State Key Laboratory of Applied Organic Chemistry, Lanzhou University, Lanzhou, 730000, China.
Anal Bioanal Chem. 2009 Oct;395(4):1125-33. doi: 10.1007/s00216-009-3020-5. Epub 2009 Aug 19.
A magnetic molecularly imprinted polymer (M-MIP) of bisphenol A (BPA) was prepared by miniemulsion polymerization. The morphological and magnetic characteristics of the M-MIP were characterized by Fourier-transform infrared spectroscopy, transmission electron microscopy, and vibrating sample magnetometry. The adsorption capacities of the M-MIP and the nonimprinted polymer were investigated using static adsorption tests, and were found to be 390 and 270 mg g(-1), respectively. Competitive recognition studies of the M-MIP were performed with BPA and the structurally similar compound DES, and the M-MIP displayed high selectivity for BPA. A method based on molecularly imprinted solid-phase extraction assisted by magnetic separation was developed to extract BPA from environmental water and milk samples. Various parameters such as the mass of sorbent, the pH of the sample, the extraction time, and desorption conditions were optimized. Under selected conditions, extraction was completed in 15 min. High-performance liquid chromatography with UV detection was employed to determine BPA after the extraction. For water samples, the developed method exhibited a limit of detection (LOD) of 14 ng L(-1), a relative standard deviation of 2.7% (intraday), and spiked recoveries ranging from 89% to 106%. For milk samples, the LOD was 0.16 microg L(-1), recoveries ranged from 95% to 101%, and BPA was found in four samples at levels of 0.45-0.94 microg L(-1). The proposed method not only provides a rapid and reliable analysis but it also overcomes problems with conventional solid-phase extraction (SPE), such as the packing of the SPE column and the time-consuming nature of the process of loading large-volume samples.
采用细乳液聚合法制备了双酚 A（BPA）的磁性分子印迹聚合物（M-MIP）。采用傅里叶变换红外光谱、透射电子显微镜和振动样品磁强计对 M-MIP 的形态和磁性特征进行了表征。通过静态吸附试验研究了 M-MIP 和非印迹聚合物的吸附容量，分别为 390 和 270 mg/g。采用 M-MIP 对 BPA 和结构类似的化合物 DES 进行了竞争性识别研究，结果表明 M-MIP 对 BPA 具有高选择性。建立了一种基于磁性固相萃取辅助分子印迹的方法，用于从环境水样和牛奶样品中提取 BPA。优化了各种参数，如吸附剂的质量、样品的 pH 值、萃取时间和解吸条件。在选定的条件下，萃取在 15 分钟内完成。萃取后采用高效液相色谱-紫外检测法测定 BPA。对于水样，所建立的方法的检测限（LOD）为 14 ng/L，日内相对标准偏差为 2.7%，加标回收率范围为 89%至 106%。对于牛奶样品，LOD 为 0.16 μg/L，回收率范围为 95%至 101%，在四个样品中检测到 BPA 的浓度为 0.45-0.94 μg/L。该方法不仅提供了快速可靠的分析，而且克服了传统固相萃取（SPE）的问题，如 SPE 柱的填充和加载大容量样品过程的耗时性质。
