含朱砂中成药中甲基汞和乙基汞含量的HPLC-ICP-MS法检测  

Determination of Methyl Mercury and Ethyl Mercury in Traditional Chinese Medicines Containing Cinnabar by HPLC-ICP-MS

作　　者：刘洪旭 吴文晞[2] 王丹红[2] 邓思珊 马振菁 张韬 

机构地区：[1]福建省医学科学研究院,福建福州350001 [2]福建出入境检验检疫局技术中心,福建福州350001

出　　处：《时珍国医国药》2012年第4期873-874,共2页Lishizhen Medicine and Materia Medica Research

基　　金：福建省自然科学基金(No.2010J01133)

摘　　要：目的建立HPLC-ICP-MS联用技术测定含朱砂中成药中甲基汞和乙基汞含量的方法。方法采用盐酸提取,二氯甲烷萃取,水封吹氮浓缩等处理,利用高效液相色谱分离,最后由ICP-MS检测甲基汞和乙基汞含量。色谱柱为GRACE的Altima HP C18(5μm,150 mm×4.6 mm),流动相为含有5%甲醇,0.06 mol/L乙酸铵,0.1%半胱氨酸的水溶液。结果 19种含朱砂中成药中仅牛黄千金散检出甲基汞。甲基汞和乙基汞的线性范围均为0～50 ng/ml,相关系数大于0.999,检出限分别为0.5,0.4 ng/ml。分析龙虾肝胰脏粉标准样品TORT-2中甲基汞的回收率为84.0%,RSD为8.3%。结论该方法前处理简单高效、线性范围宽、精密度较好、准确性较高,适用于含朱砂中成药中甲基汞的测定。ObjectiveTo establish high performance liquid chromatography and inductively coupled plasma mass spectrometer coupled techniques for determination methyl mercury and ethyl mercury contents in traditional Chinese medicines containing cinnabaranalysis method. MethodsAfter hydrochloric acid extraction,methylene chloride extraction,water treatment,nitrogen comentration and high performance liquid chromatographic separation,the contents of medthyl mercury and ethyl mercury were determined by ICP-MS.GRACE Altima HP C18（5μm,150mm×4.6mm） was adopted and the mobile phase consisted of 5% methanol,0.06 mol/L ammonium acetate and 0.1% homocysteine. ResultsOf 19 species of traditional Chinese medicines containing cinnabar,the content of methyl mercury could be detected in Niuhuang Qianjin Powder.The linear range of methyl mercury and ethyl mercnng was within the range of 0～50 ng/ml,the correlation cefficient was 0.999 and detection limit was 0.5,0.4,respectively.The recovery rate of methyl mercury in TORT-2 was 84% and RSD was 8.3%. ConclusionThis method is simple,precise,accurate and can be used for determination of methyl mercury in Chinese medicines containing cinnabar.

关 键 词：朱砂 甲基汞 乙基汞 液相色谱 电感耦合等离子体质谱 

分 类 号：R284.1[医药卫生—中药学]