高效液相色谱-质谱法测定人血浆中布洛芬浓度  

Determination of Ibuprofen in Human Plasma by HPLC-MS

作　　者：薛洪源[1] 刘军[1] 王宇奇[1] 贺文涛[1] 贾丽霞[1] 

机构地区：[1]解放军白求恩国际和平医院临床药理室,石家庄050082

出　　处：《华北国防医药》2007年第6期51-53,共3页Medical Journal of Beijing Military Region

摘　　要：目的：建立高效液相色谱．电喷雾质谱联用（HPLC-ESI-MS）法，测定人血浆中布洛芬的浓度。方法：将血浆经乙腈沉淀蛋白后，取上清液进样检测。液相分离采用Diamonsil C18分析柱，柱温30℃．以乙腈-2mmol／L乙酸铵缓冲液（80：20）为流动相，流速为0．5ml／min，进样量5μl；采用四极杆质谱检测器，电喷雾源（ESI）．雾化气（N2）压力为30psig．干燥气（N2）流速为13．0 L／min，干燥气（M）温度为350℃，毛细管电压3．5kV，碎片电压为75V，峰宽0．10，负离子方式检测．在选择离子监测（SIM）模式下检测质荷比（m／z）为205．2（布洛芬）和356．1（内标吲哚美辛）的准分子离子[M·H]。结果：血浆中无干扰测定的内源性物质，每个样品的分析时间小于5.0min；布洛芬在1．25—48μg／ml范围内呈良好的线性关系，回收率为98．5％-102．3％，日内精密度（RSD）〈3．9％．日间RSD〈8．1％。结论：本方法操作简便、选择性好、准确、灵敏，可用于布洛芬的药代动力学和生物利用度研究。Objective：To introduce the method for the determination of Ibuprofen in human plasma using HPLC-ESI-MS. Methods：The plas- ma was precipitated by the addition of acetonitrile. The supernatant was used for injection, then separated on a Diamonsil C18 analytical column. The mobile phase consisted of acetonitrile-2 mmol/l ammonium acetate solution（ 80： 20）, at a flow rate of O. 5 ml/min. A Agilent quadruple MSD equipped with an electrospray ionization（ ESI）source was used as detector and was operated in the negative ion mode. The nebulizer （ N2 ）pressure was at 30 psig. The drying gas（ N2 ） flow and its temperature were set at 13.0 L/min and 350℃. Capillary voltage and fragmentor voltage were set at 3.5 kV and 75 V, respectively. In selected ion monitoring（ SIM ） mode, the ion combinations of m/z 205.2 and 356. l was used to qualify Ibuprofen and internal standard （Indometacin）. Results： Chromatograms showed no endogenous interfering peaks with the respective blank human plasma samples. Each analysis was completed within 5.0 min. The linear range of Ibuprofen in plasma was 1. 25 -48 μg/ml. The method recoveries were 98.5% - 102.3%. The intra-day and inter-day RSDs were less than 3.9% and 8.1% . respectiyely. Conclusion：The method is supposed to be convenient, specific, accurate and sensitive enough to be applied to the pharmacokinetic and bioavailability studies of Ibuprofen in human plasma.

关 键 词：布洛芬 血药浓度 高效液相色谱-质谱法 

分 类 号：R969.1[医药卫生—药理学]