在线电化学还原为碘化物后反相离子对高效液相色谱-安培检测器超灵敏高选择性测定碘酸盐

Qingwei Jiang, Tao Wang, Gao Li
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引用次数: 0

摘要

我们开发了一种超灵敏和高选择性的方法来定量碘化盐和生物样品中的碘酸盐(IO3 -)。在高效液相色谱(HPLC)系统中,采用库仑检测器(CD)作为柱前反应器,将IO3 -注入进样器,在线还原为碘化物(I -),在离子对的帮助下由C18柱保留,再由安培检测器(AD)测定。在分析IO3 -时,对库仑检测器的应用电位、pH值、盐浓度等参数和反应条件进行了优化,以获得最佳还原效率。优化后的HPLC-CD-AD方法在IO3 -浓度(0.05 ~ 0.25 μg/mL)范围内呈良好的线性关系,在良好的检出限(100 pg)和可接受的变异性下,回收率为86.90 ~ 94.70%。通过对志愿者尿液、碘盐、海水等实际样品中碘的分析,发现该方法选择性高,干扰小。结果表明,该方法具有超灵敏、高选择性的痕量碘检测方法。
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Ultrasensitive and highly selective determination of iodate by reversed-phase ion pair HPLC–amperometric detector after online electrochemical reduction to iodide
We developed an ultrasensitive and highly selective method to quantify iodate (IO3–) in iodized salt and biological samples. In the high-performance liquid chromatography (HPLC) system, IO3– was injected with sampler and reduced to iodide (I–) online using a Coulomb detector (CD) as a pre-column reactor, retained by C18 column with the help of ion pairs, and then determined by an amperometric detector (AD). For analysis of IO3–, several parameters and reactive conditions of Coulomb detector, including applied potential, pH value, and salt concentration, were optimized to obtain the best reduction efficiency. The optimized HPLC–CD-AD method was found to be linear over a wide range of IO3– concentration (0.05–0.25 μg/mL) with appreciable recovery rates (86.90– 94.70%) of quality controls at excellent detection limits (100 pg) and acceptable variability. The analysis of IO3– in actual samples, such as urine of volunteers, iodized salt, and seawater, discovered that the method has high selectivity and little interference. It can be concluded that the proposed method was ultrasensitive and highly selective in the trace detection of IO3.
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