【摘要】 目的 建立高效液相色谱-电感耦合等离子体质谱联用技术（HPLC-ICP-MS）测定尿液中4种碘形态的方法。方法 尿样经离心、过滤、稀释后，选用DIONEX^?AS7色谱柱（4×250 mm）,采用NH₄NO₃（含4%甲醇）作为流动相梯度洗脱，对4种碘形态进行分离，电感耦合等离子体质谱测定，外标法定量。结果 在1.00μg/l～50.00μg/L范围内，碘酸钾、一碘酪氨酸、二碘酪氨酸、碘化钾成良好的线性关系，相关系数均>0.999。尿液中4种碘形态化合物平均回收率为94.00%～119.00%,日间精密度及日内精密度相对标准偏差为1.85%～7.83%。碘酸钾、一碘酪氨酸、二碘酪氨酸、碘化钾的检出限分别为0.015μg/L、0.045μg/L、0.035μg/L与0.010μg/L,定量限分别为0.045μg/L、0.135μg/L、0.105μg/L与0.030μg/L。4种碘形态加合值与采用电感耦合等离子体质谱仪测定的尿液中碘的总含量基本一致。结论 利用高效液相色谱串联电感耦合等离子体质谱建立了一种方便、高效、准确的碘形态分析方法，可快速测定尿液中碘酸钾、一碘酪氨酸、二碘酪氨酸、碘化钾的含量。更多还原

【Abstract】 Objective This paper aims to establish a method for the determination of four iodine species in urine by high performance liquid chromatography-inductively coupled plasma-mass spectrometry（HPLC-ICP-MS）. Methods After centrifugation, filtration and dilution, the urine samples were separated on a DIONEX? AS7 column（4×250 mm） with NH₄NO₃（containing 4% methanol） as the mobile phase, and the four iodine species were determined by ICP-MS and quantified with external standard calibration method. Results In the range of 1.00 μg/L-50.00 μg/L, potassium iodate, monoiodotyrosine, diiodotyrosine and potassium iodide showed good linearity with correlation coefficients（r） greater than 0.999. The average recoveries of the four iodine species in urine were within 94.00%-119.00%, and the relative standard deviations（RSDs） of inter-day precision and intra-day precision were within 1.85%-7.83%. The limits of detection（LODs） for potassium iodate, monoiodotyrosine, diiodotyrosine and potassium iodide were 0.015 μg/L, 0.045 μg/L, 0.035 μg/L and 0.010 μg/L, respectively; and the limits of quantification（LOQs） were 0.045 μg/L, 0.135 μg/L, 0.105 μg/L and 0.030 μg/L, respectively. The summed values of the four iodine forms were in good agreement with the total iodine content in urine determined by ICP-MS. Conclusion A convenient, efficient and accurate method for the determination of iodine forms using HPLC-ICP-MS was developed for the rapid analysis of potassium iodate, monoiodotyrosine, diiodotyrosine and potassium iodide in urine.更多还原