College of Chemistry, Jilin University, Qianjin Street 2699#, Changchun 130012, China.
College of Chemistry, Jilin University, Qianjin Street 2699#, Changchun 130012, China.
J Chromatogr A. 2014 May 23;1343:47-54. doi: 10.1016/j.chroma.2014.03.067. Epub 2014 Apr 3.
A poly(butyl methacrylate-co-ethyleneglyceldimethacrylate) (poly(BMA-EDMA)) monolithic column was prepared with in situ polymerization method and modified with allylamine-β-cyclodextrin (ALA-β-CD) and nano-cuprous oxide (Cu2O). A polymer monolith microextraction method was developed with the modified monolithic column for the preconcentration of polychlorinated biphenyls combined with gas chromatography-electron capture detector. Various parameters affecting the extraction efficiency were investigated and optimized. Under the optimum experimental conditions, we obtained acceptable linearities, low limits of detection, and good intra-day/inter-day relative standard deviations. Because of the hydrophobic properties of β-CD and the porous nano structure of Cu2O, the enrichment capacity of the poly(BMA-EDMA) monolithic column was significantly improved. The extraction efficiency followed the order: poly(BMA-EDMA-ALA-β-CD-Cu2O)>poly(BMA-EDMA-ALA-β-CD)>poly(BMA-EDMA)>direct GC analysis. When applied to the determination of polychlorinated biphenyls in wine samples, low limits of detection (0.09ngmL(-1)) were obtained under the preoptimized conditions (sample volume 1.0mL, sample flow rate 0.1mLmin(-1), eluent volume 0.1mL, and eluent flow rate 0.05mLmin(-1)). In addition, the present method was employed to determine polychlorinated biphenyls in red wine samples and the accuracy was assessed through recovery experiments. The obtained recovery values were in the range of 78.8-104.1% with relative standard deviations less than 9.0%.
一种聚（甲基丙烯酸丁酯-co-乙二醇二甲基丙烯酸酯）（poly（BMA-EDMA））整体柱是通过原位聚合方法制备的，并通过丙烯酰胺-β-环糊精（ALA-β-CD）和纳米氧化亚铜（Cu2O）进行了修饰。开发了一种带有改性整体柱的聚合物整体微萃取方法，用于与气相色谱-电子捕获检测器结合对多氯联苯进行预浓缩。研究并优化了影响萃取效率的各种参数。在最佳实验条件下，我们获得了可接受的线性度、低检测限和良好的日内/日间相对标准偏差。由于β-CD 的疏水性和 Cu2O 的多孔纳米结构，poly（BMA-EDMA）整体柱的富集能力得到了显著提高。萃取效率的顺序为：poly（BMA-EDMA-ALA-β-CD-Cu2O）>poly（BMA-EDMA-ALA-β-CD）>poly（BMA-EDMA）>直接 GC 分析。当应用于葡萄酒样品中多氯联苯的测定时，在预优化条件下（样品体积 1.0mL，样品流速 0.1mLmin(-1)，洗脱液体积 0.1mL，洗脱液流速 0.05mLmin(-1)），可获得低检测限（0.09ngmL(-1)）。此外，本方法还用于测定红酒样品中的多氯联苯，并通过回收率实验评估了准确性。得到的回收率在 78.8-104.1%范围内，相对标准偏差小于 9.0%。
