摘要
目的建立一种LC-MS/MS方法用于大鼠血浆中舒必利血药浓度的测定及其药代动力学研究。方法血浆样本经过液液萃取方法处理后,采用电喷雾离子化(ESI),正离子多重反应监测模式(MRM)。舒必利和奥美拉唑用于定量分析的离子对为m/z 342.2→112.2和346.4→198.1。色谱柱为Hedera ODS-2柱(150 mm×2.1 mm,5μm),流动相是甲醇(含0.1%甲酸)-水(0.05%甲酸铵和0.1%甲酸),按照等度洗脱方式(7∶3,V/V)进行。结果该方法的定量下限是0.5 ng·mL^(-1),舒必利在0.5~200 ng·mL^(-1)内与峰面积比值线性关系良好,舒必利和内标奥美拉唑的提取回收率在70%~80%,批间和批内精密度均小于15%,方法学验证的结果符合生物样本分析指导原则要求。结论建立的LC-MS/MS方法特异性强,分析时间短,适用于大量生物样本的检测,成功应用于大鼠血浆样本的药代动力学研究,可为舒必利的临床药物浓度监测方法的开发提供参考。
Objective To monitor the concentration of sulpiride in the plasma,and to conduct its pharmacokinetic by LC-MS/MS.Methods Plasma samples were collected by liquid-liquid extraction method.Sulpiride and omeprazole for quantitative analysis were m/z 342.2→112.2 and 346.4→198.1.The determination was performed on Hedera ODS-2 column(150 mm×2.1 mm,5μm).The mobile phase was methanol(containing 0.1%formic acid)and water(0.05%ammonium formate and 0.1%formic acid)=(7∶3,V/V).Results The lower limit of quantification of the method was 0.5 ng·mL^(-1),and the linearity was good at 0.5~200 ng·mL^(-1).The extraction recovery of sulpiride and internal standard omeprazole ranged 70%~80%,and the RSD were less than 15%.The methodology verification was in line with the requirements of guidelines for biological sample analysis.Conclusion The LC-MS/MS method is suitable for the detection of large biological samples.It has been successfully used in the pharmacokinetic study and concentration monitoring of sulpiride.
作者
梁媛
葛若衡
舒畅
LIANG Yuan;GE Ruo-heng;SHU Chang(Key Laboratory of Drug Quality Control and Pharmacovigilance in China Pharmaceutical University,Ministry of Education,Nanjing 210009;Department of Pharmaceutical Analysis,School of Pharmacy,China Pharmaceutical University,Nanjing 211198)
出处
《中南药学》
2023年第11期2875-2879,共5页
Central South Pharmacy
基金
药物质量与安全预警教育部重点实验室资助项目(No.DQCP20/21PQ02)
江苏省特色资源开发与药用研究重点实验室(No.LPRK202102)。
作者简介
梁媛,女,硕士研究生,主要从事药物分析以及多肽药物成药性研究,email:153305186175@163.com;通信作者:舒畅,女,硕士研究生导师,主要从事药物质量标准、体内药物分析新技术研究,email:shuchang@cpu.edu.cn。
