【摘要】 目的 建立三重四极杆-电感耦合等离子体质谱(ICP-MS/MS)测定血、尿液中锰(Mn)、铬(Cr)、镍(Ni)的检测方法。方法 采用0.01%Triton X-100和0.4%硝酸的稀释液，将血和尿液稀释20倍后直接对ICP-MS/MS的碰撞模式和反应模式进行比较分析，选定最优方法。结果 在氨气反应模式下直接检测血液和尿液中的Mn、 Cr、 Ni,锗(Ge)作为内标元素。方法的相关系数(r)>0.999 9, Cr, Mn, Ni 3种元素尿液中的检出限分别为0.097、 0.200、 0.481μg/L;血液中的检出限分别为0.214、 0.340、 0.669μg/L。尿液和血液中的低、高浓度加标回收率为85.14%～102.86%,批内精密度0.31%～4.07%,批间精密度0.44%～4.98%。结论 本方法检出限低，精密度和准确度较好，为快速、准确地批量检测职业接触人群血、尿样本提供了新的技术支持。更多还原

【Abstract】 Objective To establish a method for determination of manganese（Mn）, chromium（Cr）and nickel（Ni）in blood and urine by triple quadrupole-inductively coupled plasma mass spectrometry（ICP-MS/MS）.Methods Blood and urine samples were diluted 20 times with 0.01% Triton X-100 and 0.4%HNO₄, and the collision mode and reaction mode of ICP-MS/MS were directly compared and analyzed to select the optimal method.Results Mn, Cr, and Ni in blood and urine were detected directly under ammonia reaction mode, and germanium（Ge） as the internal standard.The correlation coefficient（r）was >0.999 9.The detection limits of Cr, Mn and Ni in urine were 0.097, 0.200 and 0.481 μg/L, respectively.The detection limits in blood were 0.214, 0.340 and 0.669 μg/L, respectively.The recoveries of low and high concentration spiked in urine and blood were 85.14%—102.86%, the intra-batch precision was 0.31%—4.07%, and the inter-batch precision was 0.44%—4.98%.Conclusion This method has low detection limits, good precision and accuracy, and provides a new technical support for rapid and accurate batch dection of blood and urine samples of occupational exposure population.更多还原