Institute of Pharmaceutical Analysis, College of Pharmacy, Jinan University, Guangzhou, 510632, China; Department of Pharmacy and Guangdong Province Key Laboratory of Pharmacodynamic Constituents of Traditional Chinese Medicine & New Drug Research, Jinan University, Guangzhou, 510632, China.
Institute of Pharmaceutical Analysis, College of Pharmacy, Jinan University, Guangzhou, 510632, China.
J Chromatogr A. 2019 Mar 15;1588:33-40. doi: 10.1016/j.chroma.2018.12.038. Epub 2018 Dec 18.
A novel molecularly imprinted inorganic-organic hybrid monolith (MIP hybrid monolith) was fabricated through a facile single-step polymerization strategy with levofloxacin (LEV) as the template, 3-aminopropyltriethoxysilane-methacrylic acid as the hybrid functional monomer and ethylene glycol dimethacrylate as the crosslinker in a mixed porogen of methanol, toluene and dodecanol. The optimized LEV-MIP hybrid monolith was characterized using scanning electron microscopy and fourier transform-infrared spectroscopy. Uniform monolithic matrix with large through-pores in the network skeleton of LEV-MIP hybrid monolith was observed. The influence of polymerization conditions on the specific recognition behavior of the resulting monolith was systematically investigated. The LEV-MIP hybrid monolith exhibited much better adsorption (3.62 times) and selectivity towards LEV in comparison with non-imprinted hybrid monolith. Furthermore, the LEV-MIP hybrid monolith based solid-phase extraction combining with liquid chromatography-mass spectrometry was applied for the selective determination of fluoroquinolones (FQs) in infant formula powder. The average recoveries of six FQs in milk powders spiked at 20, 50 and 100 μg kg were in the range of 82.91-102.00% with the precision of 1.04-7.39%. The limit of detection and limit of quantitation of the proposed method were in a range of 0.19-1.24 μg kg and 0.63-4.13 μg kg, respectively.
一种新型的分子印迹无机-有机杂化整体柱（MIP 杂化整体柱）通过简便的一步聚合策略制备，以左氧氟沙星（LEV）为模板，3-氨丙基三乙氧基硅烷-甲基丙烯酸为杂化功能单体，乙二醇二甲基丙烯酸酯为交联剂，甲醇、甲苯和十二醇的混合孔剂。采用扫描电子显微镜和傅里叶变换红外光谱对优化后的 LEV-MIP 杂化整体柱进行了表征。观察到 LEV-MIP 杂化整体柱的网络骨架中具有均匀的大贯通孔的整体基质。系统研究了聚合条件对所得整体柱的特异性识别行为的影响。与非印迹杂化整体柱相比，LEV-MIP 杂化整体柱对 LEV 的吸附（3.62 倍）和选择性更好。此外，将基于 LEV-MIP 杂化整体柱的固相萃取与液相色谱-质谱联用，用于婴幼儿配方奶粉中氟喹诺酮类（FQs）的选择性测定。在奶粉中添加 20、50 和 100μg/kg 的六种 FQs 的平均回收率在 82.91%-102.00%之间，精密度为 1.04%-7.39%。该方法的检出限和定量限分别在 0.19-1.24μg/kg 和 0.63-4.13μg/kg 范围内。
