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基于离子色谱/电导检测的全脂奶粉中硫氰酸盐污染物的测定及前处理方法研究
引用本文:张水锋,林珍珍,陈小珍,张东雷,王立世.基于离子色谱/电导检测的全脂奶粉中硫氰酸盐污染物的测定及前处理方法研究[J].分析测试学报,2012,31(1):85-89.
作者姓名:张水锋  林珍珍  陈小珍  张东雷  王立世
作者单位:1. 浙江省质量技术监督检测研究院,浙江杭州3 10013
2. 浙江省质量技术监督检测研究院,浙江杭州3 10013;浙江工业大学化学工程与材料学院,浙江杭州310014
3. 华南理工大学化学与化工学院,广东广州,510640
基金项目:浙江省质量技术监督局科技计划项目(20100206,20090208);浙江省分析测试研究项目(2009F0033)
摘    要:建立了氢氧根淋洗/离子色谱/电导检测分析全脂奶粉中硫氰酸盐(SCN-)污染物的分析方法,对蛋白沉淀剂、提取条件、提取液净化技术、色谱条件等作了深入研究和优化。通过对淋洗液梯度的优化,将出峰时间控制在17 min内,且不受邻近组分干扰。方法在0.02~100 mg/L范围内具有良好的线性关系,相关系数(r)为0.999 9,方法定量下限(S/N=10)为0.3 μg/g,回收率为99%~102%。方法重现性好,3 d内对2.0 mg/L的标准溶液随机测试7次,其峰面积的相对标准偏差(RSD)为1.6%。

关 键 词:硫氰酸盐  奶粉  离子色谱  电导检测  食品安全

Pretreatment and Determination of Thiocyanate Pollutant in Whole Milk Powder by Ion Chromatography/Conductivity Detection
ZHANG Shui-feng , LIN Zhen-zhen , CHEN Xiao-zhen , ZHANG Dong-lei , WANG Li-shi.Pretreatment and Determination of Thiocyanate Pollutant in Whole Milk Powder by Ion Chromatography/Conductivity Detection[J].Journal of Instrumental Analysis,2012,31(1):85-89.
Authors:ZHANG Shui-feng  LIN Zhen-zhen  CHEN Xiao-zhen  ZHANG Dong-lei  WANG Li-shi
Institution:1.Zhejiang Test Academy of Quality and Technology Supervision,Hangzhou 310013,China;2.College of Chemical Engineering and Material Science,Zhejiang University of Technology,Hangzhou 310014,China;3.College of Chemistry and Chemical Engineering,South China University of Technology,Guangzhou 510640,China)
Abstract:A method was developed for analysis of thiocyanate(SCN-) pollutant in milk powder samples on an IonPac AS19 column using KOH gradient elution-ion chromatography/conductivity detection with a conductivity suppressor.The experimental conditions,including sample preparation,chromatographic conditions,were investigated.Under the optimal conditions,the calibration curve was linear in the range of 0.02-100 mg/L,with correlation coefficient(r) of 0.999 9.The limit of quantitation(LOQ,S/N=10) was 0.3 μg/g.The recoveries were in the range of 99%-102%.The method was reproducible,and the inter-RSD(n=7) for peak areas was 1.6% in the random detection of 2.0 mg/L standard solution in 3 d.
Keywords:thiocyanate  milk powder  ion chromatography  conductivity detection  food safety
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