色谱

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混合模式色谱柱离子色谱法同时测定奶粉中的碘离子和硫氰酸根

李静, 王雨, 梁立娜*   

  1. 戴安中国有限公司应用研究中心, 北京 100085
  • 收稿日期:2009-08-20 修回日期:2009-10-20 出版日期:2010-04-28 发布日期:1980-12-25
  • 通讯作者: 梁立娜

Simultaneous determination of iodide and thiocyanate in powdered milk using ion chromatography with mixed-mode column

LI Jing, WANG Yu, LIANG Lina*   

  1. Application Research Center, Dionex China Limited, Beijing 100085, China
  • Received:2009-08-20 Revised:2009-10-20 Online:2010-04-28 Published:1980-12-25
  • Contact: LIANG Lina

摘要: 碘离子和硫氰酸根的含量是奶粉质量检测的重要项目,但由于奶粉基体复杂,色谱分析中容易产生干扰。本文使用一种带有疏水性烷基链和弱阴离子交换官能团的混合分离模式色谱柱Acclaim Mixed-Mode WAX-1,成功实现了碘离子、硫氰酸根与样品中干扰峰的基线分离,并用紫外检测器进行了检测。实验中将奶粉样品溶于水后,用乙腈沉淀蛋白,并通过OnGuard RP前处理柱除去对色谱柱有污染的有机物质。所用淋洗液为乙腈-100 mmol/L磷酸盐缓冲液(pH 6)-水(体积比为45:5:50),紫外检测波长为226 nm。该方法对碘离子和硫氰酸根的检出限分别为4.6 μg/L和13.8 μg/L,0.2 mg/L标准溶液峰面积的相对标准偏差分别为1.2%(n=6)和1.7%(n=6)。该分析方法准确可靠,线性范围宽,检出限较低,为乳制品质量检测提供了可行方法。

关键词: 碘离子, 混合模式色谱柱, 离子色谱, 硫氰酸根, 奶粉

Abstract: The contents of iodide and thiocyanate are important detection items in powdered milk quality testing. Due to the complexity of the powdered milk matrix, chromatographic analysis is easily subjected to interference. Acclaim Mixed-Mode WAX-1 column incorporated both hydrophobic and weak anion-exchange properties was used to separate iodide and thiocyanate from interfering substances in powdered milk matrix, and detected by Ultraviolet (UV) detection. After powdered milk was dissolved in water, the protein was precipitated by acetonitrile. Then OnGuard RP pre-treatment column was used to remove the organic matters which might pollute the column. The eluent was acetonitrile-100 mmol/L phosphate buffer (pH 6)-water (45:5:50,v/v/v). The UV detection wavelength was 226 nm. The limits of detection of iodide and thiocyanate were 4.6 μg/L and 13.8 μg/L respectively, and the relative standard deviations of peak areas were 1.2% (n=6) and 1.7%(n=6) for 0.2 mg/L iodide and thiocyanate standard solutions. The method is accurate and reliable, and has wide linear range, low limit of detection. This method provides a viable approach for powdered milk quality dairy products.

Key words: iodide, mixed-mode column, powdered milk , thiocyanate, ion chromatography