HPLC-MS/MS测定人血浆中米格列奈钙的浓度  

HPLC-MS/MS determination of mitiglinide calcium in human plasma

作　　者：梁海霞[1,2] 郝光涛[1] 权苗苗[3] 杜娜娜[3] 卢兴红 刘泽源[1] 

机构地区：[1]军事医学科学院附属医院药理室,北京100071 [2]万全阳光医药科技有限公司药代中心,北京100097 [3]蚌埠医学院2005级药学系本科生,蚌埠233030

出　　处：《药物分析杂志》2010年第4期596-599,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立一种简便、灵敏的测定人血浆中米格列奈钙浓度的高效液相色谱-串联质谱(HPLC-MS/MS)方法。方法:以瑞格列奈为内标,样品处理采用乙腈直接沉淀的方法,用Agilent-C_(18)反相色谱柱(2.1 mm×150 mm,3.5μm)进行分离,以乙腈-甲醇-水(70:20:10)为流动相,柱温20℃,流速0.2 mL·min^(-1)。采用电喷雾负离子化,多反应监测(MRM)进行定量分析。结果:米格列奈钙在10～4000 ng·mL^(-1)浓度范围线性关系良好,相关系数为0.9994;最低检测浓度为2 ng·mL^(-1)(S/N≥3)。日内与日间RSD均小于10%(n=6),方法回收率在97.8%～104.9%之间。结论:本方法简便快速、灵敏准确,适用于米格列奈钙在人体内的药代动力学研究。Objective：To establish a simple,sensitive method of high performance liquid chromatography tandem mass spectrometry（HPLC - MS/MS） for determination of mitiglinide calcium in human plasma.Method：The internal standard is repaglinide,the plasma samples were deposited by acetonitrile directly,then the analytes were separated by using Agilent—C_（18）（2.1 mm×150 mm,3.5μm） column,the mobile phase consisted of acetonitrile-methanol -water（70：20：10）,the column temperature was 20℃,the flow rate was 0.2 mL·min^-1.Mitiglinide calcium was quantitated by multiple reaction monitoring（MRM） mode with negative electrospray ionization （ESI^-）.Results：The minimal detectable plasma drug concentration was 2 ng·mL^-1（S/N≥3）,the calibration curve was linear in the range of 10 -4000 ng·mL^-1,with coefficient of determination 0.9994.The average recovery was between 97.8%and 104.9%.Intra - day and inter - day RSDs were less than 10%（n = 6）.Conclusion： The method is simple,sensitive and accurate.It is suitable for the study of pharmacokinetics of mitiglinide calcium in human plasma.

关 键 词：高效液相色谱-串联质谱 米格列奈钙 

分 类 号：R917[医药卫生—药物分析学]