Key Laboratory of Medicinal Chemistry and Molecular Diagnosis of Ministry of Education, College of Pharmaceutical Science, School of Life Sciences, Hebei University, Baoding, 071002, China.
Key Laboratory of Public Health Safety of Hebei Province, College of Public Health, Hebei University, Baoding, 071002, China.
Anal Chim Acta. 2022 Sep 22;1227:340328. doi: 10.1016/j.aca.2022.340328. Epub 2022 Aug 30.
Owing to the severe toxicity and health hazard of polychlorinated biphenyls (PCBs) to humans, the efficient separation and determination of PCBs in dairy products is highly desirable and challenging. In this study, a new solid-phase microextraction (SPME) fiber was prepared by coating of a new molecularly imprinted phenolic resin (MIPR) in situ using a covalent grafting method. The MIPR coating, synthesized from 4-mercaptophenol and glutaraldehyde, provides rough surface with more adsorption sites; furthermore, the coating has a thickness of 1.0 μm, resulting in rapid equilibration. This new device has the advantages such as less coating peeling from the substrate and selective recognition enhancement of the coating. A highly selective and sensitive SPME-based method was developed using the developed fiber, coupled with GC-MS/MS, for the determination of polychlorinated biphenyls (PCBs) in milk samples. The developed MIPR-HS-SPME-GC-MS/MS method showed low detection limits (0.012-0.066 pg mL), good linearity (r ≥ 0.9991), satisfactory recovery (77.5-116.7%), efficient enhancement factors (362-2034 folds) and good reusability (50 cycles). Therefore, this is a simple and efficient strategy for monitoring trace PCBs in complex samples and is a potential alternative for improving the selectivity of SPME fibers by introducing MIPR into the fiber coating.
由于多氯联苯（PCBs）对人类具有严重的毒性和健康危害，因此高效分离和测定乳制品中的 PCBs 是非常理想和具有挑战性的。在本研究中，通过共价接枝法原位合成了一种新型的分子印迹酚醛树脂（MIPR），制备了一种新型固相微萃取（SPME）纤维。MIPR 涂层由 4-巯基苯酚和戊二醛合成，提供了具有更多吸附位点的粗糙表面；此外，涂层厚度为 1.0μm，实现了快速平衡。这种新的纤维具有较少的涂层从基底剥落和涂层选择性识别增强等优点。采用开发的纤维，结合 GC-MS/MS，建立了一种基于 SPME 的高度选择性和灵敏的方法，用于测定牛奶样品中的多氯联苯（PCBs）。所开发的 MIPR-HS-SPME-GC-MS/MS 方法具有较低的检测限（0.012-0.066pgmL）、良好的线性（r≥0.9991）、令人满意的回收率（77.5-116.7%）、高效的增强因子（362-2034 倍）和良好的可重复使用性（50 次循环）。因此，这是一种简单有效的策略，用于监测复杂样品中的痕量 PCBs，通过将 MIPR 引入纤维涂层，可以提高 SPME 纤维的选择性，是一种潜在的替代方法。
