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    室温离子液体负载环糊精磁性纳米材料固相萃取分离与富集饮料中双酚A及其含量的高效液相色谱法测定

    HPLC Determination of Bisphenol A in Beverages with Its Separation and Enrichment by Solid Phase Extraction Using Room Temperature-Ionic Liquid Loaded Magnetic Nano-composite of Cyclodextrin Polymer/Fe3O4

    • 摘要: 先由羟丙基-β环糊精与环氧氯丙烷在碱性溶液中反应制得羟丙基-β-环糊精聚合物,再由所制得的羟丙基-β-环糊精聚合物与氯乙酸钠反应制得羧甲基-羟丙基-β-环糊精聚合物,并将此聚合物与硫酸亚铁及三氯化铁共溶于水中,并在90℃的氨性介质中反应得到Fe3O4/羟丙基-β-环糊精聚合物纳米材料。最后将上述纳米材料在C4minPF6中搅拌浸泡,并经抽滤和在90℃下干燥获得室温离子液体负载环糊精磁性纳米材料(简称磁性纳米材料)。应用此磁性纳米材料作为吸附剂分离、富集饮料中可能存在的双酚A,具体步骤如下:取样品50.0 mL,调节其酸度至pH 7.0,加入磁性纳米材料0.1 g,振荡提取5.0 min,弃去上层溶液,用甲醇2.0 mL将双酚A从磁性纳米材料上超声洗脱10.0 min,收集洗脱液经0.22 μm滤膜过滤,所得滤液供高效液相色谱法分析。以Agilent EC-C18色谱柱为固定相,以不同比例的乙腈(A)和水(B)的混合液作为流动相进行梯度洗脱,采用荧光检测器检测。测得双酚A的线性范围在2.40~800 μg·L-1之间,检出限(3S/N)为0.40 μg·L-1,富集倍数为25。以空白果汁样品为基体,用标准加入法进行回收试验,测得回收率在95.0%~98.0%之间,测定值的相对标准偏差(n=5)在2.3%~5.1%之间。

       

      Abstract: At first, through reaction of hydroxypropyl-β-cyclodextrin with oxacyclochloropropane in alkaline medium hydroxypropyl-β-cyclodextrin polymer was prepared. The polymer obtained was then reacted with sodium chloroacetate to give polymer of carboxymethyl-hydroxypropyl-β-cyclodextrin, which was dissolved together with ferrous sulfate and ferric chloride in water and reacted in ammoniacal solution at 90℃ to give magnetic nanocomposite of hydroxypropyl-β-cyclodextrin polymer/Fe3O4. And finally, the nanocomposite was soaked and stirred inC4minPF6, and after filtration by suction and the solid substance was dried at 90℃, and the room temperature-ionic liquid loaded magnetic nanocomposite of cyclodextrin polymer and Fe3O4 (abbreviated as mangetic nanocomposite, MNC, here after) was obtained. The MNC obtained was used as adsorbent to separate and enrich bisphenol A from samples of beverage by the following optimized procedure:50.0 mL of the sample were taken and after adjusting its acidity to pH 7.0, 0.1 g of the MNC was added and swirled for 5.0 min to have the bisphenol A adsorbed on MNC. The aqueous solution was separated and discarded. 2.0 mL of methanol were added to elute bisphenol A from MNC ultrasonically for 10.0 min. The methanol solution was collected and filtered through 0.22 μm membrane. The filtrate was used for HPLC analysis. Agilent EC-C18 chromatographic column was used as stationary phase and mixtures of acetonitrile (A) and water (B), mixed in various ratios were used as mobile phase in the gradient elution. Fluorescence detector was used for detection. Linearity range for bisphenol A was found between 2.40-800 μg·L-1, with detection limit (3S/N) of 0.40 μg·L-1. Enrichment factor found was 25. Test for recovery was made by standard addition method using blank sample of fruit juice as matrix, giving results in the range of 95.0% to 98.0%, and RSDs (n=5) found in the range of 2.3% to 5.1%.

       

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