电感耦合等离子体质谱法测定醋酸阿比特龙原料药中钯的残留量
ICP-MS Determination of Residual Amount of Palladium in Zytiga Bulk Drugs
摘 要
0.500 0 g醋酸阿比特龙原料药样品经5.0 mL硝酸和1.0 mL高氯酸微波消解后，加热至近干，将消解液用水定容至25 mL，采用电感耦合等离子体质谱法测定其中钯的残留量。采用带有碰撞反应池的氦调谐模式，以相对丰度较高、抗干扰更强的105Pd作为同位素，以115In作为内标。钯的线性范围在80.0 μg·L-1以内，检出限（3.3s/k）为0.020 8 μg·L-1。方法用于醋酸阿比特龙原料药样品的分析，测定值的相对标准偏差（n=6）为1.2%，加标回收率为94.0%~100%。
醋酸阿比特龙
原料药
钯
ICP-MS
Zytiga
bulk drug
palladium
Abstract
The sample (0.500 0 g) of Zytiga bulk drug was dissolved with 5.0 mL of HNO3 and 1.0 mL of HClO4 with microwave digestion. The above solution was heated to near dryness, and then the digestion solution was diluted to 25 mL with water. ICP-MS was applied to the determination of residual amount of palladium in the solution. He tuned mode with collision pool was used, and 105Pd with higher abundance and stronger anti-interference was used as isotope. 115In was used as internal standard. Linearity range of palladium was found in the range within 80.0 μg·L-1 with detection limit (3.3s/k) of 0.020 8 μg·L-1. The proposed method was applied to the analysis of the sample of Zytiga bulk drug, giving value of RSD (n=6) of 1.2%. Values of recovery found by standard addition method were in the range of 94.0%-100%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201808007
所属栏目 工作简报
基金项目 北京市财政项目（PXM2016-178305-000017
收稿日期 2017/9/12
修改稿日期
网络出版日期
作者单位点击查看
联系人作者赵婷(zhaoting@163.com)
备注徐聪,硕士研究生,主要从事光谱、质谱分析工作
引用该论文: XU Cong,ZHAO Ting,HUANG Zhao,ZHANG Mei,LIU Weili. ICP-MS Determination of Residual Amount of Palladium in Zytiga Bulk Drugs[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(8): 901～905
徐聪,赵婷,黄曌,张梅,刘伟丽. 电感耦合等离子体质谱法测定醋酸阿比特龙原料药中钯的残留量[J]. 理化检验－化学分册, 2018, 54(8): 901～905
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【5】BEGEROW J, TURFELD M, DUNEMANN L. Determination of physiological palladium, platinum, iridium and gold levels in human blood using double focusing magnetic sector field inductively coupled plasma mass spectrometry[J]. Journal of Analytical Atomic Spectrometry, 1997,12(9):1095-1098.
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【7】谢贞建,袁海梅,孙敏,等.基于火焰原子吸收光谱法的苯甲酸阿格列汀中残留钯测定[J].成都大学学报(自然科学版), 2016,35(3):215-217.
【8】NANCY L. The use of atomic spectroscopy in the pharmaceutical industry for the determination of trace elements in pharmaceuticals[J]. Microchemical Journal, 2011,55(4):653-661.
【9】JIA X, WANG T, WU J. Determination of palladium by graphite furnace atomic absorption spectroscopy without matrix matching[J]. Talanta, 2008,54(4):741-751.
【10】陈阳,金薇,杨永健.电感耦合等离子体发射光谱法测定盐酸奈必洛尔原料药中催化剂钯的残留量[J].药物分析杂志, 2012,32(1):2226-2228.
【11】SHI J Y, LI Z H. Application of ICP-AES method in chemical analysis[J]. Hebei Electric Power, 2003,22(Suppl 1):43-44.
【12】李莉,赵佳莉.微波消解-电感耦合等离子体质谱(ICP-MS)法测定化学原料药中痕量钯元素[J].中国无机分析化学, 2016,6(1):6-9.
【13】张振兴,王强,杨凤,等.微波消解-ICP-MS法测定利奈唑胺中残留钯[J].化学研究与应用, 2013,25(1):134-136.
【14】张亚红,李华龙.电感耦合等离子体质谱法测定阿加曲班原料药中催化剂钯的残留量[J].药物分析杂志, 2016,36(9):1667-1670.
【15】BENDAKOVSKÁ L, KREJCOVÁ A, CERNOHORSKÝ T. Development of ICP-MS and ICP-OES methods for determination of gadolinium in samples related to hospital waste water treatment[J]. Chemical Papers, 2016,70(9):1155-1165.
【16】陈岩,赵晓丽,杨慧,等.湿法消解ICP-MS法测定紫菜和海带中15种元素[J].分析试验室, 2015,34(7):803-806.
【17】王文青,张丽媛,魏宇锋,等.微波消解-ICP-MS法测定食品级润滑油(脂)中的锑、砷、镉、铅、汞、硒[J].分析试验室, 2014,33(12):1430-1433.
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