摘要
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 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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2010年第10期1829-1835,共7页
Chinese Journal of Pharmaceutical Analysis
基金
国家支撑计划子课题(2006BAI06A01-04)
中药中重金属及农药残留检测技术研究
天津市科技发展计划项目(05SYSYGX25000)
中药质量现状评价与标准研究
天津市农科院院长基金项目(08014)
含矿物药中药制剂中砷
汞元素形态分析检测技术的研究
关键词
砷形态
仿生提取
HPLC-ICP-MS
中成药
雄黄
arsenic species
bionic extraction
HPLC-ICP-MS
Chinese traditional patent medicine
realgar