基于微波消解的ICP-OES和ICP-MS法测定中药独活中的24种微量元素  

Simultaneous determination of 24 trace elements of Angelicae Pubescentis Radix by ICP-OES and ICP-MS methods based on the microwave digestion

作　　者：杨雁芳[1] 张友波[1] 杨秀伟[1] 

机构地区：[1]北京大学药学院天然药物学系天然药物及仿生药物国家重点实验室,北京100191

出　　处：《药物分析杂志》2016年第11期2004-2008,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金(No.81403068);国家科技支撑计划(2011BAI07B08)

摘　　要：目的:建立同时测定湖北中药材规范化种植基地独活药材中24种微量元素的方法。方法:微波消解法处理样品,采用电感耦合等离子体发射光谱(ICP-OES)法测定Al、Ca、Fe、K、Mg、Mn、Na、P和Zn的含量,射频功率为1 150 kW,冷却气流量为15 L·min^(-1),辅助气流量为0.5 L·min^(-1),载气为0.2 MPa。采用电感耦合等离子体质谱(ICP-MS)法测定Cu、Sr、Ba、B、Cr、Co、Ni、Ge、As、Se、Mo、Cd、Cs、Pb和Hg的含量,雾化气流量为0.96 L·min^(-1),辅助气流量为1.80 L·min^(-1),等离子体气流量为15.0 L·min^(-1)。结果:国家标准物质比对实验证明测定方法准确可靠。独活药材中含量较高的元素:K为19 633~20 178μg·g^(-1),Al、Ca、Fe、Mg和P在1 069~6 586μg·g^(-1)范围,Mn、Na和Zn在30~330μg·g^(-1)范围。重金属元素Pb含量≤1.50μg·g^(-1),Hg含量≤0.007μg·g^(-1),As含量≤0.52μg·g^(-1),Cu含量≤17.76μg·g^(-1),均符合中国药典限量要求;但Cd的含量为1.0μg·g^(-1),超过限量标准。结论:微量元素的含量测定可以为湖北中药材规范化种植基地独活药材质量控制和临床用药安全提供科学依据。Objective： To establish a method for determination of 24 trace elements of Angelicae Pubescentis Radix from the Good Agrieuhural Practice （ GAP ） planting bases of Chinese materia medica in Hubei province. Methods： The samples were treated by microwave digestion. The contents of Al, Ca, Fe, K, Mg, Mn, Na,P and Zn were determined by inductively coupled plasma optical emission spectrometry （ ICP-OES ）, with radiofrequency power of 1 150 kW, the cooling gas flow rate of 15 L. min-1, the auxiliary gas flow rate of 0. 5 L. min-1 and the carrier gas pressure of 0. 2 MPa. The contents of Cu, Sr, Ba, B, Cr, Co, Ni, Ge, As, Se, Mo, Cd, Cs, Pb and Hg were determined by inductively coupled plasma mass spectrometry （ ICP-MS ）, with the nebulizer gas flow rate of 0.96 L. min-1, the auxiliary gas flow rate of 1.80 L. min-1 and the plasma gas flow rate of 15.0 L.min-1. Results： The national standard material comparison experiment demonstrated that the method was accurate and reliable. The elements with high contents in Angelicae Pubescentis Radix were ： K （ 19 633-20 178 μ g. g-1 ） ; Al, Ca, Fe, Mg, and P （ 1 069-6 586 μ g. g-1 ） ; Mn, Na and Zn （ 30-330μ g. g-1 ）. The contents of heavy metal elements were as follows, Pb content ≤ 1.50 μ g. g-1, Hg content ≤0. 007 μg. g-1, As content ≤ 0. 52μ g. g-1, and Cu content ≤ 17.76 μ g. g-1, all met the limited requirements of Pharmacopoeia of the People＇s Republic of China, except for Cd （ 1.0 μg. g-1 ） exceeding the standard. Conclusion： Determination of trace elements can provide a scientific basis for the quality control and clinical safety of Angelicae Pubescentis Radix from the GAP planting bases of Chinese materia medica in Hubei province.

关 键 词：独活 微量元素 重金属元素 微波消解 电感耦合等离子体发射光谱法 电感耦合等离子体质谱法 

分 类 号：R917[医药卫生—药物分析学]