论文部分内容阅读
目的应用高效液相色谱-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-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、AsC 2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0.999 4,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 study the morphology of arsenic in Niuhuangjiedu tablets by HPLC-ICP-MS and to evaluate the arsenic toxicity of Niuhuangjiedu tablets quantitatively. Methods A high performance liquid chromatography-inductively coupled plasma-mass spectrometry on-line technique was developed for the determination of four arsenic species of trivalent arsenic, pentavalent arsenic, monomethyl arsenate and dimethyl arsenate and two kinds of arsenic species AsB and AsC The qualitative method was used to analyze the arsenic speciation of Niuhuangjiedu tablets water extract, artificial gastric juice extract and artificial intestinal juice extract. Results The linear correlation coefficients (r) of the four arsenic species of trivalent arsenic, pentavalent arsenic, monomethylarsenic acid, and dimethyl arsenic acid were both greater than 0.999 4 and the LOQ values ranged from 0.66 to 1.19 μg · The relative standard deviations (RSDs) of precision and stability were all less than 5% and the recoveries of spiked samples ranged from 92.78% to 100.2%. The results showed that only arsenic, dimethyl arsenate, arsenobetaine and arsenocholic acid were not detected in all the extracts except inorganic arsenic (AsIII and AsV) and a trace amount of unknown arsenic. Bezoar detoxification tablets in the water and gastrointestinal solution of arsenic are highly toxic inorganic arsenic-based. Conclusion This method can be used for the analysis of arsenic speciation in the extracts of Niuhuangjiedu tablet and artificial gastrointestinal juice.