离子色谱法检测乳制品中硫氰酸根离子  

Determination of Thiocyanate in Dairy Products by Ion Chromatography

作　　者：王云霞 杜晓华 孙丽华 李翠枝 刘丽君 邵建波 

机构地区：[1]内蒙古伊利实业集团股份有限公司,内蒙古呼和浩特010110

出　　处：《乳业科学与技术》2014年第6期22-25,共4页JOURNAL OF DAIRY SCIENCE AND TECHNOLOGY

基　　金："十二五"国家科技支撑计划项目(2012BAK17B00)

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.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.

关 键 词：离子色谱 硫氰酸根 乳制品 

分 类 号：O657.7[理学—分析化学] TS252.7[理学—化学]