Gao Die, Wang Dan-Dan, Zhang Qian, Yang Feng-Qing, Xia Zhi-Ning, Zhang Qi-Hui, Yuan Chun-Su
School of Pharmaceutical Sciences, Chongqing University , Chongqing 400030, China.
Department of Pharmaceutical Sciences, School of Pharmacy, Southwest Medical University , Luzhou, Sichuan 646000, China.
J Agric Food Chem. 2017 Feb 15;65(6):1158-1166. doi: 10.1021/acs.jafc.6b05269. Epub 2017 Feb 3.
A method based on molecularly imprinted solid-phase microextraction (MIP-SPME) coupled with liquid chromatography-quadrupole time-of-flight tandem mass spectrometry (QTOF-MS/MS) was developed for the detection of luteolin and its metabolites in vivo. The MIP-SPME fibers were first fabricated by dopamine and silane, and then luteolin MIPs-coated fibers were successfully prepared using luteolin, acrylamide (AM), and ethylene glycol dimethacrylate (EGDMA) as the template, functional monomer and cross-linker, respectively. The characterizations of polymers were analyzed by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and the Brunauer-Emmett-Teller method (BET). The properties involving adsorption and selective experiments were evaluated, and these results revealed that MIP fibers presented high adsorption capacity and selectivity to luteolin. Furthermore, the developed MIP-SPME coupled with the LC-QTOF-MS/MS method was adopted to capture and identify luteolin and its metabolites in rat livers in vivo, and eventually, apigenin, chrysoeriol, and diosmetin were rapidly identified as metabolites.
建立了一种基于分子印迹固相微萃取（MIP-SPME）与液相色谱-四极杆飞行时间串联质谱（QTOF-MS/MS）联用的方法，用于体内木犀草素及其代谢产物的检测。首先用多巴胺和硅烷制备MIP-SPME纤维，然后分别以木犀草素、丙烯酰胺（AM）和乙二醇二甲基丙烯酸酯（EGDMA）为模板、功能单体和交联剂，成功制备了木犀草素分子印迹聚合物涂层纤维。通过扫描电子显微镜（SEM）、傅里叶变换红外光谱（FT-IR）和Brunauer-Emmett-Teller法（BET）对聚合物进行了表征。对其吸附和选择性等性能进行了评价，结果表明MIP纤维对木犀草素具有高吸附容量和选择性。此外，采用所建立的MIP-SPME与LC-QTOF-MS/MS联用方法，对大鼠肝脏中木犀草素及其代谢产物进行了体内捕获和鉴定，最终快速鉴定出芹菜素、 Chrysoeriol和香叶木素为代谢产物。
