微波消解—原子荧光光谱法测定中药材中痕量镉 - 上海新仪微波化学 .pdfVIP

微波消解—原子荧光光谱法测定中药材中痕量镉* 1 1 1 1 2 1 杨东才 **，宁冬青 ，李为理 ，张文涛 ，侯海鸽 ，王素芬 （1.国家中成药工程技术研究中心 本溪 117004； 2.黑龙江大学化学化工与材料学院 哈尔滨 150080 ） 摘要 目的：建立用微波消解—原子荧光光谱法测定中药材中痕量镉的方法。方法：药材经微波消解后，以 二硫腙三氯甲烷溶液、氨基磺酸铵溶液、硫酸钾和氯化钡溶液为掩蔽剂，以硫脲和钴离子溶液为还原催化 剂，用原子荧光光谱法对药材中的痕量镉进行测定；同时考察载流盐酸、硼氢化钾浓度及共存元素的干扰。 结果：本法线性范围为 0.0~4.0 ng·mL-1 、相关系数大于 0.9990，最低检出浓度为 0.014 ng·mL-1 、回收率均 在 80% 以上。结论：本法具有操作简单、灵敏度高、重现性好等优点，能满足痕量镉的测定要求。 关键词：原子荧光光谱法；微波消解；中药材；镉 Determination of Micro Cadmium in Chinese Herbal Medicine Material with the Microwave Digestion and VG-AFS 1 1 1 1 2 1 YANG Dong-cai ，NING Dong-qing ，LI Wei-li ，ZHANG Wen-tao ，HOU Hai-ge ，WANG Su-fen (1．National Engineering Research Center for the Pharmaceutics of Traditional Chinese Medicines， Benxi 117006，China； 2. School of Chemistry and Materials Science, Heilongjiang University, Haerbin 150080，China) Abstract Objective:To establish a determination of micro cadmium in Chinese herbal medicine material with the microwave digest and VG-AFS. Methods:The samples were digested with the microwave,The dithizone- trichloromethane ammonnium sulfamate,potassium sulfate and barium chloride were used for masking some , disturbing elements，The sulfourea and Co2+ were used as reducing agent ，and VG-AFS was applied to determine micro cadmium in Chinese herbal medicine material. Meantime,the effect of concentrationof hydrochloric acid,potassium borohydride in carrier flow and the influence of the coexistence interference chemical element on the determination were studied. Results:The cadmium content showed linearity in the range of 0.5—4.0 ng mL-1,the linear correlation