摘要
建立了快速、灵敏的液相色谱-串联质谱法测定人血浆中的二甲双胍和格列吡嗪.血浆样品经0.3%甲酸-乙腈（v/v）沉淀蛋白后,以乙腈-水-甲酸（70：30：0.3,v/v/v）为流动相,流速为0.50 mL·min^-1.Zorbax Extend C18柱分离,采用大气压化学电离源;以选择反应监测（SRM）方式进行正离子检测.用于定量分析的离子反应分别为m/z 130→m/z 60（二甲双胍）,m/z 446→m/321（格列吡嗪）和m/z 256→m/z 167（内标,苯海拉明）.测定血浆中二甲双胍的线性范围为2.00～2 000 ng·mL^-1,定量下限为2.00 ng·mL^-1;格列吡嗪的线性范围为1.00～1 000ng·mL^-1,定量下限为1.00 ng·mL^-1.该方法专属性好,灵敏度高,准确快捷,适用于二甲双胍和格列吡嗪的临床药代动力学研究.
To develop a sensitive and rapid liquid chromatographic-tandem mass spectrometric （LC-MS/MS） method for simultaneous quantitation of metformin and glipizide in human plasma, metformin, glipizide and internal standard diphenhydramine were separated from plasma by protein precipitation with acetonitrile （containing 0. 3% formic acid）, then chromatographed by using a Zorbax Extend C18 column. The mobile phase consisted of acetonitrile-water-formic acid （70： 30： 0.3, v/v/v） , at a flow rate of 0.50 mL . min^-1. A tandem mass spectrometer equipped with atmospheric pressure chemical ionization source was used as detector and operated in the positive ion mode. Selected reaction monitoring （SRM） using the precursor/production combinations of m/z 130→m/z 60, m/z 446→m/z 321 and m/z 256→m/z 167 were used to quantify metformin, glipizide and diphenhydramine, respectively. The linear concentration ranges of the calibration curves for metformin and glipizide were 2. 00 - 2 000 ng . mL^-1 and 1.00 - 1 000 ng . mL^-1, respectively. The lower limits of quantitation of metformin and glipizide were 2.00 ng . mL^- 1 and 1.00 ng . mL^-1, respectively. The method proved to be sensitive, simple and rapid, and suitable for clinical investigation of compound preparation containing metformin and glipizide.
出处
《药学学报》
CAS
CSCD
北大核心
2007年第10期1087-1091,共5页
Acta Pharmaceutica Sinica
