郭爱华, 袁佗, 王玮. 离子色谱法快速测定人尿中的硫氰酸盐[J]. 环境与职业医学, 2015, 32(6): 593-596. DOI: 10.13213/j.cnki.jeom.2015.14602
引用本文: 郭爱华, 袁佗, 王玮. 离子色谱法快速测定人尿中的硫氰酸盐[J]. 环境与职业医学, 2015, 32(6): 593-596. DOI: 10.13213/j.cnki.jeom.2015.14602
GUO Ai-hua , YUAN Tuo , WANG Wei . Rapid Determination of Thiocyanate in Human Urine by Ion Chromatography[J]. Journal of Environmental and Occupational Medicine, 2015, 32(6): 593-596. DOI: 10.13213/j.cnki.jeom.2015.14602
Citation: GUO Ai-hua , YUAN Tuo , WANG Wei . Rapid Determination of Thiocyanate in Human Urine by Ion Chromatography[J]. Journal of Environmental and Occupational Medicine, 2015, 32(6): 593-596. DOI: 10.13213/j.cnki.jeom.2015.14602

离子色谱法快速测定人尿中的硫氰酸盐

Rapid Determination of Thiocyanate in Human Urine by Ion Chromatography

  • 摘要: 目的 建立离子色谱法测定人尿中硫氰酸盐的快速检测方法。

    方法 超纯水稀释尿样,离心后过0.22μm滤膜,经IonPac NG1预柱在线净化,再经IonPac AS16阴离子柱分离,用KOH洗脱,流速为1.0 mL/min,电导检测器检测,外标法定量。并对实验条件进行了优化,考察了方法的检出限、稳定性、准确度及精密度等参数。

    结果 硫氰酸盐的质量浓度在0.10~25.0 mg/L的范围内与其峰面积呈线性关系,相关系数为0.9998,方法检出限(LOD)为0.04 mg/L,定量限(LOQ)为0.10 mg/L。在0.5、5.0、20 mg/L 3个浓度水平进行加标回收试验,回收率为96.6%~105.1%,相对标准偏差(n=6)为1.3%~2.6%。

    结论 该方法简单、快速、准确,适合于人尿中硫氰酸盐含量的测定。

     

    Abstract: Objective To establish a method for rapid determination of thiocyanate in urine by ion chromatography.

    Methods The urine samples were diluted by water, then centrifugated and filtered through 0.22 μm membrane, following by online purification with IonPac NG1 pre column. The purified samples were separated through an IonPac AS16 anion column and eluted by KOH with a flow rate at 1.0 mL/min. Thiocyanate was detected by conductivity detector, and quantification was determined by external standard method. The experimental conditions were optimized, and the parameters of the proposed method including detection limit, stability, accuracy, and precision were calculated.

    Results A linear relationship was found between the values of peak area and the mass concentrations of thiocyanate in the range of 0.10-25.0 mg/L. The correlation coefficient was 0.999 8, the limit of detection (LOD) was 0.04 mg/L, and the limit of quantification (LOQ) was 0.10 mg/L. The recovery rates were in the range of 96.6%-105.1% at three spiked concentrations of 0.5, 5.0, and 20 mg/L, with relative standard deviations (n=6) ranging from 1.3% to 2.6%.

    Conclusion This simple, rapid, and accurate method is suitable for determination of thiocyanate in human urine.

     

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