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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
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2017-09-08 , DOI: 10.1016/j.chroma.2017.09.021
Chaonan Huang , Yun Li , Jiajia Yang , Junyu Peng , Jing Jin , Dhanjai , Jincheng Wang , Jiping Chen

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 quaternized 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 μm), 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 SBET (390.5 vs. 515.3 m2 g−1), pore volume (0.74 vs. 0.85 cm3 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 μg L−1 limit of detection), satisfactory recoveries (82.1%–105.5%) and repeatabilities (relative standard deviation < 7.9%, n = 3).



中文翻译:

皮克林乳液聚合制备反相/阴离子交换混合模式球形吸附剂用于废水中酸性药物的高选择性固相萃取

本工作代表了一种简单有效的方法,该方法基于一种合成的多孔聚[2-(二乙基氨基)甲基丙烯酸甲酯-二乙烯基苯](聚(DEAEMA-DVB))球形颗粒为基础的新型混合模式阴离子交换(MAX)吸附剂的制备。分步Pickering乳液聚合。聚(DEAEMA-DVB)颗粒通过环氧-胺反应先后与1,4-丁二醇二缩水甘油醚(BDDE)和三乙胺(TEA)季铵化,以提供强大的阴离子交换性能。合成的MAX吸附剂通过扫描电子显微镜,傅立叶变换红外光谱,氮吸附-解吸测量和元素分析进行​​表征。MAX吸附剂具有规则的球形形状和狭窄的直径分布(15-35μm),IEC值为0.54 meq / g,碳和氮含量分别为80.3%和1.62%。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)。而且,用于生产MAX吸附剂的N含量的变化表明成功的两步季铵化,这与如此高的IEC高度相关。最后,成功评估了MAX吸附剂从中性(氢化可的松,HYC)中选择性分离和纯化某些选定的酸性药物(酮洛芬,KEP,萘普生,NAP和布洛芬,IBP)的能力。),碱性(卡马西平,CAZ;阿米替林,AMT)药物以及使用固相萃取(SPE)的水样中的其他干扰物。建立了基于MAX的混合模式SPE与HPLC-UV结合的高效分析方法,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。所开发的方法显示出良好的灵敏度(0.009–0.085μgL -1检测限),令人满意的回收率(82.1%–105.5%)和可重复性(相对标准偏差<7.9%,n = 3)。

更新日期:2017-09-08
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