原子吸收光谱法测定化学原料药(对甲苯磺酸拉帕替尼)中的钯

Determination of Palladium Residue in Raw Material Drug(p-toluenesulfonic acid) by GFAAS

本文通过配制钯系列标准溶液,采用标准曲线法,验证了标准曲线方程和相关系数、钯回收率及检出限和定量限。结果确定该方法的相关系数为0.999以上,钯回收率较好,在92%～98%之间。方法检出限为0.0297 mg/kg,方法定量限为0.0899mg/kg,RSD值为2.45%。该法可以完全用于原料药(对甲苯磺酸拉帕替尼)中钯催化剂钯残留的测定,可为药品(对甲苯磺酸拉帕替尼)的质量控制提供依据。

Objective: to establish a method for the determination of palladium residue in raw material drug(p-toluenesulfonic acid) by graphite furnace atomic absorption spectrometry(GFAAS). The content of palladium in three batches of raw materials was determined. Methods: the working parameters of atomic absorption spectrometer: atomizer: graphite furnace;Protective gas: Ar;determination wavelength: 247.64 nm;slit: 0.7 nm;working lamp current: 10.0 Ma;sample volume: 20.0 μL;light source: Palladium hollow cathode lamp;buckling background mode: Zeeman effect;determination method: standard curve method. By preparation of palladium series standard solution, the standard curve equation, correlation coefficient, palladium recovery rate, detection limit and quantitative limit were verified. Results: the correlation coefficient of this method was more than 0.999, and the recovery rate of palladium was better. The detection limit of the method is 0.0297 mg/kg and the quantitative limit is 0.0899 mg/kg-1, and RSD was 2.45%. The method is simple, rapid, sensitive and accurate. It can be used for the determination of palladium residue over palladium catalyst in raw material drug(p-toluenesulfonate). The method can provide basis for quality control of the drug(p-toluenesulfonate rapatini).