电感耦合等离子体质谱法测定五味治肝片中的12种元素含量

Determination of Twelve Elements in Wuwei Zhigan Tablet by ICP-MS

目的:测定中成药中有害元素的含量,为中成药质量安全控制提供依据。方法:采用电感耦合等离子体质谱(ICP-MS)法。射频功率1350W,采样深度8.5mm,等离子气流速15L·min-1,辅助气(高纯氩气)流速1.0L·min-1,载气(高纯氩气)流速1.14L·min-1,雾化室冷却温度1℃,雾化器为Babington,样品提升速度为0.40L·min-1。检测五味治肝片中镉、砷、铬、铜、锡、铅、锑、镍、银、锰、钡、锌元素的含量。结果:镉、砷、铬、铜、铅、锑、镍、银、锰、钡、锌检测浓度线性范围均为0.500～20.00ng·mL-1(r=0.9993～1.000),锡为0.500～10.00ng·mL-1(r=0.9998);各元素的加样回收率为95.0%～105.0%,RSD为0.3%～8.0%;样品中检出除锑、银外的所有元素,其中镉、砷、铬、铜、铅的含量均在2010年版《中国药典》规定的中药材限量范围内。结论:五味治肝片中部分元素的含量均能达到要求,但多数元素含量无相应的限量标准,锡、银、锑、镍等有害元素暂无国家限量标准,制定我国中药及其制剂中元素限量的标准具有重要意义。

OBJECTIVE： To determine the content of harmful elements in Chinese patent medicine, and to provide reference for quality control of Chinese patent medicine. METHODS： ICP-MS method was adopted and the instrument＇ s parameters were： RF power： 1 350 W, sampling depth： 8.5 mm, flow rate of plasma gas： 15 L.min-1, flow rate of assistance gas （high purity argon）： 1.0 L.min -1, flow rate of carrier gas （high purity argon）： 1.14 L.min-1, S/C temperature： 1 ℃, atomizers： Babington, sample lifting rate ： 0.40 L.min-1. The contents of cadmium, arsenic, chromium, copper, stannum, lead, stibonium, nickel, silver, manganese, barium and zinc in Wuwei zhigan tablet were determined. RESULTS： The linear ranges of cadmium, arsenic, chromium, copper, lead, stibonium, nickel, silver, manganese, barium and zinc were 0.500--20.00 ng. mL-1（r=0.999 3- 1.000） and that of stannum was 0.500--10.00 ng. mL-1（r=0.999 8）. The recoveries of every element concentration spiked sample were between 95.0% and 105.0% （RSD=0.3%--8.0% ）. All the elements mentioned above were determined in Wuwei zhigan tab- let except for stibonium and sliver and the contents of cadmium, arsenic, chromium, copper and lead in line with the standards stated in Chinese Pharmacopeia （2010 edition）. CONCLUSION： The contents of some elements in Wuwei zhigan tablet are up to the requirements while most of them have no limit standards, such as stannum, silver, stiboniurn and nickel. It is important to formulate the standards of element limit of TCM and their preparation.