摘要
建立灵敏、简便的液相色谱串联质谱法同时测定人血浆中的瑞格列奈和二甲双胍。采用d5-瑞格列奈和d6-二甲双胍作为内标,血浆样品经乙腈沉淀蛋白,以乙腈10 mmol.L1醋酸铵为流动相,通过Venusil ASBC18柱(150 mm×4.6 mm,5μm)梯度洗脱,色谱运行时间为7.5 min。采用大气压化学电离源,以多反应监测方式进行正离子检测。瑞格列奈标准曲线的线性范围为0.2～60.0 ng.mL1,二甲双胍为4～1 000 ng.mL1。两待测物的日内、日间精密度和准确度均小于15%。本方法灵敏、简便,已成功应用于人体药动学和生物等效性研究。
A simple, sensitive, selective, and reproducible liquid chromatography-tandem mass spectrometric method was developed for the simultaneous determination of repaglinide and metformin in human plasma using ds-repaglinide and d6-metformin as internal standards （ISs）. After a simple protein precipitation using acetonitrile as the precipitation solvent, both analytes and ISs were separated on a Venusil ASB C 18 （150 mm x 4.6 mm, 5 p.m） via gradient elution using acetonitrile- 10 mmol.L-1 ammonium acetate as the mobile phase. A chromatographic total run time of 7.5 min was achieved. Mass spectrometric detection was conducted with atmospheric pressure chemical ionization under positive-ion and multiple-reaction monitoring modes. The method was linear over the 0.2 to 60.0 ng＇mL-1 concentration range for repaglinide and over the 4 to 1 000 ng .mL-l range for metformin. For both analytes, the intra- and inter-accuracies and precisions were within the a：15% acceptable limit across all concentrations. The validated method was successfully applied to a clinical bioequivalence study.
出处
《药学学报》
CAS
CSCD
北大核心
2013年第4期547-553,共7页
Acta Pharmaceutica Sinica
