离子色谱法测定蒸馏酒中氰化物含量的方法性能分析

Method Performance Analysis of Determination of Cyanide in Distilled Wines by Ion Chromatography

建立离子色谱法测定蒸馏酒中氰化物的具体测定条件。样品经0.22μm微孔滤膜过滤上机。采用Dionex IonPac^(TM) AS11-HC色谱柱,银电极为工作电极,以0.5mM乙酸钠+0.1mM氢氧化钠+0.5%(v/v)乙二胺为淋洗液进行等度洗脱,流速1.0mL/min,进样量25μL。结果表明,氰化物含量在5-150μg/L浓度范围内,线性关系良好,相关系数(R^2)为0.9996,方法检出限为0.19μg/L,最低检出浓度为0.7μg/L。保留时间相对标准偏差为0.15%,峰面积相对标准偏差为0.85%,相对标准不确定度为0.014。样品加标回收率在99.0-100.1%之间,CN-出峰时间为5.75min左右。

An ion chromatography method was developed for determination of cyanide in distilled wines. The samples were filtrated through a 0.22μm membrane with the injection volume of 25μ L. The free cyanide was separated on a Dionex IonPacTM ASll-HC anion exchange column using isocratic elution with a solution of 0.5mM sodium acetate＋ 0.1mM sodium hydroxide＋0.5%（v/v） ethylenediamine as the mobile phase at a flow rate of 1.0mL/min. The eluates were detected with an Ag working electrode. The results revealed good linear responses of cyanide over the range of 5-1501xg/L with a correlation coefficient（R2） of 0.9996, the limit of detection was 0.19μg/L, and the minimum detection eoneentration was 0.7μg/L. The relative standard deviation of the retention time was 0.15%, the relative standard deviation of the peak area was 0.85%, and the relative standard uncertainty was 0.014. The recoveries of the samples were between 99.0% and 100.1%, and the retention time of CN-was about 5.75min.