LC-MS/MS法测定健康人血浆中的拉呋替丁  

Determination of Lafutidine in Human Plasma by LC-MS/MS

作　　者：邱聪[1] 李博[2] 陈沄[3] 

机构地区：[1]广州市第一人民医院药剂科,广州510180 [2]中国药科大学药学院食品质量与安全教研室,南京210009 [3]中国医学科学院皮肤病研究所,南京210042

出　　处：《药学与临床研究》2011年第5期417-420,共4页Pharmaceutical and Clinical Research

摘　　要：本文建立了一种快速测定人血浆中拉呋替丁血药浓度的LC-MS/MS法,采用CN柱(4.6 mm×150 mm,5μm),柱温30℃,流动相为甲醇-水(含20 mmol.L-1乙酸铵,0.2%甲酸)(97:3);流速1.0 mL.min-1;气动辅助电喷雾离子化(ESI),正离子检测,多反应离子检测(MRM)拉呋替丁和内标氯苯那敏分别为:m/z 432.20→351.15;m/z 275.10→230.05。拉呋替丁在1.98～396 ng.mL-1范围内线性关系良好(r=0.9991),定量限1.98 ng.mL-1。拉呋替丁低、中、高三个浓度批内及批间变异、准确度、绝对回收率均符合方法学要求,无显著基质效应。该方法专属性强,分析周期短,适合于临床上拉呋替丁血浆含量的测定。A rapid liquid chromatograph-electro-spray ionization（ESI） tandem mass spectrometric method was developed for the quantification of lafutidine in human plasma.Separation was performed using a Kromasil CN column（4.6 mm×150 mm,5 μm）maintained at 30℃ and the mobile phase consisting of a mixture of methyl alcohol and water（containing 20 mmol·L-1 ammonium acetate and 0.05% formic acid）（97∶3） was delivered at a flow rate of 1.0 mL·min-1;The analytes were analyzed by ESI in a multiple reaction monitoring（MRM） mode.The precursor to product ion transition of m/z 432.20→351.15 and m/z 275.10→230.05 were used to measure lafutidine and IS,respectively.The linearity ranged from 1.98 to 396 ng·mL-1（r=0.9991） and the limit of detection of lafutidine in human plasma was 1.98 ng·mL-1.The intra-and inter-assay precisions,accuracy and absolute recovery met the requirements of bioanalytical method,significant matrix effect was absent.The method is selective and suitable for the quantification of lafutidine in human plasma clinically.

关 键 词：血浆 拉呋替丁 LC-MS/MS 

分 类 号：R969.1[医药卫生—药理学]