仿生提取-HPLC-ICP-MS测定含雄黄中成药中可溶性砷含量

目的: 建立仿生提取-高效液相色谱-电感耦合等离子体质谱联用技术(HPLC-ICP-MS)测定含雄黄中药制剂中可溶性砷形态含量的分析测定方法。 方法: 通过模拟人体胃肠道环境,采用人工胃液提取含雄黄中药制剂中的可溶性砷,结合HPLC-ICP-MS进行分离测定。 结果: 应用阴离子色谱柱10 min内成功分离4种形态砷——亚砷酸盐As(Ⅲ)、砷酸盐As(Ⅴ)一甲基砷(MMA)和二甲基砷(DMA)。方法的重复性良好,RSD为1.4%~1.5%;4种砷形态:亚砷酸盐As(Ⅲ)、砷酸盐As(Ⅴ)一甲基砷(MMA)和二甲基砷(DMA)的检出限分别为:0.10,0.10,0.10,0.20 μg·L^-1。 结论: 方法简便、灵敏、准确、重现性好,可用于含雄黄中药制剂中可溶性砷形态的分析测定。

Objective: To establish a method for determination of soluble arsenic in Chinese traditional patent medicine containing realgar by bionic extraction-HPLC-ICP-MS. Method: Through simulating stomach conditions,the arsenic species were extracted by artificial gastric juice and separated by high-pressure liquid chromatography (HPLC) with ICP-MS detection. Results: Separation of four arsenic species-As(Ⅲ),As(Ⅴ),MMA,DMA-was achieved with a anion-exchange column.The entire separation was accomplished in 10 min.The precision was calculated to be 1.4%-1.5% (RSD) for arsenic species.The HPLC-ICP-MS detection limits for the four arsenic species were in 0.10-0.20 μg·L^-1. Conclusion: The developed method is rapid,sensitive and accurate.It can be used for determination of arsenic species in Chinese traditional patent medicine.