Citation: LU Yangfang, WANG Hui, WANG Guiming, WANG Yan, GU Xue, YAN Chao. Preparation of 1 μm non-porous C18 silica gel stationary phase for chiral-pressurized capillary electrochromatography[J]. Chinese Journal of Chromatography, ;2015, 33(3): 209-214. doi: 10.3724/SP.J.1123.2014.11030 shu

Preparation of 1 μm non-porous C18 silica gel stationary phase for chiral-pressurized capillary electrochromatography

1.
School of Pharmacy, Shanghai Jiao Tong University, Shanghai 200240, China

Corresponding author: WANG Yan, YAN Chao,
Received Date: 26 November 2014
Available Online: 26 December 2014
Fund Project: 国家自然科学基金项目(21175092,21105064) (21175092,21105064)国家重大科学仪器设备开发专项(2011YQ150072,2011YQ15007204,2011YQ15007207,2011YQ15007210) (2011YQ150072,2011YQ15007204,2011YQ15007207,2011YQ15007210)上海市自然科学基金项目(12ZR1413600). (12ZR1413600)

Non-porous C18 silica gel stationary phase (1 μm) was prepared and applied to chiral separation in pressurized capillary electrochromatography (pCEC) for the enantioseparation of various basic compounds. The non-porous silica particles (1 μm) were synthesized using modified Stöber method. C18 stationary phase (1 μm) was prepared by immobilization of chloro-dimethyl-octadecylsilane. Using carboxymethyl-β-cyclodextrin (CM-β-CD) as the chiral additive, the pCEC conditions including the content of acetonitrile (ACN), concentration of buffer, pH, the concentration of chiral additive and flow rate as well as applied voltage were investigated to obtain the optimal pCEC conditions for the separation of four basic chiral compounds. The column provided an efficiency of up to 190000 plates/m. Bupropion hydrochloride, clenbuterol hydrochloride, metoprolol tartrate, and esmolol hydrochloride were baseline separated under the conditions of 5 mmol/L ammonium acetate buffer at pH 4.0 with 20% (v/v) acetonitrile, and 15 mmol/L CM-β-CD as the chiral additive. The applied voltage was 2 kV and flow rate was 0.03 mL/min with splitting ratio of 300:1. The resolution were 1.55, 2.82, 1.69, 1.70 for bupropion hydrochloride, clenbuterol hydrochloride, metoprolol tartrate, esmolol hydrochloride, respectively. The C18 coverage was improved by repeating silylation method. The synthesized 1 μm C18 packings have better mechanical strength and longer service life because of the special, non-porous structure. The column used in pCEC mode showed better separation of the racemates and a higher rate compared with those used in the capillary liquid chromatography (cLC) mode. This study provided an alternative way for the method of pCEC enantioseparation with chiral additives in the mobile phase and demonstrated the feasibility of micron particle stationary phase in chiral separation.
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沈阳化工大学材料科学与工程学院沈阳 110142