正丁醇萃取-稀盐酸溶解原子荧光光谱法间接测定中草药中钼

建立了正丁醇萃取稀盐酸溶解原子荧光光谱法间接测定中草药中钼的方法。基于As(Ⅴ)和钼酸铵在浓度为0.3 mol·L-1硫酸介质中能形成砷钼杂多酸，且该杂多酸可以被有机试剂萃取，萃取后蒸干有机试剂，残渣用稀盐酸加以溶解，原子荧光光谱法间接测定钼的含量。在优化的实验条件下，钼的含量在0～15 μg·L-1范围内呈良好的线性关系。方法的检出限是0.44 μg·L-1, 相对标准偏差1.1%。据此对中草药样品进行分析，平均加标回收率介于95.6%～101.3%之间。

Butanol Extraction Combined with Dilute Hydrochloric Acid Dissolution-Atomic Fluorescence Spectrometric Method for Indirect Determination of Molybdenum in Chinese Herbal Medicine

A method for indirectly determining the molybdenum in Chinese herbal medicine by butanol extraction and dilute hydrochloric acid dissolution was established for atomic fluorescence spectrometry. The molybdoarsenate heteropoly acid, formed in the presence of As(Ⅴ) and ammonium molybdate in 0.3 mol·L-1 sulphuric acid medium, was separated and enriched in the organic solvent, then the evaporation of organic reagent was implemented and the left residue was dissolved in dilute hydrochloric acid in which the arsenic content was determined on behalf of molybdenum. In the optimum experimental conditions, molybdenum content in 0～15 μg·L-1 range depicts a good linear relationship, the detection limit and relative standard deviation of 0.44 μg·L-1 and 1.1% were obtained, respectively. Spiked Chinese herbal medicine samples were determined with the proposed method, and recoveries of 95.6%～101.3% were achieved.