摘要
目的建立测定生脉注射液中硼、镉、铜、镍、钯、铬、锰、砷、铝、铅、硒、钼、锡、锑14种元素含量的电感耦合等离子体-质谱(ICP-MS)法。方法生脉注射液经微波消解后采用ICP-MS法测定,射频(RF)入射功率为1. 55 kW,采样深度为5 mm,冷却气、辅助气和载气流量分别为14. 0,0. 8,0. 9 L/min(积分时间为0. 5～2 s)。通过在线加入锗、铟、铋内标溶液的方法来校正基体效应和干扰。结果各元素在各自的检测质量浓度范围内线性关系良好(r≥0. 999 0),检出限为0. 02～0. 40 ng/m L,加样回收率为86. 9%～109. 2%,RSD为0. 6%～4. 1%(n=6)。参照2015年版《中国药典(四部)》,各批样品中重金属及有害元素铅、镉、砷、铜的含量均在规定范围内。结论该方法简便、灵敏、准确,可用于生脉注射液中多种元素的检测,为其风险监控提供技术参数。
ObjectiveTo establish an ICP-MS method for content determination of boron, cadmium, copper,nickel, palladium,chromium, manganese,arsenic, aluminium,lead,selenium,molybdenum,tin and antimony in Shengmai Injection.Methods The Shengmai Injection was determined by ICP-MS method after microwave digestion.The radio frequency(RF)incident power was 1.55 kW,the sampling depth was 5 mm,the flow rates of cooling gas,auxiliary gas and carrier gas were 14.0,0.8,0.9 L/min(the integral time was 0.5-2 s).The matrix effect and interference were corrected by the method of internal standard germanium,indium and bismuth.ResultsThe elements showed good linear relationship in a certain concentration ranges(r≥0.999 0),respectively,the detection limits were 0.02-0.40 ng/m L,the average recovery rate was 86.9%-109.2%,and RSD was 0.6%-4.1%(n=6).According to Chinese Pharmacopoeia(2015 edition,volumeⅣ),the contents of heavy metals and harmful elements of lead,cadmium,arsenic and copper in the samples were basically within the qualified range.Conclusion The method is simple,sensitive and accurate.It can be used for the determination of various elements in Shengmai Injection,and provide technical parameters for its risk monitoring.
作者
黄小琴
钱保勇
Huang Xiaoqin;Qian Baoyong(Taizhou Institute for Food andDrug Control,Taizhou,Jiangsu,China 225300)
出处
《中国药业》
CAS
2018年第24期19-21,共3页
China Pharmaceuticals
