电感耦合等离子体质谱法测定鲜河蚌肉水提物中5种元素含量  

Determination of Five Elements in Water Extract of Fresh Mussel Meat by ICP-MS

作　　者：刘瑾[1] 章恒周 史万忠[1] 许政 LIU Jin;ZHANG Hengzhou;SHI Wanzhong;XU Zheng(Shuguang Hospital Affiliated to Shanghai University of Traditional Chinese Medicine,Shanghai,China 200021;Shanghai Wanshicheng Pharmaceutical Co.,Ltd.,Shanghai,China 201506)

机构地区：[1]上海中医药大学附属曙光医院,上海200021 [2]上海万仕诚药业有限公司,上海201506

出　　处：《中国药业》2024年第16期92-95,共4页China Pharmaceuticals

基　　金：上海市科技计划项目[22S21900700,22S21900800];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]。

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0.90L/min,雾化气流速为1.05L/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。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.

关 键 词：鲜河蚌肉 重金属元素 有害元素 电感耦合等离子体质谱法 含量测定 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]