论文部分内容阅读
建立了超声浸提-液相色谱/原子荧光光谱联用(LC-AFS)测定动物源性中药中As的4种形态(亚砷酸盐As(Ⅲ)、砷酸盐As(Ⅴ)、一甲基砷MMA、二甲基砷DMA)的分析方法。采用HNO_3(1+99)在75℃超声浸提1 h,与振荡热浸提方法进行对比,优化了仪器条件。方法应用于地龙、牡蛎、蛤壳、鸡内金和水蛭的测定,As各形态在7 min内实现基线分离,线性良好,相关系数在0.9993~0.9999之间,方法检出限为2.68~7.66μg/kg,精密度(RSD)为0.89%~2.2%,提取效率为91.0%~102.0%,鸡内金加标回收率为93.2%~104.0%。样品中4种砷形态之和占可提取态总量的11.8%~94.8%不等,表明大分子有机砷在动物源性中药中比例很高。
The four forms of As (Ⅲ), As (Ⅴ) and As (Ⅴ) in animal origin medicine were determined by LC-AFS. Methyl arsenic MMA, dimethyl arsenic DMA) analysis. Ultrasonic leaching with HNO 3 (1 + 99) at 75 ℃ for 1 h was compared with the oscillating hot extraction method to optimize the instrument conditions. The method was applied to the determination of earthworm, oyster, clam shell, chickweed and leeches. Each As species was baseline isolated within 7 min with a good linearity, the correlation coefficient was between 0.9993 and 0.9999, and the detection limit was 2.68 ~ 7.66 μg / kg, precision (RSD) was 0.89% ~ 2.2%, extraction efficiency was 91.0% ~ 102.0%, spike recovery was 93.2% ~ 104.0%. The sum of the four arsenic species in the sample ranged from 11.8% to 94.8% of the total amount of extractable species, indicating that the proportion of macromolecular organic arsenic in animal-derived traditional Chinese medicine is very high.