摘要
目的 建立测定保儿宁颗粒中铅(Pb)、镉(Cd)、汞(Hg)、砷(As)、铜(Cu)5种有害元素含量的电感耦合等离子体质谱法.方法 采用微波消解法对样品进行前处理,通过在线加入内标锗(Ge)、铟(In)、铋(Bi)元素校正基体效应和干扰.采用跳峰采集模式,等离子气流量为15.0L/min,蠕动泵转速为0.10r/s,雾化室温度为2℃,氦气流量为5 mL/min,辅助气流量为1.2L/min,载气流量为 0.8 L/min,射频功率为 1 550 W.结果 Pb,Cd,Hg,As,Cu 的质量浓度分别在 1.987～99.35 ng/mL、0.100～5.00 ng/mL、1.032～5.00 ng/mL、0.100～51.60 ng/mL、10.075～503.75 ng/mL范围内与待测元素和内标响应值的比值线性关系良好(r≥0.999 7,n=6);精密度和重复性试验结果的RSD均小于10％(n=6);平均加样回收率分别为94.65％,105.52％,100.88％,109.35％,96.87％,RSD分别为5.17％,2.68％,6.87％,2.06％,1.34％(n=9).20批样品中5种有害元素的含量均低于规定限度,总含量为0.059 8～0.879 8 mg/kg.结论 所建立的方法操作简便、结果准确、灵敏度高,可用于保儿宁颗粒中5种有害元素的含量测定.
Abstract
Objective To establish an inductively coupled plasma-mass spectrometry(ICP-MS)method for the content determination of five harmful elements[lead(Pb),cadmium(Cd),mercury(Hg),arsenic(As),and copper(Cu)]in Bao'erning Granules.Methods Microwave digestion was used for sample pretreatment,and the matrix effect and interference were corrected by adding internal standards of germanium(Ge),indium(In),and bismuth(Bi)elements online.Peak jumping acquisition mode was adopted,the plasma gas flow rate was 15.0 L/min,the peristaltic pump speed was 0.10 r/s,the atomization chamber temperature was 2 ℃,the flow rate of helium gas was 5 mL/min,the flow rate of auxiliary gas was 1.2 L/min,the flow rate of carrier gas was 0.8 L/min,and the RF power was 1 550 W.Results The linear ranges of Pb,Cd,Hg,As,and Cu were 1.987-99.35 ng/mL,0.100-5.00 ng/mL,1.032-5.00 ng/mL,0.100-51.60 ng/mL,10.075-503.75 ng/mL(r ≥ 0.999 7,n=6),respectively.The RSDs of precision and repeatability test results were all lower than 10％(n=6).The average recoveries of Pb,Cd,Hg,As,and Cu were 94.65％,105.52％,100.88％,109.35％,and 96.87％,with RSDs of 5.17％,2.68％,6.87％,2.06％,and 1.34％(n=9),respectively.The content of five harmful elements in twenty batches of samples was lower than the specified limit,with a total content of 0.059 8-0.879 8 mg/kg.Conclusion The established method is easy,accurate,reliable,and highly sensitive,which can be used for the content determination of five harmful elements in Bao'erning Granules.
基金项目
江苏省市场监督管理局科技计划项目(KJ2022033)
维普
万方数据