离子色谱法检测乳制品中硫氰酸根离子.pdf

※分析检测 Journal of Dairy Science and Technology 2014, Vol.37 No.6 22 离子色谱法检测乳制品中硫氰酸根离子 * 王云霞，杜晓华，孙丽华，李翠枝 ，刘丽君，邵建波 （内蒙古伊利实业集团股份有限公司，内蒙古呼和浩特 010110 ） 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-C SPE柱提纯去除干扰的 18 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 R2可达到0.99 以上，检测范围为0.1～20 mg/kg （mg/L ），回 酸根离子定量检出限为2.0 mg/kg，标准曲线线性相关系数 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 Determination of Thiocyanate in Dairy Products by Ion Chromatography * WANG Yun-xia, DU Xiao-hua, SUN Li-hua, LI Cui-zhi , LIU Li-jun, SHAO Jian-bo (Inner Mongolia Yili Industrial Group Co. Ltd., Hohhot 010110, China) 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