佐太等珍宝矿物类藏药材中总砷、总汞及可溶性砷汞含量的对比研究

目的:测定佐太等珍宝矿物类藏药材中总砷、总汞以及可溶性砷汞的含量,对比评价分析珍宝矿物类藏药材中有关砷汞类有害物质的安全性。方法:通过高压密闭微波消解及聚焦微波消解技术消解珍宝矿物类藏药材样品提取其中总砷、汞,同时通过模拟人体胃肠道环境,采用人工胃液仿生提取样品中的可溶性砷、汞,结合氢化物-原子荧光法进行分析测定。最佳仪器工作条件为光电倍增管负高压270 V,原子化器高度10 mm,载气流量400 mL·min^-1,屏蔽气流量800 mL·min^-1,砷灯电流为40 mA、汞的灯电流为20 mA。结果:在选定的最佳条件下,仪器对砷与汞的检测限分别为0.15μg·L^-1和0.02μg·L^-1,日内精密度RSD分别为1.94%和2.18%,日间精密度RSD分别为2.02%和2.39%;总砷、总汞的平均回收率分别为94.3%、92.0%,可溶性砷、可溶性汞的平均回收率为93.0%、91.3%,RSD均小于5%。佐太、朱砂、银珠、雄黄4个品种10批样品的总砷含量为31.49~485829μg·g^-1,总汞含量为0.004~742187μg·g^-1;可溶性砷的含量为0.43~1162μg·g^-1,可溶性汞的含量为0~79.55μg·g^-1。结论:珍宝矿物类藏药材中可溶性砷汞的含量远远低于总砷汞的含量。

Objective: To simultaneously determine the total and soluble arsenic, mercury in the Tsothel and other precious Tibetan medicines, so as to compare and analyze the safety of poisonous elements such as arsenic and mercury.Methods: Through Closed-vessel microwave-assisted digestion, total arsenic and mercury were extracted from the samples.Then, the soluble arsenic, and mercury were extracted by artificial gastric juice simulating stomach conditions, and detected by hydride generation-atomic fluorescence spectrometry.The optimum operational conditions of the instrument was as follows: photomultiplier tube negative pressure was 270 V, atomization device-height was 10 mm, the carrier flow was 400 mL·min^-1, shielding flow was 800 mL·min^-1, lamp current of arsenic was 40 mA, and lamp current of mercury was 20 mA.Results: Under optimal conditions, the detection limits of arsenic and mercury were 0.15 μg·L^-1and 0.02 μg·L^-1, RSDs of within-day were 1.94% and 2.18%, and RSDs of between-day were 2.0% and 2.4%. The average recoveries of total As and Hg were 94.3% and 92.0%.The average recoveries of soluble As and Hg were 93.0% and 91.3%, while RSDs were less than 5%. The result of total As and Hg in the 10 batches of samples of Tsothel, Cinnabaris, Realgar, et al, were 31.49-485 829 μg·g^-1and 0.004-742 187 μg·g^-1;the result of soluble As and Hg were 0.43-1 162 μg·g^-1 and 0-79.55 μg·g^-1.Conclusion: The content of soluble arsenic, mercury in the Tsothel and other precious Tibetan crude drugs is much less than the total.