中文摘要：

目的：建立二甲双胍和格列吡嗪尿药浓度的测定方法,研究健康人群口服二甲双胍格列吡嗪片后二甲双胍和格列吡嗪的尿药排泄特征。方法：二甲双胍尿液样品用流动相稀释,经涡旋高速离心后,采用LichrospherODS色谱柱分离,流动相为乙腈-3mmol.L-1十二烷基硫酸钠（25：75）,用紫外检测器检测,波长为232nm。格列吡嗪尿液样品经盐酸酸化后用乙酸乙酯提取,采用LichrospherODS色谱柱分离,流动相为乙腈-0.1%的乙酸水溶液（55：45）,质谱采用电喷雾离子源和选择性离子检测方式。10名健康受试者单次口服二甲双胍格列吡嗪片2片后,测定给药前及给药后0～2、2～4、4～6、6～8、8～10、10～12、12～16、16～24h各时间段的二甲双胍及格列吡嗪尿药浓度。结果：高、中、低浓度的批间与批内精密度（RSD）相对标准差均小于10%。10名健康受试者单次口服二甲双胍格列吡嗪片后,24h内尿液中二甲双胍及格列吡嗪的累积排泄量分别为（102.5±27.3）mg和（452.2±191.4）μg,平均累积排泄率分别为（26.27±7.00）%和（9.04±3.83）%。结论：建立的人尿样中格列吡嗪的高效液相色谱-质谱联用（HPLC-MS）测定方法和二甲双胍的高效液相色谱（HPLC）测定方法准确、灵敏,适用于尿药排泄检测。

英文摘要：

Objective：To develop methods for determinating the urine level of metformin and glipizide and to study the urinary excretions of drugs in healthy Chinese volunteers after single dose administration.Methods：After metformin urine samples were diluted by mobile phase,the supernatant was injected into the system directly by using Lichrospher ODS column with a mobile phase of 3 mmol/L sodium dodecylsulfate（pH 4）：acetonitrile（75：25）,and the detected wavelength was 232 nm.Glipizide in urine samples was extracted with ethyl acetate after urine acidation,and separated on Lichrospher ODS column using acetonitrile and 0.1% acetic acid（10 mmol·L-1ammonium acetate）（55：45） as mobile phase.The mass spectrum was performed in the selected anion monitoring mode.Ten health Chinese volunteers were treated with single dose of two metformin-glipizide tablets.The metformin and glipizide concentrations in urine were determined before treatment and 0-2,2-4,4-6,6-8,8-10,10-12,12-16 and 16-24 h after treatment.Results：The inter-day and intra-day precision values were below 10%.In 24 h,the accumulation amounts of metformin and glipizide excreted in urine were（102.5±27.3） mg and（452.2±191.4） μg,respectively,the accumulated excretion rates were（26.27±7.00）% and（9.04±3.83）%,respectively after treatment.Conclusion：The assays（HPLC-MS and HPLC） have been proved to be accurate and sensitive,which can be used in the study of human urinary excretions of glipizide and metformin.