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目的:建立快速准确“浙八味”中微量砷元素测定方法。方法:采用MK-Ⅲ型微波消解仪消解“浙八味”药材,并结合原子荧光光谱法(AFS)测定砷元素含量。结果:在混合酸体系HNO3—HCl中,当混合酸摩尔比为10∶2、微波功率300 W、消解时间5 min、固液比为1∶14的条件下,消解结果最佳。在此条件下进行精密度实验和回收率实验,所得结果的相对标准偏差在0.595%~3.016%之间,回收率在98.59%~104.1%之间。结论:微波消解法处理“浙八味”药材,具有快速、简便、节省试剂、消解完全等特点,测定结果的精密度和准确度令人满意。
Objective: To establish a rapid and accurate method for the determination of trace arsenic in “Zhe Ba Zawei”. Methods: The MK-III microwave digestion device was used to digest the “Zhe Ba Wei” medicinal materials, and the content of arsenic was determined by atomic fluorescence spectrometry (AFS). Results: In the mixed acid system HNO3-HCl, when the mixed acid molar ratio was 10:2, the microwave power was 300 W, the digestion time was 5 min, and the ratio of solid to liquid was 1:14, the digestion result was the best. The precision experiments and recovery experiments were performed under these conditions. The relative standard deviations of the obtained results were between 0.595% and 3.016%, and the recoveries were between 98.59% and 104.1%. Conclusion: The microwave digestion method for processing the “Zhe Ba Wei Wei” medicinal materials has the characteristics of rapidity, simplicity, saving of reagents, complete digestion, etc. The precision and accuracy of the results are satisfactory.