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机构地区:[1]广西中医药大学药学院,南宁530299 [2]玉林食品药品检验所,广西玉林537000
出 处:《中国药房》2015年第24期3406-3409,共4页China Pharmacy
基 金:广西科学研究与技术开发计划项目(No.桂科攻10124008-15)
摘 要:目的:建立同时测定感冒清热颗粒中镁(Mg)、钙(Ca)、铬(Cr)、锰(Mn)、铁(Fe)、镍(Ni)、铜(Cu)、锌(Zn)、砷(As)、硒(Se)、镉(Cd)、锑(Sb)、钡(Ba)和铅(Pb)14种常见金属元素含量的方法。方法:采用微波消解-电感耦合等离子体质谱(ICP-MS)法。样品用浓硝酸-双氧水(2∶1,V/V)微波消解后采用ICP-MS法测定14种金属元素的含量,以锂(Li)、钪(Sc)、锗(Ge)、钇(Y)、铟(In)、铋(Bi)、铽(Tb)混合溶液作为内标,以灌木枝叶作为标准物质。结果:该方法对14种金属元素的标准曲线相关系数r〉0.999 6,检出限在0.002~0.035μg/L之间,加样回收率在80.57%~104.2%之间,RSD在0.34%~2.71%之间。结论:该方法专属性强、快速灵敏,适用于感冒清热颗粒中14种常见金属元素含量的测定。6个批次样品中的重金属的总量都符合《药用植物及制剂进出口绿色行业标准》的要求。OBJECTIVE: To establish a method for simultaneous determination of the content of 14 common metal elements (Mg, Ca, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Cd, Sb, Ba and Pb) in Ganmao qingre granules. METHODS: Microwave digestion-inductively coupled plasma mass spectrometry (ICP-MS) method was conducted. The samples were digested with concentrated nitric acid-hydrogen peroxide(2 : 1, V/V), and then ICP-MS was used to determine the mass concentration of 14 metal elements. Li, Sc, Ge, Y, In, Bi and Tb were used as internal standards, and branches and leaves of bush were used as standard substances. RESULTS: The correlation coefficient of the standard curves of 14 elements was larger than 0.999 6, detection limits were in the range of 0.002-0.035 ktg/L, recoveries were in the range of 80.57%-104.2% and RSDs were in the range of 0.34%-2.71%. CONCLUSIONS: The method is specific, accurate and sensitive, and suitable for the content determination of 14 common metal elements in Ganmao qingre granules. The total mass concentrations of 6 batches of heavy metals are all meet the requirements of Green Trade Standards of lmporting & Exporting Medicinal Plants & Preparations.
关 键 词:微波消解 电感耦合等离子体质谱 感冒清热颗粒 金属元素
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