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基于整体材料的阳离子交换搅拌棒吸附萃取的制备及其在离子色谱法分析牛奶中可溶性阳离子中的应用。

Preparation of cation-exchange stir bar sorptive extraction based on monolithic material and its application to the analysis of soluble cations in milk by ion chromatography.

机构信息

State Key Laboratory of Marine Environmental Science, Environmental Science Research Center, Xiamen University, P. O. Box 1009, Xiamen, 361005, China.

出版信息

Analyst. 2011 Oct 21;136(20):4289-94. doi: 10.1039/c1an15344g. Epub 2011 Aug 31.

Abstract

In this study, a new cation-exchange coating for stir bar sorptive extraction (SBSE) based on poly (acrylic acid-ethylene dimethacrylate) monolithic material was synthesized. The effect of polymerization conditions such as the ratio of functional monomer to cross-linker and the content of porogenic solvent on the extraction efficiencies were investigated in detail. The monolithic material was characterized by elemental analysis, scanning electron microscopy and infrared spectroscopy. In order to evaluate the usability of the new coating for the extraction of inorganic cations, the analysis of soluble K(+), Mg(2+) and Ca(2+) in milk by ion chromatography with conductivity detection was selected as a paradigm. Several extractive parameters, including pH value in sample matrix, desorption solvent, extraction and desorption time were optimized. Under the optimum conditions, low detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target cations were achieved within the range of 0.12-0.28 and 0.4-0.92 μg L(-1), respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction of inorganic cations. Finally, the proposed method was successfully used to analyse three different trademarks of commercial milk samples with satisfactory recoveries in the range of 71.1% to 102.8%.

摘要

在这项研究中,合成了一种基于聚(丙烯酸-乙二醇二甲基丙烯酸酯)整体材料的新型搅拌棒吸附萃取(SBSE)阳离子交换涂层。详细研究了聚合条件,如功能单体与交联剂的比例和致孔溶剂的含量对萃取效率的影响。通过元素分析、扫描电子显微镜和红外光谱对整体材料进行了表征。为了评估新涂层用于萃取无机阳离子的可用性,选择了离子色谱法结合电导率检测分析牛奶中的可溶性 K(+)、Mg(2+)和 Ca(2+)作为范例。优化了几个萃取参数,包括样品基质中的 pH 值、洗脱溶剂、萃取和洗脱时间。在最佳条件下,该方法对目标阳离子的检测限(S/N = 3)和定量限(S/N = 10)在 0.12-0.28 和 0.4-0.92 μg L(-1)范围内,方法还表现出良好的线性、简单性、实用性和低成本,用于萃取无机阳离子。最后,该方法成功地用于分析三种不同品牌的商业牛奶样品,回收率在 71.1%至 102.8%之间,结果令人满意。

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