微波消解-电感耦合等离子体质谱法测定脉络宁注射液中25种矿物质元素  

Determination of 25 kinds of minerals in Mailuoning Injection by inductively coupled plasma mass spectrometry with microwave digestion

作　　者：汤卫国 王奇志[2] 印敏[2] 王鸣[2] 陈雨[2] 张建华[2] 冯煦[2] 

机构地区：[1]金陵药业股份有限公司,江苏南京210009 [2]江苏省中国科学院植物研究所/江苏省药用植物研究开发中心,江苏南京210014

出　　处：《中草药》2014年第15期2172-2177,共6页Chinese Traditional and Herbal Drugs

基　　金：江苏省产学研联合创新资金--前瞻性联合研究项目(BY2012210);江苏省科技成果转化专项资金项目(BA2011001)

摘　　要：目的建立微波消解-电感耦合等离子体质谱（ICP-MS）直接稀释测定脉络宁注射液中25种矿物质元素（Mg、Ca、Fe、Cu、Zn、Mn、Al、B、Ba、Co、Cr、K、Li、Mo、Na、Ni、P、Pb、Sr、Th、Ti、V、As、Cd和Hg）的方法。方法分别对微波消解条件和测试条件进行考察;样品经微波消解后,采用电感耦合质谱仪测定25种矿物质元素,并对测定方法学进行考察。结果确定最佳消解条件为3步缓慢升温：400 W 80℃升温10 min,保留5 min;600 W 120℃升温10 min,保留5 min;900 W 200℃升温20 min,保留20 min;25种矿物质元素在各自的线性范围内线性关系良好,r≥0.999 6,精密度、稳定性和重复性试验的RSD均符合定量分析要求;加标回收率为94.7%~106.1%,RSD在0.34%~2.79%。脉络宁注射液中检测出Mg、Ca、Fe、Cu、Zn、Mn、Al、B、Ba、Co、Cr、K、Li、Mo、Na、Ni、P、Pb、Sr、Th、Ti、V,未检出As、Cd和Hg。结论该方法简便、迅速、准确,适用于脉络宁注射液中25种矿物质元素的同时测定。Objective To establish an inductively coupled plasma mass spectrometry（ICP-MS） with microwave digestion method for the determination of the amounts of trace elements（Mg, Ca, Fe, Cu, Zn, Mn, Al, B, Ba, Co, Cr, K, Li, Mo, Na, Ni, P, Pb, Sr, Th, Ti, V, As, Cd, and Hg） in Mailuoning Injection. Methods The conditions of microwave digestion and test were studied respectively. After the microwave digestion, 25 kinds of minerals in the samples were determined by ICP-MS, and the methodology was investigated. Results The optimal digestion conditions were 3-step slowly heating： 400 W 80 ℃ to heat up for 10 min and keep 5 min; 600 W 120 ℃ to heat up for 10 min and keep 5 min; 900 W 200 ℃ to heat up for 20 min and keep 20 min. The determination results of 25 kinds of mineral elements all have a good linear relationship, r ≥ 0.999 6. The RSD values of the precision, stability, and repeatability all met the demands of quantitative analysis. The recovery was 94.7%—106.1% and RSD was 0.34%—2.79%. Mg, Ca, Fe, Cu, Zn, Mn, Al, B, Ba, Co, Cr, K, Li, Mo, Na, Ni, P, Pb, Sr, Th, Ti, and V were detected in Mailuoning Injection, and there was no detection of As, Cd, and Hg. Conclusion This method is simple, sensitive, and precise, and could satisfy the simultaneous determination of minerals in Mailuoning Injection.

关 键 词：脉络宁注射液 电感耦合等离子体质谱(ICP-MS)法 微波消解 矿物质 Mg Ca Fe Cu Zn Mn Al B 

分 类 号：R286.014[医药卫生—中药学]