Simultaneous speciation analysis of arsenic and iodine in human urine by high performance liquid chromatography-inductively coupled plasma mass spectrometry

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.