微波消解-电感耦合等离子体质谱法测定糖代衍生物药粉中锇的残留量  

Determination of osmium residues in glycosylated derivative powder by microwave digestion-inductively coupled plasma mass spectrometry

作　　者：墨淑敏 胡月[2] 王长华 潘元海 李娜 邱长丹 MO Shu-min;HU Yue;WANG Chang-hua;PAN Yuan-hai;LI Na;QIU Chang-dan(Guobiao(Beijing)Testing&Certification Co.Ltd.,Beijing 100088;Central Iron&Steel Research Institute,Beijing 100081)

机构地区：[1]国标(北京)检验认证有限公司,北京100088 [2]钢铁研究总院,北京100081

出　　处：《分析试验室》2019年第11期1345-1347,共3页Chinese Journal of Analysis Laboratory

摘　　要：建立了微波消解-电感耦合等离子体质谱法(ICP-MS)测定糖代衍生物药粉中锇(Os)的残留量的方法。药粉中加入浓硝酸后微波消解,溶解完全后直接采用电感耦合等离子体质谱测定。由于Os的记忆效应严重,两次数据采集之间采用5%硝酸清洗5 min以上。方法检出限为7 ng/g。用建立的方法测定糖三种药粉中锇元素的残留量,加标回收率为91.7%~100.7%。3个批次的药粉分别测定11次,平行结果的相对标准偏差均小于5%。Method for the the determination of osmium residues in glycosylated derivative powder by microwave digestion-inductively coupled plasma mass spectrometry(ICP-MS)was established.The powder was digested by microwave after adding concentrated nitric acid,and then directly determined by inductively coupled plasma mass spectrometry(ICP-MS).Due to the serious memory effect of Os,5%nitric acid was used to clean the system between two data acquisitions for more than 5 minutes.The detection limit of Os was 7 ng/g.Osmium residues in three samples were detected by the established method.The recoveries were 91.7%-100.7%.Three batches of powder were determined11 times,and the relative standard deviations(RSDs)of parallel results were less than 5%.

关 键 词：微波消解 电感耦合等离子体质谱 糖代衍生物药粉 锇 

分 类 号：O657.63[理学—分析化学]