Zhao Xiao-hua, Song Bo, Zhong Da-fang, Zhang Shu-qiu, Chen Xiao-yan
Shanxi Medical University, Taiyuan 030001, China.
Yao Xue Xue Bao. 2007 Oct;42(10):1087-91.
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 x 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 - 2000 ng x mL(-1) and 1.00 - 1000 ng x mL(-1), respectively. The lower limits of quantitation of metformin and glipizide were 2.00 ng x mL(-1) and 1.00 ng x mL(-1), respectively. The method proved to be sensitive, simple and rapid, and suitable for clinical investigation of compound preparation containing metformin and glipizide.
建立一种灵敏、快速的液相色谱 - 串联质谱（LC-MS/MS）法，用于同时定量测定人血浆中的二甲双胍和格列吡嗪。采用含0.3%甲酸的乙腈进行蛋白沉淀，从血浆中分离出二甲双胍、格列吡嗪和内标苯海拉明，然后使用Zorbax Extend C18柱进行色谱分析。流动相由乙腈 - 水 - 甲酸（70:30:0.3，v/v/v）组成，流速为0.50 mL·min⁻¹。配备大气压化学电离源的串联质谱仪用作检测器，以正离子模式运行。分别使用m/z 130→m/z 60、m/z 446→m/z 321和m/z 256→m/z 167的前体/产物组合进行选择反应监测（SRM），以定量二甲双胍、格列吡嗪和苯海拉明。二甲双胍和格列吡嗪校准曲线的线性浓度范围分别为2.00 - 2000 ng·mL⁻¹和1.00 - 1000 ng·mL⁻¹。二甲双胍和格列吡嗪的定量下限分别为2.00 ng·mL⁻¹和1.00 ng·mL⁻¹。该方法灵敏、简便、快速，适用于含二甲双胍和格列吡嗪复方制剂 的临床研究。
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