HPLC-MS/MS法测定阿哌沙班中硝基物和酰氯物  

Determination of nitro compound and acyl chloride in Apixaban by HPLC-MS/MS

作　　者：冯秀珍 邵伍军 和燕玲 FENG Xiuzhen;SHAO Wujun;HE Yanling(Zhejiang Hisun Pharmaceutical Co.,Ltd.,Taizhou Zhejiang 318000,China)

机构地区：[1]浙江海正药业股份有限公司,浙江台州318000

出　　处：《中兽医医药杂志》2025年第2期74-77,共4页Journal of Traditional Chinese Veterinary Medicine

基　　金：台州市科学技术局(24nya17);浙江省2023年度高校国内访问工程师校企合作项目(FG2023323)。

摘　　要：建立高效液相色谱-三重四极杆质谱(HPLC-MS/MS)法测定阿哌沙班中硝基物和酰氯物的方法。样品用50%乙腈溶液溶解,经Agilent Eclipse Plus C_(18) RRHD(50.0 mm×2.1 mm,1.8µm)色谱柱梯度洗脱分离,以三重四极杆质谱为检测器,质谱采用电喷雾离子源及MRM(multi-reaction monitoring,多反应监测),以正离子模式采集数据,对阿哌沙班中硝基物和酰氯物同时进行检测。结果显示,硝基物和酰氯物在1.0~20.0 ng/mL浓度范围内与峰面积线性关系良好,相关系数r>0.99;检测限浓度为0.3 ng/mL,定量限浓度为1.0 ng/mL;阿哌沙班溶液中硝基物和酰氯物的回收率为96.2%~98.8%,RSD为1.4%~2.7%。该方法可有效消除溶剂效应与基质效应对硝基物和酰氯物检测的影响,可用来准确测定阿哌沙班中硝基物和酰氯物的含量。To establish a HPLC-MS/MS(high-performance liquid chromatography triple quadrupole mass spectrometry)method for the determination of nitro compound and acyl chloride in Apixaban.Sample was dissolved by acetonitrile aqueous solution and were separated by gradient elution on an Agilent Eclipse Plus C_(18) RRHD(50.0 mm×2.1 mm,1.8µm)chromatographic column.Triple quadrupole mass spectrometry detector was used to collect data using the positive mode,ion electrospray ionization(ESI)source and MRM(multi reaction monitoring)mode.The nitro compound and acyl chloride were simultaneously detected by HPLC-MS/MS in Apixaban.The correlation coefficient(r)of the nitro compound and acyl chloride in the concentration range of 1.0-20.0 ng/mL were greater than 0.99.The detection limit concentrations were 0.3 ng/mL,and the quantification limit concentrations were 1.0 ng/mL.The recovery rate were 96.2%-98.8%with RSD of 1.4%-2.7%.This method can effectively eliminate the effects of solvent and matrix on the detection of nitro compound and acyl chloride,meanwhile it can be used to accurately determine the content of nitro compound and acyl chloride in Apixaban.

关 键 词：高效液相色谱 三重四极杆质谱 阿哌沙班 硝基物 酰氯物 

分 类 号：S859.1[农业科学—临床兽医学]