摘要
目的 建立测定鲜河蚌肉水提物中铜(Cu)、砷(As)、镉(Cd)、汞(Hg)、铅(Pb)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,等离子体射频功率为 1550 W,等离子体气体流速为 15.0 L/min,辅助气体(氩气)流速为 0.90 L/min,雾化气流速为1.05 L/min,蠕动泵速为0.1r/s,采样深度为 8 mm,调谐模式为No Gas模式,重复 3次.结果 Cu、As、Cd、Hg、Pb质量浓度分别在 0～500 ng/mL、0～200 ng/mL、0～10 ng/mL、0～5 ng/mL、0～20 ng/mL范围内与仪器响应值线性关系良好(r≥0.9996,n=5),检测限分别为 0.0205,0.0045,0.0008,0.0042,0.0051 mg/kg,定量限分别为 0.0682,0.0149,0.0027,0.0141,0.0170 mg/kg;精密度、重复性试验结果的RSD均小于 5%;平均加样回收率分别为 99.60%,106.16%,108.93%,115.30%,103.40%,RSD分别为 0.84%,6.03%,1.15%,3.56%,0.55%(n=6).参考《药用植物及制剂外经贸绿色行业标准》,9 批样品中的Cu、Hg、Pb均符合限量标准,As、Cd超标的样品分别有 8 批、2 批.结论 该方法操作简单,结果准确,可用于测定鲜河蚌肉水提物中Cu、As、Cd、Hg、Pb的含量.
Abstract
Objective To establish an inductively coupled plasma-mass spectrometry(ICP-MS)method for determining the contents of copper(Cu),arsenic(As),cadmium(Cd),mercury(Hg),and lead(Pb)in the water extract of fresh mussel meat.Methods The samples were pretreated by microwave digestion,and the contents of five elements were determined by the ICP-MS method.The plasma radio frequency power was 1550 W,the plasma gas flow rate was 15.0 L/min,the auxiliary gas(argon)flow rate was 0.90 L/min,the atomization gas flow rate was 1.05 L/min,the peristaltic pump speed was 0.1 r/s,the sampling depth was 8 mm,the tuning mode was No Gas mode,the repetition frequency was three times.Results The linear ranges of Cu,As,Cd,Hg,and Pb were in the range of 0-500 ng/mL,0-200 ng/mL,0-10 ng/mL,0-5 ng/mL,and 0-20 ng/mL(r≥0.9996,n=5)respectively.The limits of detection(LOD)were 0.0205,0.0045,0.0008,0.0042,0.0051 mg/kg respectively,the limits of quantification(LOQ)were 0.0682,0.0149,0.0027,0.0141,0.0170 mg/kg respectively.The RSDs of precision and repeatability tests were lower than 5%.The average recovery rates of the above five elements were 99.60%,106.16%,108.93%,115.30%,103.40%with RSDs of 0.84%,6.03%,1.15%,3.56%,0.55%(n=6)respectively.Based on the Green Standards for Medicinal Plants and Preparations for Foreign Trade and Economy,Cu,Hg and Pb in nine batches of samples met the limits,while As and Cd levels were over the limits in eight and two batches of samples respectively.Conclusion This method is simple and accurate,which can be used to determine the contents of Cu,As,Cd,Hg,and Pb in the water extract of fresh mussel meat.
基金项目
上海市科技计划项目(22S21900700)
上海市科技计划项目(22S21900800)
上海中医药大学产业发展中心医养结合科创项目(YYKC-2021-01-145)
国家科技期刊平台
NSTL
万方数据