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

目的: 考察盐酸奈必洛尔原料药中催化剂钯的残留量。 方法: 采用电感耦合等离子体发射光谱法,测定波长为340.458 nm,以微波消解法进行样品前处理,并将测定结果与石墨炉原子吸收光谱法比较。 结果: 在10~100 ng·mL^-1的浓度范围内,钯的发射强度与浓度呈良好的线性关系,重复性试验的RSD为1.6%,加样回收率为94.2%,检测限为0.5 μg·g^-1。 结论: 该法可作为石墨炉原子吸收法的替代或补充,可用于原料药中催化剂钯的残留量测定。

Objective: To determine the residue amount of palladium which was used as a catalyst in drug substances of nebivolol hydrochloride. Methods: An inductively coupled plasma atomic emission spectrometry method was established and the detection wavelength was 340.458 nm.Microwave digestion was used for sample pretreatment.The determination results were compared with those by graphic furnace atomic absorption spectrometry. Results: The emission intensity and the concentration showed a good linear relationship in the 10-100 ng·mL^-1 concentration range,with the relative standard deviation of repeatability 1.6%,the recovery 94.2%,and the limit of detection 0.5 μg·g^-1. Conclusion: The method can be used for the determination of catalyst palladium residues in drug substances,as GFAAS methods alternative and complementary.

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