一步酸稀释-电感耦合等离子体质谱法测定全血中17种元素的含量

Determination of 17 Elements in Whole Blood by Inductively Coupled Plasma Mass Spectrometry with One-Step Acid Dilution

鉴于经典方法(原子吸收光谱法)存在过程繁琐、引入污染风险高、样品量大、耗时较长等缺点,进行了题示研究。采用含0.1%(体积分数)硝酸、0.1%(体积分数)曲拉通、1%(体积分数)异丙醇的稀释液一步稀释全血样品(样品量最低为50μL),所得溶液直接进电感耦合等离子体质谱仪分析。以Sc、Rh、In、Tb、Bi作为内标元素,碰撞模式选择氦(He)模式。结果显示:一步酸稀释法过程简单,引入污染风险小,且低、高浓度水平样品不会相互干扰,样品中17种元素可在45s内完成同时检测;各目标元素的质量浓度分别在0.05~30mg·L^(-1)(Ca、Mg、Fe)和0.5~300μg·L^(-1)(Cr、Co、Cd、Cu、Mn、Mo、Ni、Pb、Se、V、Zn、Rb、Sr、Cs)内与对应的质谱响应值比值呈线性关系,检出限(3s)为0.3ng·L^(-1)~0.22μg·L^(-1);对全血痕量元素标准物质L-1、L-2进行准确度试验,测定值均在认定值的95%置信区间内;对质控样品进行日内(n=10)、日间(n=15)精密度试验和方法比对试验,测定值的相对标准偏差均小于15%,且上述方法和经典方法测定值的相对误差的绝对值均不大于11%。

In view of the disadvantages of the classical method(atomic absorption spectrometry),such as cumbersome process,high pollution risk,high sample amount,and time-consuming,the title study was carried out.Dilution solution containing 0.1%(volume fraction)nitric acid,0.1%(volume fraction)triton and 1%(volume fraction)isopropanol was used for diluting the whole blood sample in one step with minimum sample amount of 50μL,and the solution obtained was directly analyzed by inductively coupled plasma mass spectrometer,with Sc,Rh,In,Tb and Bi as internal standard elements,and the He mode as the collision mode.It was shown that the one-step acid dilution method had a simple process,low pollution risk,and samples with low and high concentration levels did not interfere with each other.The 17 elements in the samples could be detected simultaneously within 45 s.Linear relationships between values of the mass concentration of each target element and mass spectrometry response value ratio were kept in the ranges of 0.05-30 mg·L^(-1)(Ca,Mg and Fe)and 0.5-300μg·L^(-1)(Cr,Co,Cd,Cu,Mn,Mo,Ni,Pb,Se,V,Zn,Rb,Sr and Cs),with detection limits(3s)in the range of 0.3 ng·L^(-1)-0.22μg·L^(-1).Test for accuracy was conducted on the whole blood trace element reference materials of L-1 and L-2,and the determined values were within 95%confidence intervals of the identified values.Tests for intra-day precision(n=1o),inter-day precision(n=15)and method comparison were conducted on quality control samples,and RSDs of the determined values were less than 15%,with the absolute values of the relative errors of the determined values using the above method and classical method not more than 11%.