title: Preparation and evaluation of monodispersed, submicron, non-porous silica particles functionalized with β-CD derivatives for chiral-pressurized capillary electrochromatography.
abstract: Submicron, non-porous, chiral silica stationary phase has been prepared by the immobilization of functionalized β-CD derivatives to isocyanate-modified silica via chemical reaction and applied to the pressurized capillary electrochromatography (pCEC) enantio-separation of various chiral compounds. The submicron, non-porous, cyclodextrin-based chiral stationary phases (sub_μm-CSP2) exhibited excellent chiral recognition of a wide range of analytes including clenbuterol hydrochloride, mexiletine hydrochloride, chlorpheniramine maleate, esmolol hydrochloride, and metoprolol tartrate. The synthesized submicron particles were regularly spherical and uniformly non-porous with an average diameter of around 800 nm and a mean pore size of less than 2 nm. The synthesized chiral stationary phase was packed into 10 cm × 100 μm id capillary columns. The sub_μm-CSP2 column used in the pCEC system showed better separation of the racemates and at a higher rate compared to those used in the capillary liquid chromatography mode (cLC) system. The sub_μm-CSP2 possessed high mechanical strength, high stereoselectivity, and long lifespan, demonstrating rapid enantio-separation and good resolution of samples. The column provided an efficiency of up to 170,000 plates/m for n-propylbenzene.
authors.affiliation: School of Pharmacy, Shanghai Jiao Tong University, Shanghai, Shanghai, P. R. China.
authors.forename: Lu
authors.initials: L
authors.lastname: Yangfang
authors.affiliation: School of Pharmacy, Shanghai Jiao Tong University, Shanghai, Shanghai, P. R. China.
authors.forename: Wang
authors.initials: W
authors.lastname: Hui
authors.affiliation: School of Pharmacy, Shanghai Jiao Tong University, Shanghai, Shanghai, P. R. China.
authors.forename: Xue
authors.initials: X
authors.lastname: Yun
authors.affiliation: School of Pharmacy, Shanghai Jiao Tong University, Shanghai, Shanghai, P. R. China.
authors.forename: Gu
authors.initials: G
authors.lastname: Xue
authors.affiliation: School of Pharmacy, Shanghai Jiao Tong University, Shanghai, Shanghai, P. R. China.
authors.forename: Wang
authors.initials: W
authors.lastname: Yan
authors.affiliation: School of Pharmacy, Shanghai Jiao Tong University, Shanghai, Shanghai, P. R. China.
authors.forename: Yan
authors.initials: Y
authors.lastname: Chao
mesh_terms: D000085:Acetates; D000097:Acetonitriles; D053801:Capillary Electrochromatography / Q000379:methods*; D056148:Chromatography, Reverse-Phase; D053758:Nanoparticles / Q000737:chemistry*; D016062:Porosity; D012822:Silicon Dioxide / Q000737:chemistry*; D013237:Stereoisomerism; D047392:beta-Cyclodextrins / Q000737:chemistry*
chemical_list: D000085:Acetates; D000097:Acetonitriles; D047392:beta-Cyclodextrins; D012822:Silicon Dioxide; C018824:ammonium acetate; C032159:acetonitrile
keywords: Chiral separation; Submicron non-porous chiral stationary phase; cLC; pCEC; β-CD