摘要
目的建立同时测定杨梅根药材中铅(Pb)、镉(Cd)、砷(As)、汞(Hg)、铜(Cu)5种重金属及有害元素含量的电感耦合等离子体质谱(ICP-MS)法。方法采用微波消解法对样品进行前处理。采用ICP-MS法测定重金属及有害元素含量,等离子体射频功率为1600 W,气体流量为18.0 L/min,辅助气体流量为1.2 L/min,雾化气流速为0.86 L/min,采样深度为0.5 mm,样品提升转速为24 r/min,液氩压力为0.65 MPa,脉冲电压为1850 V,样品冲洗时间为30 s,延迟10 s,调谐模式为KED碰撞模式,数据采集模式为全定量方法。结果Pb,Cd,As,Hg,Cu的质量浓度分别在2.0~100.0 ng/mL、0.2~10.0 ng/mL、1.0~50.0 ng/mL、0.1~5.0 ng/mL、5.0~250.0 ng/mL范围内与待测元素/内标元素响应信号值线性关系良好(r≥0.9998,n=6);精密度、重复性、稳定性试验结果的RSD均低于6%;平均加样回收率分别为99.30%,109.58%,101.35%,93.83%,97.61%,RSD分别为2.70%,1.62%,4.99%,4.79%,2.92%(n=6)。16批药材中,Pb,Cd,As,Hg,Cu的含量分别为0.49~5.26 mg/kg、0.06~1.17 mg/kg、0.04~0.11 mg/kg、0.01~0.02 mg/kg、1.26~4.47 mg/kg,其中1批药材Pb超标,1批药材Cd超标。结论该方法操作简单、结果准确,可用于同时测定杨梅根药材中5种重金属及有害元素的含量。
Objective To establish an inductively coupled plasma-mass spectrometry(ICP-MS)method for the simultaneous determination of five heavy metals and harmful elements[lead(Pb),cadmium(Cd),arsenic(As),mercury(Hg)and copper(Cu)]in Myricae Radix.Methods The sample was pre-treated by the microwave digestion method.The ICP-MS method was used to determine the content of heavy metals and harmful elements.The plasma RF power was 1600 W,the gas flow rate was 18.0 L/min,the auxiliary gas flow rate was 1.2 L/min,the atomized gas flow rate was 0.86 L/min,the sampling depth was 0.5 mm,the sample lifting speed was 24 r/min,the liquid argon pressure was 0.65 MPa,the pulse voltage was 1850 V,the sample washing time was 30 s,and the delay time was 10 s.The tuning mode was kinetic energy discrimination(KED)mode,and the data collection mode was the fully quantitative method.Results The mass concentrations of Pb,Cd,As,Hg,and Cu in the ranges of 2.0-100.0 ng/mL,0.2-10.0 ng/mL,1.0-50.0 ng/mL,0.1-5.0 ng/mL,5.0-250.0 ng/mL showed a good linear relationship with the response signal values of the tested element/internal standard element(r≥0.9998,n=6).The RSDs of precision,repeatability,and stability test results were lower than 6%.The average recoveries of Pb,Cd,As,Hg,and Cu were 99.30%,109.58%,101.35%,93.83%,and 97.61%with RSDs of 2.70%,1.62%,4.99%,4.79%,and 2.92%(n=6),respectively.The contents of Pb,Cd,As,Hg,and Cu in 16 batches of Myricae Radix were in the ranges of 0.49-5.26 mg/kg,0.06-1.17 mg/kg,0.04-0.11 mg/kg,0.01-0.02 mg/kg,1.26-4.47 mg/kg,with Pb exceeding the standard in one batch of Myricae Radix and Cd exceeding the standard in one batch of Myricae Radix.Conclusion This method is simple and accurate,which can be used for the simultaneous determination of five heavy metals and harmful elements in Myricae Radix.
作者
耿冶飞
王永杰
刘会艳
赵丛
GENG Yefei;WANG Yongjie;LIU Huiyan;ZHAO Cong(Hebi Food and Drug Inspection and Testing Center,Hebi,Henan,China 458030)
出处
《中国药业》
CAS
2023年第11期71-74,共4页
China Pharmaceuticals
基金
河南省药品监督管理局中药材标准及中药饮片炮制规范制修订任务[2020DB003]。
