非那雄胺原料药中7种元素的ICP-MS分析  

ICP-MS Analysis of 7 Elements in Finasteride Bulk Drug

作　　者：李智明 杨娜 朱健萍 邓鸣 郑美玲 LI Zhiming;YANG Na;ZHU Jianping;DENG Ming;ZHENG Meiling(Guangxi Institute for Food and Drug Control,Nanning,Guangxi,530021,China)

机构地区：[1]广西食品药品检验所,广西南宁530021

出　　处：《广西科学》2020年第4期425-431,共7页Guangxi Sciences

基　　金：广西重点研发计划项目“一致性评价关键技术研究与应用——口服固体制剂溶出研究体系构建”(桂科AB18221125);“盐酸地芬尼多片质量与疗效一致性评价”(桂科AB17292049)资助。

摘　　要：建立电感耦合等离子体质谱(ICP-MS)法测定非那雄胺原料药中7种元素(As、Cd、Cr、Hg、Pb、Pd、Se)。样品经微波消解后,根据待测元素的特性,选用标准模式测定Se、选用碰撞模式(氦模式)测定其余元素,根据各元素的质量数选择相应元素作为内标,采用ICP-MS进行测定。积分时间为50 ms,射频功率为1550 W,作为载气的氩气流量为1.0 L/min,作为碰撞气的氦气流量为4.3 L/min,等离子体气流量为16.0 L/min,雾化器流量为1.0 L/mim;样品扫描20次,重复次数3次,使用Syngistix软件进行采集并分析数据。结果显示:As、Cd、Cr、Pb、Pd、Se的检测质量浓度线性范围均为1—20 ng/mL(r≥0.9995)、Hg的检测质量浓度线性范围为0.1—2.0 ng/mL(r=0.9998);检出限为1—30μg/kg,定量限为2—100μg/kg;回收率为92.0%—103.9%;精密度、稳定性试验的RSD均小于3.9%。该方法操作简便、灵敏度高、分析速度快、准确度好,适用于测定非那雄胺原料药中各元素的含量,对完善其质量标准具有参考意义。To establish a method for the determination of 7 elements(As,Cd,Cr,Hg,Pb,Pd,Se)in finasteride bulk drug by inductively coupled plasma mass spectrometry(ICP-MS).After the sample was digested by microwave,according to the characteristics of the element to be measured,the standard mode was selected to determine Se and the collision mode(helium mode)was selected to measure other elements.And then according to the mass of each element,the corresponding element was selected as the internal standard,and ICP-MS was used to determine.The integration time was 50 ms.The radio frequency power was 1550 W.The flow of argon as the carrier gas was 1.0 L/min.The flow of helium as the collision gas was 4.3 L/min.The plasma gas flow was 16.0 L/min.The flow rate of the atomizer was 1.0 L/mim.The samples were scanned 20 times and repeated 3 times.The data was collected and analyzed by Syngistix software.The result showed that the linear range of detection mass concentration of As,Cd,Cr,Pb,Pd,Se were 1 to 20 ng/mL(r≥0.9995),and the linear range of detection mass concentration of Hg was 0.1 to 2.0 ng/mL(r=0.9998).The detection limit was 1 to 30μg/kg,and the limit of quantification was 2 to 100μg/kg.The recovery rate was between 92.0%and 103.9%.The RSD of the precision and stability tests were both less than 3.9%.The method is simple to operate,high in sensitivity,fast in analysis speed,and good in accuracy.It is suitable for determining the content of each element in finasteride bulk drug,and it has reference significance for improving its quality standards.

关 键 词：非那雄胺 原料药 元素 电感耦合等离子体质谱 微波消解 重金属 

分 类 号：R917[医药卫生—药物分析学]