Abstract: This report describes an ion chromatography method for determining thiocyanate in dairy products. Milk samples were deproteinized by adding acetonitrile followed by centrifugation, microporous filtration and chromatography on LC-C18 SPE column. The analyte was monitored by ion chromatography. The optimized mobile phase consisted of 1.7 mmol/L sodium bicarbonate, 1.8 mmol/L sodium carbonate and 10% aqueous acetone solution. The suppressor was activated and regenerated with 0.2% sulfuric acid as an inhibitor. The detection limit for thiocyanate was 2.0 mg/kg, and the standard curve exhibited a correlation coefficient above 0.99 in the linear range of 0.1–20 mg/kg (mg/L). Recovery rates for spiked samples ranged from 93% to 97%, and repeatability expressed as relative standard deviation varied between 0.8% and 1.34% (n = 5). The detection accuracy for milk powder standard was 98%. The presented method was characteristic of easy operation, accurate and repeatable results and low detection limit, and was useful for the determination of thiocyanate in dairy products.

Key words: ion chromatography; thiocyanate; dairy products

摘要： 通过采用乙腈沉淀乳粉和牛乳中的蛋白质后,移取上清液经过微孔滤膜过滤、LC-C18 SPE柱提纯去除干扰的有机物质后,滤液经离子色谱检测仪检测分析,从而得到样品中硫氰酸根离子含量.淋洗液经过优化后选用1.7 mmol/L碳酸氢钠+ 1.8 mmol/L碳酸钠+10％丙酮水溶液进行洗脱,抑制剂使用0.2％硫酸进行抑制器活化再生.该方法的硫氰酸根离子定量检出限为2.0 mg/kg,标准曲线线性相关系数R2可达到0.99以上,检测范围为0.1～20 mg/kg (mg/L),回收率在93％～97％之间,重复性实验得出相对标准偏差在0.8％～1.34％.对标准乳粉进行准确度检测,准确度可达到98％.该方法操作简便、结果准确,重复性良好,检测限低,适用于乳制品中硫氰酸根离子的检测.

关键词: 离子色谱；硫氰酸根；乳制品