微波消解火焰-原子吸收光谱法测定药用辅料 硬脂酸镁中痕量铅、镍、镉

目的:建立火焰原子吸收光谱法测定药用辅料硬脂酸镁中痕量铅、镍、镉的含量。方法:药用辅料硬脂酸镁经微波消解或经湿法消解后,采用火焰-原子吸收光谱法测定痕量铅、镍、镉,并同时考察这两种样品处理方法对测定结果的影响。结果:微波消解法对样品测定结果优于湿法消解;镉0.42～1.12 mg·L-1,镍3.80～4.06 mg·L-1,铅5.07～10.31 mg·L-1。在选定分析条件下,镉、镍、铅检出限分别为0.001 2,0.002 9,0.003 4 mg·L,1,RSD分别为0.2%,2.9%,2.7%,回收率分别为为109.18%,101.30%,99.69%。结论:本法具有操作简单、灵敏度高、重复性好等优点,能满足痕量铅、镍、镉的测定要求,为药用辅料硬脂酸镁的质量控制提供依据。

Determination of Trace Amount Lead,Niccolum,and Cadmium in Oficinal Magnesium Stearate with Microwave Digestion and Flame-atomic Absorption Spectroscopy

Objective: Set up a flame-atomic absorption spectroscopy method with cadmium,niccolum,and lead in oficinal magnesium stearate. Method: Oficinal magnesium stearate disposed via microwave digestion or accustomed digestion,adopting Flame-Atomic Absorption Spectroscopy to determine trace amount lead,niccolum,and cadmium,and review the influence of determination from both disposal. Result: The result of determination by microwave digestion is better than accustomed digestion.The results of determination are as follows: cadmium was 0.42-1.12 mg ·L^-1,niccolum was 3.80-4.06 mg ·L^-1,lead was 5.07-10.31 mg ·L^-1.The limit of determination of cadmium,niccolum,and lead are 0.001 2,0.002 9,0.003 4 mg ·L^-1,the RSD are 0.2%,2.9%,2.7%,the recovery are 109.18%,101.30%,99.69%. Conclusion: This method possesses excellence of simplify manipulation,high veracity and nicer repeatability.It can content the need of trace amount,cadmium,niccolum,and lead determination and offer basis for quality control of oficinal magnesium stearate.