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

[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Ion Pac NG1预柱在线净化,再经Ion Pac AS16阴离子柱分离,用KOH洗脱,流速为1.0mL/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0.999 8,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。

[ 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 Ixm 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 1.0mL/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 coeffcient was 0.999 8, the limit of detection （LOD） was 0.04mg/L, and the limit of quantification （LOQ） was 0.10mg/L. The recovery rates were in the range of 96.6%-105.1% at three spiked concentrations of 0.5, 5.0, and 20mg/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.