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建立HPLC-MS/MS法测定人血浆中奥美拉唑(OPZ)及代谢物奥美拉唑砜(S-OPZ)、5-羟基奥美拉唑(HOPZ)的浓度,以用于奥美拉唑的药代动力学研究。采用Phenomenex Gemini C18(50 mm×3.0 mm,5μm)色谱柱,乙腈-水(体积比40∶60)为流动相,流量0.2 m L/min,以d3-奥美拉唑(d3-OPZ)作内标,血浆样本用二氯甲烷∶异丙醇(体积比97∶3)萃取,采用ESI源,正离子MRM模式检测。OPZ在0.5~600 ng/m L范围内,S-OPZ和H-OPZ在0.25~300 ng/m L范围内线性良好;OPZ、S-OPZ、H-OPZ及IS的保留时间分别为3.19,4.18,1.96,3.19 min左右;萃取回收率在53.8%~84.6%;高浓度血浆样品稀释4倍测定不影响结果 ;精密度、基质效应经内标校准后均合格;稳定性各项数据均符合相关要求。该法快速、灵敏、专属性强、重现性好,适用于奥美拉唑及其代谢物的血药浓度测定。
To establish a method for the determination of omeprazole (OPZ) and its metabolites omeprazole sulfone (S-OPZ) and 5-hydroxy omeprazole (HOPZ) in human plasma by HPLC-MS / Pharmacokinetic study of. The mobile phase consisted of Phenomenex Gemini C18 (50 mm × 3.0 mm, 5 μm) column with acetonitrile-water (40:60 by volume) at a flow rate of 0.2 mL / min and d3-omeprazole The internal standard, plasma samples were extracted with dichloromethane: isopropanol (97: 3 by volume) and detected by ESI source and positive ion MRM mode. OPZ was linear over the range of 0.5-600 ng / m L and S-OPZ and H-OPZ were linear over the range of 0.25-300 ng / m L. The retention times of OPZ, S-OPZ, H-OPZ and IS were 3.19, 4.18,1.96,3.19 min or so; extraction recovery was 53.8% ~ 84.6%; high concentration plasma samples diluted 4 times did not affect the results measured; precision, matrix effect after passing the internal standard calibration are qualified; the stability of the data are in line with related requirements. The method is fast, sensitive, specific and reproducible. It is suitable for the determination of plasma concentration of omeprazole and its metabolites.