Preparation of a reversed-phase/anion-exchange mixed-mode spherical sorbent by Pickering emulsion polymerization for highly selective solid-phase extraction of acidic pharmaceuticals from wastewater
Preparation of a reversed-phase/anion-exchange mixed-mode spherical sorbent by Pickering emulsion polymerization for highly selective solid-phase extraction of acidic pharmaceuticals from wastewater
复制标题
Pickering乳液聚合制备反相/阴离子交换混合模式球形吸附剂用于高选择性固相萃取废水中的酸性药物
DOI：
10.1016/j.chroma.2017.09.021
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发表时间：
2017-10-27
影响因子：
4.1
通讯作者：
Chen, Jiping
中科院分区：
文献类型：
--
作者：
Huang, Chaonan;Li, Yun;Chen, Jiping
采用一步Pickering乳液聚合法合成了聚甲基丙烯酸二乙氨基乙酯-二乙烯基苯（poly（DEAEMA-DVB））球形多孔粒子，并以此为基础制备了一种简单有效的新型混合模式阴离子交换（MAX）吸附剂。聚（DEAEMA-DVB）粒子用1，4-丁二醇二缩水甘油醚（BDDE）季铵化，然后通过环氧-胺反应三乙胺（TEA）提供强的阴离子交换性能。采用扫描电镜、傅里叶变换红外光谱、氮吸附-脱附和元素分析等手段对合成的MAX吸附剂进行了表征。MAX吸附剂球形规则，粒径分布窄（15-35 μ m），IEC值为0.54 meq/g，碳含量为80.3%，氮含量为1.62%。与聚（DEAEMA-DVB）相比，MAX吸附剂表现出降低的S-BET（390.5 vs. 515.3 m（2）g（-1））、孔体积（0.74 vs. 0.85 cm（3）g（-1））和孔径（16.8 vs. 17.3 nm）。此外，用于生产MAX吸附剂的N含量的变化揭示了成功的两步季铵化，这可能与如此高的IEC高度相关。最后，MAX吸附剂被成功地评价为选择性分离和纯化的一些选定的酸性药物（酮洛芬，KEP;萘普生，NAP;和布洛芬，IBP）从中性（氢化可的松，HYC），碱性（卡马西平，CAZ;阿米替林，AMT）药物和其他干扰的水样品中使用固相萃取（SPE）。建立了一种基于MAX混合模式固相萃取与HPLC-UV联用的高效分析方法，用于高选择性萃取和净化加标废水样品中的酸性KEP、NAP和IBP。该方法具有良好的灵敏度（0.009-0.085 μ g L ~（-1））、回收率（82.1%~ 105.5%）和重复性（RSD <7.9%，n = 3）。(C)2017爱思唯尔B. V.保留所有权利。
The present work represents a simple and effective preparation of a novel mixed-mode anion exchange (MAX) sorbent based on porous poly[2-(diethylamino)ethyl methacrylate-divinylbenzene] (poly(DEAEMA-DVB)) spherical particles synthesized by one-step Pickering emulsion polymerization. The poly(DEAEMA-DVB) particles were quatemized with 1,4-butanediol diglycidyl ether (BDDE) followed by triethylamine (TEA) via epoxy-amine reaction to offer strong aniOn exchange properties. The synthesized MAX sorbent was characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, nitrogen adsorption-desorption measurements and elemental analysis. The MAX sorbent possessed regular spherical shape and narrow diameter distribution (15-35 mu m), a high IEC of 0.54 meq/g, with carbon and nitrogen contents of 80.3% and 1.62%, respectively. Compared to poly(DEAEMA-DVB), the MAX sorbent exhibited decreased S-BET (390.5 vs. 515.3 m(2) g(-1)), pore volume (0.74 vs. 0.85 cm(3) g(-1)) and pore size (16.8 vs. 17.3 nm). Moreover, changes of N content for producing the MAX sorbent reveal a successful two-step quaternization, which can be highly related to such a high IEC. Finally, the MAX sorbent was successfully evaluated for selective isolation and purification of some selected acidic pharmaceuticals (ketoprofen, KEP; naproxen, NAP; and ibuprofen, IBP) from neutral (hydrocortisone, HYC), basic (carbamazepine, CAZ; amitriptyline, AMT) pharmaceuticals and other interferences in water samples using solid phase extraction (SPE). An efficient analytical method based on the MAX-based mixed-mode SPE coupled with HPLC-UV was developed for highly selective extraction and cleanup of acidic KEP, NAP and IBP in spiked wastewater samples. The developed method exhibited good sensitivity (0.009-0.085 mu g L-1 limit of detection), satisfactory recoveries (82.1%-105.5%) and repeatabilities (relative standard deviation < 7.9%, n = 3). (C) 2017 Elsevier B.V. All rights reserved.