetics was developed to determine carvedilol in human serum.