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

Determination of Iodate and Iodine Ion by Ion Chromatography with Inductively Coupled Plasma Mass Spectrometry

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 NH_4NO_3淋洗液,1.2m L·min^(-1)流速条件下,IO-3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。

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 3154455001 was used as the separation column and Agilent G 3154455002 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 NHaNO3 and 1.2mL @min-1 mln 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.