微波溶解体系电感耦合等离子质谱仪测定人体头发、尿样中铬砷镉铅

Determination of chromium,arsenic,cadmium and lead in human hair and urine by inductively coupled plasma mass spectrometry with microwave dissolution system

用HNO3-H2O2微波溶解体系电感耦合等离子质谱仪(Inductively Coupled Plasma Mass Spectrometry,ICP-MS)建立了一种测定人体样品头发和尿样中Cr、As、Cd、Pb 4种金属元素的方法。采用内标法进行校正,在线方式加入内标元素钪(45Sc)、铟(115In)、铋(209Bi),有效克服了基体效应和信号漂移所产生的影响。选择52Cr、75As、114Cd、208Pb为待测同位素,有效地克服了因质谱干扰带来的影响。对国家标准物质GBW07601、GBW09102进行了测定,测定结果与标准值相吻合。Cr、As、Cd、Pb校准曲线的线性相关系数分别为0.999 9、0.999 8、0.999 9、1.000 0,检出限分别为0.053 0、0.009 0、0.011 0和0.014 0μg/L。该方法应用到实际的样品分析回收率为97%~102%,操作简便快捷,结果准确且灵敏度高,尤其适于大批量人体样品的检测。

Cr,As,Cd and Pb in human hair and urine are digested with microwave in HNO 3-H 2 O 2 system and detected by inductively coupled plasma mass spectrometry(ICP-MS).It is found that signal shift aroused by matrix effect of non-suppression-enhancement can be corrected well by the internal standards,such as 45 Sc,115 In and 209 Bi,which are added on line.52 Cr,75 As,114 Cd and 208 Pb are selected as measured isotope to eliminate non-spectral interference and spectrum interference.China's standard substance(GBW07601 and GBW09102)are detected by ICP-MS with microwave digestion.The result is coincided with the standard value.The correlation coefficients of linear regression equations of Cr,As,Cd and Pb are 0.9999,0.9998,0.9999 and 1.0000,respectively.Meanwhile,the detection limits are 0.0530,0.0090,0.0110 and 0.0140μg·L^-1 for Cr,As,Cd and Pb,respectively.As this method is applied for detecting the actual samples,the standard addition recovery is in the range of 97%-102%.This method is simple,accurate and high sensitivity,and especially suitable for the detection of large quantities of human samples.