今日药学

2021, v.31(02) 128-130

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电感耦合等离子体发射光谱法(ICP-OES)测定枸橼酸托法替布中钯、铑残留量
Determination of Pd and Rh Metal Residues in Tofacitinib Citrate by Inductively Coupled Plasma-optical Emission Spectrometer( ICP-OES)

廖佳;刘健;吴晓妍;陈巧兰;梁玉英;
LIAO Jia;LIU Jian;WU Xiaoyan;CHEN Qiaolan;LIANG Yuying;Technical Centre of Gongbei Customs District;Ecological and Environmental Monitoring Center of Chongqing;Zhuhai Labfy Technical Services Co.,Ltd;

摘要(Abstract):

目的建立枸橼酸托法替布中钯、铑残留量的测定方法。方法样品用浓硫酸碳化,加浓硝酸及高氯酸消解后,采用电感耦合等离子体发射光谱法(ICP-OES)测定钯、铑元素含量。结果各元素线性关系良好,相关系数(r)均大于0.999,钯和铑的方法检出限为分别为0.10 mg·kg~(-1)和0.25 mg·kg~(-1),加标回收率在88.9%~104.1%之间,相对标准偏差RSD为1.3%~4.3%(n=12)。结论该方法准确、可靠,可用于枸橼酸托法替布中钯、铑的残留量的测定。
OBJECTIVE To establish a method for determination of Pd and Rh metal residues in tofacitinib citrate. METHODS After the samples were carbonized by concentrated sulphuric acid,digested by nitric acid and perchloric acid,Pd and Rh residues were determined by inductively coupled plasma-optical emission spectrometer( ICP-OES). RESULTS The linearity of each metal was good and the correlation coefficient were over 0.999. The method detection limits of Pd and Rh were 0.10 mg·kg~(-1) and 0.25 mg·kg~(-1).The recovery percentage of standard samples was 88.9%-104.1%. RSD was between 1.3%-4.3%. CONCLUSION The method is accurate and reliable,and can be used for the determination of Pd and Rh residues in tofacitinib citrate.

关键词(KeyWords): 电感耦合等离子体发射光谱法;枸橼酸托法替布;钯;铑
ICP-OES;tofacitinib citrate;Pd;Rh

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基金项目(Foundation): 珠海进出口公共技术服务平台产学研协同创新计划目(IETP201901012)

作者(Author): 廖佳;刘健;吴晓妍;陈巧兰;梁玉英;
LIAO Jia;LIU Jian;WU Xiaoyan;CHEN Qiaolan;LIANG Yuying;Technical Centre of Gongbei Customs District;Ecological and Environmental Monitoring Center of Chongqing;Zhuhai Labfy Technical Services Co.,Ltd;

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