Determination of toxic impurity palladium in tofacitinib citrate by inductively coupled plasma emission spectrometry
XU Hui, XU Xiaoping, DONG Yao, PENG Tingting, HUANG Ting
Productivity Centre of Jiangsu Province, Physics & Chemistry Test Center of Jiangsu Province, Nanjing 210042, China
摘要：建立了电感耦合等离子体发射光谱法测定橼酸托法替布片中毒性杂质钯的含量。试样用体积分数为5%的硝酸溶液溶解，采用等离子体发射光谱法进行测定。钯的分析谱线为340.458 nm，质量浓度在0～1.0 mg/L
范围内与发射强度线性良好，线性相关系数为0.999 7，方法检出限为0.10 mg/kg。试样测定结果的相对标准偏差为2.55%(n=7)，加标回收率为96.8%～100.6%。该方法操作简便、重现性好、准确可靠，适用于橼酸托法替布片中毒性杂质钯的测定。
Abstract：ICP-OES method for the determination of toxic impurity palladium in tofacitinib citrate was established.The sample was dissoluted with 5% nitric acid solution, and then palladium in which was determined by ICP-OES. The analysis wavelength were 340.458 nm for Pd and the mass concentration of Pd was linear with the emission intensity in the range of 0-1.0 mg/L with the linear correlation coefficient of 0.999 7. The detection limit was 0.10 mg/kg. The relative standard deviation of the measurement results was 2.55%(n=7), and the recovery was 96.8%-100.6%. The method is simple, good reproducibility with the accurate and reliable results, and it is applicable to the determination of toxic impurity palladium in tofacitinib citrate.
Keywords：tofacitinib citrate; ICP-OES; Pd