Poly(glycidyl methacrylate)-co-(ethylene dimethacrylate) [poly(GMA-co-EDMA)] monoliths were used as a support to grow a zeolitic imidazolate framework-8 (ZIF-8) via layer-by-layer self-assembly. Pepsin, acting as as chiral selector, was covalently linked to the surface of the amino-modified ZIF-8 through the Schiff base method. The material was characterized by scanning electron microscopy, thermogravimetric analysis, X-ray diffraction, Fourier transform infrared spectroscopy and elemental analysis. The pepsin-ZIF-8-poly(GMA-co-EDMA) column was utilized to the enantioseparation of the racemic forms of hydroxychloroquine (HCQ), chloroquine (CHQ), hydroxyzine (HXY), nefopam (NEF), clenbuterol (CLE) and amlodipine (AML). In comparison with a pepsin-poly(GMA-co-EDMA) monolithic column (without self-assembled ZIF-8 nanoparticles), the resolution is strongly enhanced (HCQ: 0.34 → 2.50; CHQ: 0.45 → 1.97; HXY: 0.39 → 1.43; NEF: 0.27 → 0.81; CLE: 0 → 0.81; AML: 0.16 → 0.72). Effects of self-assembly layers of ZIF-8, pepsin concentration, buffer pH values and applied voltage were investigated with hydroxychloroquine as the model analyte. The reproducibility of run-to-run, day-to-day and column-to-column were explored, and found to be satisfactory.
Schematic representation of capillary electrochromatography (CEC) systems with a pepsin-zeolitic imidazolate framework-8 (ZIF-8) modified poly(glycidyl methacrylate)-co-(ethylene dimethacrylate) [poly(GMA-co-EDMA)] monolithic column as stationary phases for separation of basic racemic drugs. ZIF-8 modified column was prepared via layer-by-layer self-assembly.
Ma Mingxuan,Du Yingxiang,Yang Jiangxia,Feng Zijie,Ding Wen,Chen Cheng
Poly(glycidyl methacrylate)-co-(ethylene dimethacrylate) [poly(GMA-co-EDMA)] monoliths were prepared, and used as a support to attach gold nanoparticles (AuNP) via Au-S bond. Pepsin, acting as a chiral selector, was linked to the surface of the carboxyl-modified AuNP through a hydrochloride/N-hydroxysuccinimide coupling reaction. The material was characterized by scanning electron microscopy, energy dispersive X-ray spectrometry, transmission electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy and N 2 adsorption-desorption isotherm. The pepsin@AuNP@poly(GMA-co-EDMA) monolith showed preferable enantioselectivity for hydroxychloroquine (HCQ), chloroquine (CHQ), hydroxyzine (HXY), labetalol (LAB), nefopam (NEF), clenbuterol (CLE), amlodipine (AML) and chlorpheniramine (CHL) in capillary electrochromatography (CEC). These racemic drugs were monitored at the maximum absorption wavelength (220 nm for HXQ, CHQ, HXY, LAB, NEF; 240 nm for AML; 215 nm for CLE, CHL). In comparison with the pepsin@poly(GMA-co-EDMA) monolith loaded with 5 nm AuNP, the pepsin@poly(GMA-co-EDMA) monolith loaded with 13 nm AuNP shows significantly enhanced enantiomeric resolution (HCQ: 0.62 → 3.45; CHQ: 0.60 → 2.11; HXY: 0.49 → 2.30; LAB: 1.03 → 2.45, 1.45 → 3.46, 0 → 0.67; NEF: 0.53 → 1.29; CLE: 0.42 → 0.56; AML: 0 → 0.83; CHL: 0.24 → 0.55). Pepsin concentration, buffer pH value, buffer concentration and applied voltage were investigated in detail with (±) HCQ and (±) HXY as model analytes. The reproducibility of intra-day, inter-day and column-to-column were explored, and found to be satisfactory.
Schematic presentation of the preparation of gold nanoparticles (AuNP) modified.
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