毛细管电色谱法用于头孢羟氨苄的手性拆分

Chiral separation of cefadroxil by capillary electrochromatography.

作者信息

Liu Haixing, Yu Aimin, Liu Fengqin, Shi Yuhua, Han Likun, Chen Yunfa

机构信息

Department of Chemistry, Weifang University, Weifang 261061, China.

出版信息

J Pharm Biomed Anal. 2006 Jun 16;41(4):1376-9. doi: 10.1016/j.jpba.2006.02.032. Epub 2006 Apr 4.

DOI:10.1016/j.jpba.2006.02.032

PMID:16600557

Abstract

In this paper, the chiral separation of cefadroxil was studied by capillary electrochromatography. Monolithic capillary column was prepared for the separation of cefadroxil enantiomers. The optimum buffer contained 28.5 mmol/L sodium acetate, 0.95% (v/v) acetic acid, 19 mmol/L beta-cyclodextrin (beta-CD) and 5% (v/v) isopropanol in formamide solution (pH 7.0), with the running voltage of 12 kV, the UV detector wavelength of 254 nm, the sample injected time of 8s and the temperature of 25 degrees C. Under these conditions, the column efficiency of cefadroxil enantiomers were N1=5324 and N2=23,768 with a selectivity factor (alpha) of 1.056 and resolution (Rs) of 0.978. The effect of buffer pH value, beta-CD concentration, organic modifier (isopropanol) concentration and voltage was also investigated for the separation by CEC.

摘要

本文采用毛细管电色谱法研究了头孢羟氨苄的手性拆分。制备了整体式毛细管柱用于分离头孢羟氨苄对映体。最佳缓冲液为在甲酰胺溶液（pH 7.0）中含有28.5 mmol/L醋酸钠、0.95%（v/v）乙酸、19 mmol/Lβ-环糊精（β-CD）和5%（v/v）异丙醇，运行电压为12 kV，紫外检测器波长为254 nm，进样时间为8 s，温度为25℃。在此条件下，头孢羟氨苄对映体的柱效分别为N1 = 5324和N2 = 23768，选择性因子（α）为1.056，分离度（Rs）为0.978。还研究了缓冲液pH值、β-CD浓度、有机改性剂（异丙醇）浓度和电压对毛细管电色谱分离的影响。