ICP-MS研究牛黄解毒片中20种微量元素的总量及在水和胃肠液中的溶出特性

Study on total contents of 20 trace elements in Niuhuang Jiedu tablets and their extract rates in water and gastrointestinal fluids by ICP-MS

目的： 应用电感耦合等离子体质谱（ICP-MS）技术研究牛黄解毒片中20种微量元素的总量及其在水和胃肠液中的溶出特性。 方法： 应用ICP-MS技术建立20种微量元素的同时测定方法，并用该方法对不同厂家牛黄解毒片中20种元素的总量、水中溶出率、人工胃液中溶出率及人工肠液中溶出率进行测定、比较和分析。 结果： 测定方法中20种元素的线性相关系数（r）均大于0.9990；牛黄解毒片及提取液中元素测定方法的精密度、稳定性和回收率均能满足实验要求；NIST西红柿叶标准物质（SRM 1573a）的测定值和标准值之间也有良好的一致性。测定结果显示：部分牛黄解毒片存在雄黄投药不足的问题；牛黄解毒片中砷元素在胃肠液和水中的溶出率基本一致，其他19种元素在胃肠液中的溶出率普遍高于水中；虽然牛黄解毒片中砷在胃肠液中的溶出率不高（0.805%-1.926%），但由于总量很高，因而溶出砷的绝对量仍较高；部分牛黄解毒片中汞总量超标，但在胃肠液中的溶出量很小且较为恒定。 结论： 牛黄解毒片中砷的溶出形态有待进一步研究。

Objective： To investigate total contents of 20 trace elements in Niuhuang Jiedu tablets and their extract rates in water and gastrointestinal fluids by inductively coupled plasma mass spectrometry （ICP-MS）. Methods： An ICP-MS method for simultaneous determination of 20 trace elements was established,and the contents of these 20 trace elements in Niuhuang Jiedu tablets and their extract rates in water,artificial gastric fluid and artificial intestinal fluid were determined,compared and analyzed. Results： The method validation indicated that the correlative coefficients （r） for all elements were over 0.9990;the precisions,stabilities and recoveries for all elements in both Niuhuang Jiedu tablets and extracting solutions met the determination requirements;the determined values of NIST tomato leaves （SRM 1573a） were in accordance with those certified.The results of sample analysis showed that insufficient realgar was formulated in some Niuhuang Jiedu tablets;almost the same extract rates for arsenic were found in water and in gastrointestinal fluids,while higher extract rates for other 19 elements were found in gastrointestinal fluids than that in water;the extract rates for arsenic were low （0.805%-1.926%）;however,the amount extracted in gastrointestinal fluids was still large due to the extreme high arsenic contents in Niuhuang Jiedu tablets;the contents of mercury in some Niuhuang Jiedu tablets were also found over regulation defined limit;however,only very few and constant mercury was extracted in gastrointestinal fluids. Conclusion： The dissolved aresenic species of Niuhuang Jiedu tablets should be further researched.