人血浆中格列美脲的LC-MSMS测定.pdfVIP

• 292 • 中闺眩药工业杂志 Chinese JoumaJ of Phannaceuticals 2009 ,40(4) 人血浆中格列美服的 LC-MS/MS 测定 任进民l ，李杏;fJ2 ，赵曦3 ，都立志1 ，刘剑l (1.闸北医科大学第二版院，问北布家庄 050000; 2. 北京出版社教材中心，北京 100088; 3. 中奇制药技术有限公司，河北石家庄 050051) 色谱柱，以格列齐特为内标，流动相为 摘要t 建立了LC-MS/MS措测定人血浆中格列荣服的浓度。采用C 2 mmollL乙 18 酸锻浴液(含0.5% 甲酸)-甲醇(27 : 73) ，电喷雾离子化源，选探性正离子多反耐脱测，检恻离子分别为mlz 491.2叶m/z 352.0(格列类服)和mlz 324.1→m々 127.2(格列齐特)。结果将列英踩在1400 nglml浓度范围内战性关系良好，相对回收 率大于99.1 %，提取回收率大于95.7% ，日内和日问RSD均小子10.1%. 关键诩z 格列荧腺:液相色谱唰串联质谱:测定 中团分§挂号: R969 )c献标志码:A 文意编号: 1ω1-8255 (2009) 04-0292-03 Detennination of Glimepiride in Human Plasma by LC嗣MSIMS 1 3 1 1 REN Jin-min , LI Xing-le , ZHAO Xi , GUO Li-zhi ,L肌J Jían (1.1加SecondHospital ofHebeí Medícal Univers;秒:， Sh扩iazhuang 050000; 2. Dept. ofTe.r:劝ook， Beijing Publishing House. Beijing 100088; 3. Zhol啊iPhamωceutical Technology Co.. Ltd , Shijiazhuang 050051) ABSTRACT: A LC幽MS/MS method wωestablished for the detennination of glím叩iride in human plasma. A CI8 column was used with gliclazide as the intemal standa时， using 2 mmollL ammoniUID acetate (con切ining 0.5 % formic acid) -methanol (27 : 73) 幽 the mobíle phase. ESI w;部 applied and operated ín positive iron multiple-reaction moni嗣 toring mode. 丁he detected ions were m々 491.2叫m1z 352.0 (glim叩iride) and m々 324.1→m1z 127.2 (glíclazide).ηm calibratíon curve was linear in the concentratíon range of 1 - 400 ngiml.The relative recove叩 was over 99.1 % and the average extraction recovery was above 95.7 %. The RSDs of inter- and intra-day were les