LC-MS/MS法测定人血浆中阿哌沙班的浓度  

Determination of apixaban concentration in human plasma by LC-MS/MS

作　　者：田继堂 王娜 张红菱[3] 陈琳 TIAN Ji-tang;WANG Na;ZHANG Hong-ling;CHEN Lin(Zhejiang Huayuan Pharmaceutical Co.,Ltd.,Dongyang Zhejiang 322100;College of Life Sciences and Technology,Wuhan Polytechnic University,Wuhan 430023;College of Medicine and Health Sciences,Wuhan Polytechnic University,Wuhan 430023;Nanjing Simoslab Testing Technology Corp.,Ltd.,Nanjing 210000)

机构地区：[1]浙江花园药业有限公司,浙江东阳322100 [2]武汉轻工大学生命科学与技术学院,武汉430023 [3]武汉轻工大学医学与健康学院,武汉430023 [4]南京西默思博检测技术有限公司,南京210000

出　　处：《中南药学》2023年第8期2106-2110,共5页Central South Pharmacy

摘　　要：目的建立LC-MS/MS法测定人血浆中阿哌沙班的浓度。方法以阿哌沙班-^(13)C-d_(3)为内标,血浆经乙腈沉淀蛋白后,采用Poroshell 120 EC-C_(18)(4.6 mm×50 mm,2.7μm)色谱柱分离,以5%乙腈水溶液为流动相A,乙腈为流动相B,流速0.7 mL·min^(-1),线性梯度洗脱,电喷雾离子化源(ESI)正离子模式,以选择反应监测(SRM)模式监测阿哌沙班(m/z 460.08→443.17)和内标阿哌沙班-^(13)C-d_(3)(m/z 464.08→447.08)。结果人血浆中的阿哌沙班标准曲线方程为Y=2.303X+0.121(R^(2)=0.994),经验证阿哌沙班在0.500~200ng·mL^(-1)内线性关系良好。结论本法操作灵敏简便,具有可靠性,可用于阿哌沙班人体内血药浓度的测定及药代动力学和生物等效性研究。Objective To establish a liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for the determination of apixaban concentration in human plasma.Methods Apixaban-^(13)C-d_(3) was used as the internal standard.After protein precipitation by acetonitrile,Poroshell 120 EC-C_(18)(4.6 mm×50 mm,2.7μm)chromatographic column was used for the separation with 5%acetonitrile aqueous solution as mobile phase A,and acetonitrile as mobile phase B at 0.7 mL·min-1 with linear gradient elution.Electrospray ionization source under positive ion and selected reaction monitoring mode were used.The ion transitions were m/z 460.08→443.17(apixaban)and m/z 464.08→447.08(apixaban-^(13)C-d_(3)).Results The standard curve equation of apixaban in human plasma was Y=2.303X+0.121(R^(2)=0.994).Apixaban had a good linear relationship at 0.500~200 ng·mL^(-1).Conclusion The LC-MS/MS method is sensitive,simple and reliable.It can be used for the determination of plasma concentration of apixaban in human body,and study its pharmacokinetics and bioequivalence.

关 键 词：阿哌沙班 LC-MS/MS 血药浓度 

分 类 号：R917[医药卫生—药物分析学] R96[医药卫生—药学]