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建立了酸热浸提-高效液相色谱-原子荧光光谱联用技术对植物源性中药的砷形态分析的方法,同时建立了微波消解-原子荧光光谱法对植物源性中药总砷的分析方法。对砷形态分析技术的工作条件进行了优化,优化条件下,As(Ⅲ),As(Ⅴ),一甲基砷(M M A),二甲基砷(DM A)等4种砷形态的检出限在13.7~30.7μg/kg之间;形态砷标准溶液6次连续测定的相对标准偏差小于5%。方法应用于牛膝、油桂、菟丝子、巴戟天、补骨脂和大云等6种中药中的砷形态分析中,4种砷形态含量占砷总量比例80.8%~96.0%之间;牛膝样品各形态砷平均加标回收率在91.0%~104.6%之间。
A method for the determination of arsenic speciation in plant-derived Chinese herbs by acid-hot extraction-high performance liquid chromatography-atomic fluorescence spectrometry was established. At the same time, a method for the determination of total arsenic in plant-derived Chinese herbs was established by microwave digestion-atomic fluorescence spectrometry . The working conditions of arsenic speciation analysis were optimized. Under the optimum conditions, four kinds of arsenic speciation such as As (Ⅲ), As (Ⅴ), MMA and DM A were detected The limit is between 13.7 ~ 30.7μg / kg; the relative standard deviation of six consecutive determination of arsenic standard solution is less than 5%. Methods Arsenic speciation analysis was applied to 6 kinds of traditional Chinese medicines (Achyranthes, Anemarrhenae, Dodder, Morinda officinalis, Psoralen and Dahyun). The contents of four arsenic species accounted for 80.8% -96.0% of the total arsenic species. The average recoveries of arsenic in atrodia samples ranged from 91.0% to 104.6%.