Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023, China; University of Chinese Academy of Sciences, Beijing 100049, China.
Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023, China.
Anal Chim Acta. 2015 May 4;872:35-45. doi: 10.1016/j.aca.2015.02.058. Epub 2015 Feb 23.
The bisphenol A (BPA) imprinted polymer microspheres were prepared by simple Pickering emulsion polymerization. Compared to traditional bulk polymerization, both high yields of polymer and good control of particle sizes were achieved. The characterization results of scanning electron microscopy and nitrogen adsorption-desorption measurements showed that the obtained molecularly imprinted polymer microsphere (MIPMS) particles possessed regular spherical shape, narrow diameter distribution (30-60 μm), a specific surface area (S(BET)) of 281.26 m(2) g(-1) and a total pore volume (V(t)) of 0.459 cm(3) g(-1). Good specific adsorption capacity for BPA was obtained in the sorption experiment and good class selectivity for BPA and its seven structural analogs (bisphenol F, bisphenol B, bisphenol E, bisphenol AF, bisphenol S, bisphenol AP and bisphenol Z) was demonstrated by the chromatographic evaluation experiment. The MIPMS as solid-phase extraction (SPE) packing material was then evaluated for extraction and clean-up of these bisphenols (BPs) from human urine samples. An accurate and sensitive analytical method based on the MIPMS-SPE coupled with HPLC-DAD has been successfully established for simultaneous determination of eight BPs from human urine samples with detection limits of 1.2-2.2 ng mL(-1). The recoveries of BPs for urine samples at two spiking levels (100 and 500 ng mL(-1) for each BP) were in the range of 81.3-106.7% with RSD values below 8.3%.
双酚 A(BPA)印迹聚合物微球通过简单的 Pickering 乳液聚合制备而成。与传统的本体聚合相比,该方法既可以获得高收率的聚合物,又可以很好地控制粒径。扫描电子显微镜和氮气吸附-脱附测量的表征结果表明,所得到的分子印迹聚合物微球(MIPMS)颗粒具有规则的球形形状、较窄的粒径分布(30-60μm)、比表面积(S(BET))为 281.26m(2)g(-1)和总孔体积(V(t))为 0.459cm(3)g(-1)。在吸附实验中,对 BPA 具有良好的特异性吸附能力,通过色谱评价实验证明了对 BPA 及其七种结构类似物(双酚 F、双酚 B、双酚 E、双酚 AF、双酚 S、双酚 AP 和双酚 Z)具有良好的类选择性。然后,将 MIPMS 作为固相萃取(SPE)填充材料,用于从人尿样中萃取和净化这些双酚类化合物(BPs)。建立了一种基于 MIPMS-SPE 与 HPLC-DAD 相结合的准确、灵敏的分析方法,用于同时测定人尿样中 8 种 BPs,检测限为 1.2-2.2ngmL(-1)。在两个加标水平(每个 BP 为 100 和 500ngmL(-1))下,BPs 在尿样中的回收率在 81.3-106.7%之间,相对标准偏差(RSD)低于 8.3%。