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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10min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:0.10,0.10,0.10,0.20μg.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 the determination of soluble arsenic in realgar-containing traditional Chinese medicine preparations by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS). Methods: Soluble arsenic in realgar-containing traditional Chinese medicine preparations was extracted by artificial gastric juice by simulating the human gastrointestinal tract, and the content of soluble arsenic was determined by HPLC-ICP-MS. Results: Four kinds of arsenic - arsenite (As), arsenate As (Ⅴ) monomethyl arsenate (MMA) and dimethyl arsenic (DMA) were successfully separated by anion chromatography in 10 min. The repeatability of the method was good, with a RSD of 1.4% -1.5%. Four arsenic species: arsenite As (Ⅲ), arsenate As (Ⅴ) monomethyl arsenate (MMA) and dimethyl arsenic The detection limits were: 0.10,0.10,0.10,0.20μg.L-1. Conclusion: The method is simple, sensitive, accurate and reproducible. It can be used for the determination of soluble arsenic in realgar preparations containing realgar.