Citation: CHENG Biaoping, LI Laisheng, ZHOU Rendan, NIE Guizhen, ZHANG Hongfu. Enantioseparation and determination of atenolol enantiomers in tablets on a β-cyclodextrin-based chiral stationary phase by high performance liquid chromatography[J]. Chinese Journal of Chromatography, ;2014, 32(11): 1219-1224. doi: 10.3724/SP.J.1123.2014.07018 shu

Enantioseparation and determination of atenolol enantiomers in tablets on a β-cyclodextrin-based chiral stationary phase by high performance liquid chromatography

1.
Center of Analysis and Testing, Nanchang University, Nanchang 330047, China

Corresponding author: LI Laisheng,
Received Date: 9 July 2014
Available Online: 21 August 2014
Fund Project: 国家自然科学基金项目(21165012) (21165012)江西省自然科学基金项目(2010GZH0089) (2010GZH0089)江西省教育厅科技项目(GJJ11274). (GJJ11274)

A novel dinitrophenyl ether β-cyclodextrin-bonded chiral stationary phase (NESP) for HPLC was prepared with ordered mesoporous SBA-15 as matrix. The fast enantioseparation of atenolol enantiomers on the new stationary phase was achieved through the optimization of mobile phase composition, column temperature and other factors in polar organic solvent mode. The optimized composition of mobile phase was acetonitrile/methanol/glacial acetic acid/triethylamine (90:10:2.5:3.0, v/v/v/v) at the flow rate of 0.5 mL/min. The column temperature was set at 20 ℃. The detection wavelength was 275 nm. The resolution of atenolol enantiomers was 1.73 with a rather short analysis time, about 20 min, under the above conditions. The atenolol was extracted with methanol from the tablets and analyzed by direct injection for HPLC. A new quantitative method of atenolol enantiomers in tablets was established after the condition optimization. The good linear relationships for two atenolol enantiomers were observed in the range of 2.5-100 mg/L with r of 0.9992 and 0.9989, respectively. The recoveries of atenolol enantiomers in tablet samples were 94.60%-97.24%. The relative standard deviations (RSDs) of this method were not greater than 0.92% for intra-day and 1.86% for inter-day, respectively. The detection limits (S/N=3) of concentrations were less than 0.2 mg/L for both enantiomers. The established method is simple and of high selectivity, high recovery and low cost for enantiomer analysis by using homemade cyclodextrin-based chiral column. It has a good application prospect for the fast quality control and the pharmacokinetics study of chiral drugs.
- high performance liquid chromatography (HPLC),
- β-cyclodextrin-bonded SBA-15 stationary phase (NESP),
- β-adrenergic blockers,
- atenolol,
- quantification of enantiomers,
- tablets
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沈阳化工大学材料科学与工程学院沈阳 110142