离子色谱法检测乳制品中硫氰酸根离子

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.

DeterminAtion of ThiocyAnAte in DAiry Products by Ion ChromAtogrAphy

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 liiaear range of 0.1-20 mg/kg （rag/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.