直接稀释ICP-MS法快速测定尿液中14种元素的方法建立

Establishment of a method for rapid determination of 14 elements in urine by direct dilution ICP-MS

目的建立直接稀释-电感耦合等离子体质谱法(ICP-MS)快速测定尿液中14种元素的方法。方法利用1%硝酸作为稀释剂,直接10倍稀释待测样品后,配制混合标准溶液,利用ICP-MS仪器完成尿液中14种元素[铍(Be)、钒(V)、铬(Cr)、锰(Mn)、钴(Co)、镍(Ni)、铜(Cu)、砷(As)、镉(Cd)、锡(Sn)、锑(Sb)、钡(Ba)、铊(Tl)、铅(Pb)]的同时测定。通过选取合适的内标溶液,采用氦气碰撞模式(KED),以消除基体中多原子干扰。对方法的线性范围、检出限、精密度和准确度以及稳定性进行评价,并应用在实际尿液样品测定中。结果本方法测定尿液中14种元素的含量,线性范围为0.0~20.0μg/L,相关系数均>0.999,检出浓度为0.01~0.22μg/L,样品加标回收率为89.3%~104.1%,相对标准偏差为0.2%~6.2%。结论本研究建立的ICP-MS测定尿液中多元素的方法操作简便快捷,灵敏度、准确度、精密度较好,能够较好地应用于日常大批量筛查尿液样品中14种元素的测定。

Objective To establish a rapid method for the determination of 14 elements in urine by inductively coupled plasma mass spectrometry(ICP-MS).Methods Using 1%nitric acid solution as diluent,the 14 elements[Be,V,Cr,Mn,Co,Ni,Cu,As,Cd,Sn,Sb,Ba,Tl,Pb]were determined simultaneously with mixed standard solution prepared by diluting the sample 10 times.This method adopted helium collision mode(KED)by selecting a suitable internal standard solution,which eliminated the multiatomic interference in the matrix.The linear range,detection limits,precision and accuracy,and stability of the method were evaluated,then this method was applied to the determination of actual urine samples.Results The linear range of 14 elements in urine were 0.0-20.0μg/L,the correlation coefficient were>0.999,the detection concentration were 0.01-0.22μg/L,the recoveries rate were 89.3-104.1%,the relative standard deviations were 0.2-6.2%.Conclusion The ICP-MS method which was established in this study for the determination of multiple elements in urine is simple and rapid,and it has the advantages of good sensitivity,accuracy and precision.It can be applied to the determination of urine samples in daily mass screening with the high practical value.