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作 者:黄可龙[1] 胡卫国[1] 王蔚玲[1] 刘素琴[1] 焦飞鹏[1]
出 处:《分析科学学报》2007年第1期9-12,共4页Journal of Analytical Science
基 金:高校科技创新工程重大培育资金(No.704036);中南大学文理研究基金(No.0601042)
摘 要:以羟丙基-β-环糊精(HP-β-CD)作为手性添加剂,采用毛细管区带电泳(CZE)成功分离了克伦特罗(Clenbuterol,Cle)对映体。研究了β-CD种类与浓度,缓冲液pH值及浓度,操作温度等对分离的影响。结果表明,以30 mmol/L的HP-β-CD为手性添加剂,50 mmol/L的磷酸盐缓冲溶液(pH 2.5)为缓冲液,分离电压24 kV,操作温度20℃,可使Cle对映体实现基线分离,其分离度为6.78。对拆分机理也进行了探讨,测定了HP-β-CD与两对映体的结合常数及热力学参数;对CZE定量能力(线性,精度)进行了考察,R和S型的线性相关系数都大于0.998,两者的相对标准偏差(RSD)均低于2.2%。Capillary zone electrophoresis (CZE) was used for the enantiomeric separation of racemic clenbuterol with an uncoated capillary and hydroxypropyl-β-cyclodextrin (Hp-β-CD) as chiral selector. The type and concentration of β-CDs, pH and concentration of buffer, separation voltage, and operation temperature were studied and optimized, respectively. By using the concentration of 30 mmol/L HP-β-CD as chiral selector, 50 mmol/L phosphate solution (pH 2. 5) as running buffer, separation voltage of 24 kV,and operation temperature of 20℃ ,the baselines separation could be obtained with resolution of 6.78. The binding constants and thermodynamic parameters were evaluated for clenbuterol enantiomers to HP-β-CD. It was found that the chiral matching of HP-β-CD to clenbuterol enantiomers were related to the equilibrium constants of binding complexes and selectivity factor (a). The quantitative ability of CZE including linearity and precision are also investigated. The linearity coefficient of (-)-R-clunbuterol and (+)-S-clenbuterol were all above 0. 998,and both RSD were all below 2.2%.
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