微波消解-电感耦合等离子体质谱法测定DPP-4抑制剂原料药中7种元素杂质  

Determination of 7 Impurity Elements in DPP-4 Inhibitor APIs by Microwave Digestion and Inductively Coupled Plasma Mass Spectrometry

作　　者：乔敏莎 郑秋莹 乔晓娜 张绿茵 兰为环 路晓慧 潘晓男 Qiao Minsha;Zheng Qiuying;Qiao Xiaona;Zhang Luyin;Lan Weihuan;Lu Xiaohui;Pan Xiaonan(Research Academy of Tasly Pharmaceutical Group Co.,Ltd.,Tianjin 300410,China)

机构地区：[1]天士力医药集团股份有限公司研究院,天津300410

出　　处：《化工与医药工程》2023年第3期23-28,共6页Chemical and Pharmaceutical Engineering

摘　　要：通过微波消解仪结合电感耦合等离子体质谱仪(ICP-MS)建立了DPP-4抑制剂原料药中钒、钴、镍、砷、镉、汞、铅7种元素杂质的含量测定方法,并对方法学进行了全面的验证。实验结果表明,7种元素标准曲线的相关系数在0.9993~0.9999之间,检出限均低于0.013 ng·mL^(-1),定量限低于0.038 ng·mL^(-1);重复性RSD低于3.0%;加标回收率为92.27%~107.58%;专属性、系统适用性和中间精密度均符合分析要求。测定的三批样品中7种元素的含量均远小于其限度值。所建立的方法稳定、准确、可靠,且操作简便,检测效率高,可用于DPP-4抑制剂原料药中元素杂质的分析检测,同时为药物的质量控制研究提供数据支持。A method for the determination of seven impurity elements including V,Co,Ni,As,Cd,Hg and Pb in DPP-4 inhibitor APIs was established by microwave digestion and inductively coupled plasma mass spectrometry(ICP-MS),and the methodology was comprehensively validated.The experiments show that the correlation coefficients of the standard curves of the seven elements-1 range from 0.9993 to 0.9999,the limits of detection are all below 0.013 ng·mL^(-1) and the limits of quantification are below 0.038 ng·mL^(-1);the RSD of reproducibility is below 3.0%;the recoveries are 92.27%-107.58%.Additionally,the specificity,system suitability and intermediate precision are all in accordance with the analytical requirements.The concentration of the seven elements in the three batches of samples determined are all lower than their limit values.The established method is stable,accurate,reliable,and easy to operate with high detection efficiency,which can be used for the analysis and detection of elemental impurities in DPP-4 inhibitor APIs,as well as providing data support for quality control studies of drugs.

关 键 词：电感耦合等离子体质谱(ICPMS) DPP-4抑制剂 原料药 元素杂质 

分 类 号：O657[理学—分析化学]