Abstract：
A high-performance liquid chromatography-inductively coupled plasma mass spectrometry-based method was developed for the simultaneous determination of four iodine species (i.e. iodate, 3-iodo-tyrosine, 3,5-diiodo-tyrosine, and iodide) and six arsenic species (i.e. arsenobetaine, arsenite, dimethylarsinic acid, arsenocholine, methylarsonic acid, and arsenate) in human urine. The chromatographic separation was performed on a Dionex IonPac As7 anion exchange column. The mobile phase was initiated with 0.5 mmol/L ammonium carbonate solution, followed by 50 mmol/L ammonium carbonate/100 mmol/L ammonium nitrate solution (with 4% methanol). The limits of quantification of the analytes ranged from 0.045 to 2.26 μg/L. At three spiked levels (10.0, 20.0, 50.0 μg/L), the average recoveries (%) ranged from 87.4 to 113.1%, and the relative standard deviations (RSD, %) ranged from 0.4 to 17.2%. The ratio of the sum of six arsenic species to the total arsenic measured by ICPMS ranged from 77.4 to 121.2%, and the ratio of the sum of the four iodine species to the total iodine ranged from 70.7 to 114.7%, indicating a good agreement between these two methods for both arsenic and iodine.
摘要：
开发了一种基于高效液相色谱-电感耦合等离子体质谱法的方法，用于同时测定四种碘物种（即碘酸盐，3-碘-酪氨酸,3,5-二碘-酪氨酸,和碘化物)和六种砷物种(即砷甜菜碱，亚砷酸盐,二甲基arsinicacid,砷胆碱,甲基arsonic酸，和砷酸盐）在人体尿液中。在DionexIonPacAs7阴离子交换柱上进行色谱分离。用0.5mmol/L碳酸铵溶液引发流动相，然后是50mmol/L碳酸铵/100mmol/L硝酸铵溶液(含4%甲醇)。分析物的定量限范围为0.045至2.26μg/L。在三个加标水平(10.0、20.0、50.0μg/L)下，平均回收率(%)为87.4%至113.1%，和相对标准偏差(RSD，%)范围从0.4%到17.2%。ICPMS测得的六种砷的总和占总砷的比例为77.4％至121.2％，四种碘的总和占总碘的比例为70.7%至114.7%，表明这两种方法对砷和碘都有很好的一致性。
