微波消解样品-原子荧光光谱法测定维药中砷

HG-AFS Determination of Arsenic in Victoria Medicines with Microwave Assisted Sample Digestion

维药鹰嘴豆、花椒、黑胡椒样品经微波消解处理,采用氢化物发生-原子荧光光谱法测定其中砷的含量。试验优化了灯电流、负高压、载气流量、屏蔽气流量等仪器工作参数,并考察了相关化学反应的介质酸度、硼氢化钾浓度、预还原剂种类、微波消解条件和共存离子的干扰等试验条件。砷（Ⅲ）质量浓度在1.0-10.0μg.L^-1范围内与其荧光强度呈线性关系,方法的检出限（3s/k）为0.5μg.L^-1。方法用于维药分析,所得加标回收率在90.2%-99.4%之间。

The sample of Victoria medicines,i.e.chickpeas,pepper or black pepper,was treated by microwave digestion,and the content of arsenic（Ⅲ） in the sample solution was determined by hydride generation-atomic fluorescence spectrometry（HG-AFS）.Working parameters of the instrument including lamp current,negative high-voltage,the flow-rates of carrier gas and shielding gas and the chemical reaction conditions,including acidity of medium,concentration of potassium borohydride added,kinds of pre-reductants,conditions of sample digestion,and interferences of coexisting ions were studied and optimized.Linear relationship between values of fluorescence intensity and mass concentration of As（Ⅲ） was kept in the range of 1.0-10.0 μg·L^-1,with detection limits（3s/k） of 0.5 μg·L^-1.The proposed method was applied to the analysis of Victoria medicines,and values of recovery found were ranged from 90.2%-99.4%.