液相色谱-串联质谱法测定人血浆中艾普拉唑的浓度  

LC-MS/MS determination of ilaprazole content in human plasma

作　　者：梁嘉碧[1] 冯文周[1] 边壮[1] 田琳[1] 郭惠学[1] 胡海棠 秦湘红 

机构地区：[1]中山大学附属第五医院,珠海519000 [2]丽珠医药集团股份有限公司,珠海519000

出　　处：《药物分析杂志》2013年第6期935-940,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：珠海市科技计划项目(珠科[2009]57号)

摘　　要：目的:建立LC-MS/MS法测定人血浆中艾普拉唑的浓度。方法:人血浆样本用乙酸乙酯提取后,选用Zorbax SB-C18色谱柱(150 mm×2.1 mm,5μm),以乙腈-10 mmol.L-1醋酸铵溶液(80∶20)为流动相,流速为0.20 mL.min-1;选用三重四极杆串联质谱仪的多重反应监测(MRM)扫描方式进行监测,电喷雾离子化源,正离子方式,选择监测离子反应分别为m/z367.5→m/z184.1(艾普拉唑)和m/z 383.2→m/z 266.8(内标氯雷他定)。结果:艾普拉唑和氯雷他定的保留时间分别为2.0 min和3.9 min;血浆中艾普拉唑的线性范围为5～1500 ng.mL-1(r>0.99),定量下限为5 ng.mL-1;日内、日间RSD均小于15%;低、中、高3个浓度下的提取回收率分别为(76.5±4.9)%、(78.8±6.3)%、(77.1±4.9)%。结论:该方法快速、灵敏、准确,专属性强,重复性好,适用于人血浆中艾普拉唑浓度的测定,可应用于艾普拉唑肠溶片的人体药代动力学及生物等效性研究。Objective： To develop an LC - MS/MS method for concentration determination of ilaprazole in human plasma. Methods： Human plasma samples were first extracted by ethyl acetate, and the analyte as then separated on a Zorbax SB -C18column （150 mm×2.1 mm,5μm）with the mobile phase of acetonitrile and 10 mL·mmol^-1 am-monium acetate （80： 20）at a flow rate of 0. 20 mL·min^-1. Detection was carried out by electrospray positive ioni-zation mass spectrometry in the multiple reaction monitoring （MRM） mode of the triple quadrupole rod tandem mass spectrometer. The MRM transitions of m/z 367.5→m/z 184. 1 and m/z 383.2→m/z 266. 8 were used to quantify ilaprazole and loratadine （the internal standard）, respectively. Results： Ilaprazole and the internal standard were e-luted at 2.0 min and 3.9 min, respectively. The calibration curve was linear over the concentration range of 5 - 1500 ng · mL^ -1 （ r 〉 0. 99 ）, with the lower limit of quantitation （LLOQ） of 5 mg · L^-1 . Intra - day and inter - day relative standard deviations were both below 15%. The （76.5 ±4. 9）% ,（78.8 ±6. 3）% ,and （77. 1 ±4. 9）% rapid, sensitive, accurate, specific and reliable, which can recoveries of low, middle and high concentrations were , respectively. Conclusion： The established method is be applied in pharmacokinetic and bioequivalent study.

关 键 词：液相色谱-串联质谱 艾普拉唑 血药浓度 药代动力学 生物利用度 

分 类 号：R917[医药卫生—药物分析学]