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尿样用1%HNO3稀释50倍,并以209Bi为内标元素校准基体效应及信号漂移,用电感耦合等离子体-质谱法直接测定,外标法绘制校准曲线进行定量。分别用ICP-MS和双硫腙分光光度法测定同一批尿样中铅的含量,统计并比较两种方法的测定结果,结果经t检验差异无统计学意义。该方法测定尿样中铅的检出限为0.010mg/L,线性良好,相关系数r为0.9997,相对标准偏差为1.05%—4.88%,加标回收率在94.4%—106.8%之间。该方法简化了样品的前处理过程,灵敏快速,效率高,干扰小,重现性好。应用于大量尿铅生物样品测定,结果令人满意。
Urine samples were diluted 50 times with 1% HNO3 and the matrix effect and signal drift were calibrated with 209Bi as internal standard element. The samples were directly determined by inductively coupled plasma-mass spectrometry and the calibration curve was drawn by external standard method. The contents of lead in the same batch of urine samples were determined by ICP-MS and dithizone spectrophotometry respectively. The results of two methods were statistically compared and compared. There was no significant difference by t-test. The detection limit of lead in urine samples was 0.010mg / L. The correlation coefficient r was 0.9997, the relative standard deviation was 1.05% -4.88%, and the recoveries were in the range of 94.4% -106.8%. The method simplifies the sample pretreatment process, sensitive and fast, high efficiency, small interference, good reproducibility. Applied to a large number of urine lead biological sample determination, the results are satisfactory.