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Citation: NIE Guizhen, LI Laisheng, CHENG Biaoping, ZHOU Rendan, ZHANG Hongfu. Preparation of β-Cyclodextrin Capillary Column for Enantioseparation and Determination of Nicardipine and Manidipine by Capillary Electrochromatography[J]. Chinese Journal of Applied Chemistry, ;2014, 31(12): 1472-1480. doi: 10.3724/SP.J.1095.2014.40059 shu

Preparation of β-Cyclodextrin Capillary Column for Enantioseparation and Determination of Nicardipine and Manidipine by Capillary Electrochromatography

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

Corresponding author: LI Laisheng,
Received Date: 3 March 2014
Available Online: 5 June 2014
Fund Project: 国家自然科学基金(21165012) (21165012)江西省自然科学基金(2010GZH0089) (2010GZH0089)江西省教育厅科技项目(GJJ11274)资助 (GJJ11274)

The separation and determination methods of calcium antagonists manidipine hydrochloride and nicardipine hydrochloride enantiomers were developed by open-tubular capillary electrochromatography(CEC),respectively.A new capillary column with p-nitrophenylcarbamation β-cyclodextrin was prepared by sol-gel method.The sol-gel modified with cyclodextrin derivative was characterized by infrared spectroscopy(IR) and scanning electron microscopy(SEM).In polar organic mode,the effect of the volume fraction and concentration of added triethylamine and glacial acetic acid,the content of organic solvents,the operating voltage,and temperature on the resolution(R_S) were investigated.The optimized conditions were at 20℃,detection wavelength at 236 nm,and injection pressure at 3.448 kPa×3 s.The compositions of mobile phases were V(MeOH):V(ACN):V(TEA):V(HOAc)=57:43:0.05:0.07 for manidipine hydrochloride and V(MeOH):V(ACN):V(TEA):V(HOAc)=55:45:0.05:0.08 for nicardipine hydrochloride.The resolution(R_s) of manidipine hydrochloride was 1.39 at 25 kV.The resolution(R_s) of nicardipine hydrochloride was 1.30 at 20 kV.The RSDs of retention time and peak area were less than 1.2% and 5.6%(n=5) for the drugs,respectively.It was indicated that new column has stable electrochromatography performance.The single run time were less than 5 min for manidipine hydrochloride and less than 7 min for nicardipine hydrochloride.Good linearity were observed in the concentration range of 5.2~125.0 mg/L with correlation coefficients 0.9969 or more for both drug enantiomers.The limit of detection values were 1.8 mg/L for manidipine and 2.3 mg/L for nicardipine,respectively.The nitrophenyl carbamated β-cyclodextrin phase(NCDP) column were preliminarily used for determinations of manidipine hydrochloride and nicardipine hydrochloride tablet and capsule.
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