高效液相色谱-电感耦合等离子体质谱研究牛黄解毒片在水和胃肠液中溶出砷的形态  

Arsenic Speciation of Niuhuang Jiedu Tablets in Water and Gastrointestinal Fluids by HPLC-ICP-MS

作　　者：金鹏飞[1] 夏路风[1] 梁晓丽[1] 邝咏梅[1] 邹定[1] 胡欣[1] 

机构地区：[1]卫生部北京医院药学部,北京100730

出　　处：《中国药学杂志》2013年第24期2162-2165,共4页Chinese Pharmaceutical Journal

基　　金：北京市自然科学基金项目资助(7113164)

摘　　要：目的应用高效液相色谱一电感耦合等离子体质谱联机技术（HPLC—ICP—MS）考察牛黄解毒片在水和胃肠液中溶出砷的形态，对牛黄解毒片的砷毒性进行定量评价。方法应用高效液相色谱一电感耦合等离子体质谱联机技术技术建立三价砷、五价砷、单甲基砷酸、二甲基砷酸4种砷形态的定量方法和AsB、AsC2种砷形态的定性方法，并用该方法对牛黄解毒片的水提物、人工胃液提取物、人工肠液提取物分别进行砷形态分析。结果测定方法中三价砷、五价砷、单甲基砷酸、二甲基砷酸4种砷形态的线性相关系数（r）均大于0．9994，定量限（LOQ）在0．66～1．19μg·L-1之间，精密度和稳定性的相对标准偏差（RSD）都小于5％，加标回收率在92．78％～100．2％之间。分析结果显示，各提取物中只检出无机砷（AsⅢ和AsⅤ）和极微量的未知砷形态，均未检出单甲基砷酸、二甲基砷酸、砷甜菜碱、砷胆酸；牛黄解毒片在水和胃肠液中的溶出砷均以高毒性的无机砷为主。结论本方法可用于牛黄解毒片水提物和人工胃肠液提取物中砷形态的分析。OBJECTIVE To investigate the arsenic spcciation of Niuhuang Jiedu Tablets （ traditional Chinese medicines） in water and gastrointestinal fluids by HPLC-ICP-MS, so as to quantitatively evaluate the arsenical toxicity of Niuhuang Jiedu Tablets. METH- ODS An HPLC-ICP-MS method for the determination of Asm, Asv, MMA, DMA and the identification of AsB and AsC was estab- lished, and the arsenic speciation of Niuhuang Jiedu Tablets in water, gastric fluid, and intestinal fluid was determined and analyzed. RESULTS The method validation indicated that the correlation coefficients （r） for AsⅢ , AsⅤ , MMA, and DMA were all over 0.999 4, the limits of quantitation （LOQ） were between 0. 66 and 1.19μg · L-1, the precisions and stabilities were satisfactory with all RS- Ds less than 5%, and the spiked recoveries ranged from 92. 78% to 100. 2%. The results of samples analysis showed that only inor- ganic arsenic （ Asm and Asv ） and trace amount of unknown arsenic speciation were detected, while MMA, DMA, AsB, and AsC were not found in any cases;highly toxic inorganic arsenic （AsⅢ and AsⅤ） were dominating arsenic speciation of Niuhuang Jiedu Tablets in water and gastrointestinal fluids. CONCLUSION This method could be used for the arsenic speciation analysis of Niuhuang Jiedu Tablets in water and gastrointestinal fluids.

关 键 词：高效液相色谱法 电感耦合等离子体质谱 牛黄解毒片 水 胃肠液 砷形态 砷毒性 

分 类 号：R917[医药卫生—药物分析学]