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 0 μg/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 HNO₃-H₂O₂ 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 ⁴⁵Sc,¹¹⁵In and ²⁰⁹Bi,which are added on line.⁵²Cr,⁷⁵As,¹¹⁴Cd and ²⁰⁸Pb 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 0.999 9,0.999 8,0.999 9 and 1.000 0,respectively.Meanwhile,the detection limits are 0.053 0,0.009 0,0.011 0 and 0.014 0 μg·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.

张歌(1991-),男,工程师,从事清洁生产技术研发及应用,gzlove_666@163.com