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Inspired by the distinct chemical and physical properties of nanoparticles, here a novel open‐tubular capillary electrochromatography column was prepared by electrostatic assembly of poly(diallydimethylammonium chloride) onto the inner surface of a fused‐silica capillary, followed by self‐adsorption of negatively charged SH‐β‐cyclodextrin/gold nanoparticles. The formation of the SH‐β‐cyclodextrin/gold nanoparticles coated capillary was confirmed and characterized by scanning electron microscopy and energy dispersive spectrometry. The results of scanning electron microscopy and energy dispersive spectrometry studies indicated that SH‐β‐cyclodextrin/gold nanoparticles were successfully coated on the inner wall of the capillary column. The performance of the SH‐β‐cyclodextrin/gold nanoparticles coated capillary was validated by the analysis of six pairs of chiral drugs, namely zopiclone, carvedilol, salbutamol, terbutaline sulfate, phenoxybenzamine hydrochloride, and ibuprofen. Satisfactory enantioseparation results were achieved, confirming the use of gold nanoparticles as the support could enhance the phase ratio of the open‐tubular capillary column. Additionally, the stability and reproducibility of the SH‐β‐cyclodextrin/gold nanoparticles coated capillary column were also investigated. Then, this proposed method was well validated with good linearity (≥0.999), recovery (90.0–93.5%) and repeatability, and was successfully used for enantioseparation of ibuprofen in spiked plasma samples, which indicated the new column's potential usage in biological analysis. [ABSTRACT FROM AUTHOR]

A novel open‐tubular capillary electrochromatography column coated with β‐cyclodextrin was prepared using the sol‐gel technique. In the sol‐gel approach, owing to the three‐dimensional network of sol‐gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating enantiomers were shown. The influences of capillary inner diameter, coating time, organic modifier, buffer pH, and buffer concentration on separation were investigated. The sol‐gel‐coated β‐cyclodextrin column has shown improved enantioseparation efficiency of chlorphenamine, brompheniramine, pheniramine, zopiclone in comparison with the sol‐gel matrix capillary column. The migration time relative standard deviation of the separation of the enantiomers was less than 0.89% over five runs and 2.9% from column to column. This work confirmed that gold nanoparticles are promising electrochromatographic support to enhance the phase ratio of open‐tubular capillary electrochromatography column in capillary electrochromatography. [ABSTRACT FROM AUTHOR]

[Display omitted] • An anionic carboxymethyl- β -cyclodextrin (CM- β -CD) silica hybrid monolithic column was first prepared by "one-pot" sequential reaction. • The novel CM-β-CD monolithic columns were successfully used in enantioseparation of 10 drugs. • The columns' preparation conditions (DMSO, AIBN and PEG) and separation conditions (buffer pH, ACN proportion, separation voltage and buffer solution) were optimized using model analytes. • The mechanism of chiral recognition was demonstrated using molecular modeling with AutoDock. In this paper, an anionic carboxymethyl- β -cyclodextrin (CM- β -CD) silica hybrid monolithic column was first prepared by "one-pot" sequential reaction. The chiral stationary phase (CSP) and prepared monolithic column were demonstrated by fourier transform infrared (FT-IR), nuclear magnetic resonance (1H NMR) and scanning electron microscope (SEM). To obtain better separation efficiency, the columns' preparation conditions (DMSO, AIBN and PEG) and separation conditions (buffer pH, ACN proportion, separation voltage and buffer solution) were optimized using model analytes. The resulting columns were finally used in chiral separations of ten racemic compounds, and satisfactory separation selectivity was obtained. The RSDs lower than 3.0% were obtained through run-to-run (n = 6), day-to-day (n = 3), and column-to-column determinations (n = 3). Furthermore, the mechanism of chiral recognition was demonstrated using molecular modeling with AutoDock. This proposed method was also well validated with good linearity (≥0.998), recovery (96.79–97.88%) and repeatability, and was successfully used for enantiomeric impurity detection of S -ofloxacin tablet. As a novel chiral stationary phase, CM- β -CD was supposed to be a promising prospect in the further analysis of chiral samples. [ABSTRACT FROM AUTHOR]