离子色谱-电感耦合等离子体质谱联用法测定碘酸根和碘离子

摘要

目的：采用离子色谱（ IC）与电感耦合等离子体质谱（ ICP-MS）联用技术建立测定碘酸根和碘离子的方法。方法使用 Agilent G3154-65001分析柱和Agilent G3154-65002保护柱，通过改变色谱柱柱温，淋洗液浓度、流速，调谐 ICP-MS工作参数等，确定了碘酸根和碘离子测定的最佳条件，并在此条件下对方法的线性范围、检出限、精密度和回收率进行测试。结果40℃柱温，30mM NH4NO3淋洗液，1.2mL· min -1流速条件下，IO3-与I-检出限分别为0.10μg· L-1和0.93μg· L -1，加标回收率在93.0%~120.0%之间，相对标准偏差RSD均<5.0%。在此条件下对实际尿样进行了测定。结论实验证明该方法灵敏度和选择性高、检测结果可靠、检测快速。%ABSTRACT:OBJECTIVE An analytical method was developed for separation and determination of iodate and io-dine ion using hyphenated technology of ion chromatography ( IC) and inductively coupled plasma mass spectrometry ( ICP-MS).METHODS Agilent G 3154-65001 was used as the separation column and Agilent G 3154-65002 was used as the guard column.The optimum conditions for speciation of iodate and iodine ion were summed up by chan-ging the column temperature,the concentration and flow rate of the eluent.Also ICP-MS parameters were tuned.On the basis of this method, the linear range, detection limit, precision and recovery rate of the method were test-ed.RESULTS The results showed that using 40℃as the column temperature,with 30mM NH4 NO3 and 1.2mL· min-1 as the flow rate of the eluent,the detection limits of IO3-and I -were 0.10μg· L-1 and 0.93μg· L-1 .The recoveries were between 93.0%and 120.0%.RSDs were under 5%.At last,the iodate and iodine ion were deter-mined in the urine.CONCLUSION It was showed that the method had the characteristics of high sensitivity,high selectivity,fast detection,good accuracy and precision.