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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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ICP-MS法测定马来酸艾维替尼中钯、砷、镉、汞、铅的残留量

Determination of Pd,As,Cd,Hg and Pb residue in avitinib maleate by ICP-MS

分类号:R917
出版年·卷·期(页码):2020,40 (5):837-842
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立电感耦合等离子体质谱法(ICP-MS法)测定马来酸艾维替尼原料药中钯、砷、镉、汞、铅的残留量。方法:用微波消解进行样品前处理,采用ICP-MS以锗、铟、铋为内标进行测定,射频功率1.55kW,碰撞气为氦气,载气为氩气,载气流量0.8 L·min-1,泵速0.3 r·s-1,数据采集重复次数3次。结果:各待测元素线性关系良好(r>0.994 0);钯、砷、镉、汞、铅的平均加样回收率(n=3)范围分别为100.3%~111.9%、107.5%~111.9%、98.6%~101.4.%、90.5%~97.4%、116.9%~120.1%,RSD范围分别为2.8%~5.0%、1.4%~2.0%、0.50%~1.2%、1.1%~2.0%、1.9%~2.3%;精密度(重复性)、中间精密度的RSD<5%;检测下限为0.000 5~0.035 μg·g-1,定量下限为0.002~0.106 μg·g-1。3批样品(批号170501、A1000001、A1000002)中的钯含量分别为0.040 8、0.160 4、0.051 5 μg·g-1,砷、镉、汞、铅含量测定结果均低于检测下限。结论:该方法可用于马来酸艾维替尼原料药中钯、砷、镉、汞、铅残留量的测定。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To establish a method for the determination of Pd,As,Cd,Hg,Pb residue in avitinib maleate. Methods: Sample was digested by microwave and was determined by inductively coupled plasma mass spectrometry with Ge,In and Bi as internal standards. The detection conditions were as follows:RF power of 1.55 kW,collision gas of He,argon gas (carrier) flow rate of 0.8 L·min-1,pump speed of 0.3 r·s-1,and data collection time of 3. Results: The linearity of the detected elements was good (r>0.994 0),the average recoveries of Pd,As,Cd,Hg,Pb were 100.3%-111.9%,107.5%-111.9%,98.6%-101.4.%,90.5%-97.4%,116.9%-120.1%,and RSDs were 2.8%-5.0%,1.4%-2.0%,0.50%-1.2%,1.1%-2.0%,1.9%-2.3%(n=3),respectively. The RSDs of precison (repeatability) and intermediate precision tests were less than 5.0%,the detection limit values were 0.000 5-0.035 μg·g-1 and the quantitation limit values were 0.002-0.106 μg·g-1. The results of Pd residue in three batches (lot No. 170501,A1000001,A1000002) of samples were 0.040 8,0.160 4,0.051 5 μg·g-1,respectively. As,Cd,Hg and Pb were all less than respective limit of detection. Conclusion: The method is suitable for the determination of Pd,As,Cd,Hg and Pb in avitinib maleate.

-----参考文献:---------------------------------------------------------------------------------------
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