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机构地区:[1]桂林理工大学化学与生物工程学院,广西桂林541004
出 处:《分析测试学报》2011年第8期853-857,共5页Journal of Instrumental Analysis
基 金:国家自然科学基金资助项目(20665003);广西自然科学基金资助项目(0728214)
摘 要:以磺化β-环糊精(S-β-CD)为手性选择剂,建立了毛细管电泳-电化学发光法测定文拉法辛(VEN)对映体浓度的方法。考察了S-β-CD浓度、缓冲液pH值及浓度、进样时间与电压、分离电压和检测电位对VEN对映体分离以及联吡啶钌电致化学发光检测的影响,优化了分离条件,考察了VEN的电化学行为与发光机理。在优化条件下,2种VEN对映体在0.1~1 000μg/L质量浓度范围内与其发光强度呈良好线性,检出限分别为0.01、0.05μg/L。该法用于人血浆中VEN对映体的分离检测,两对映体的回收率为94%~100%,相对标准偏差不大于3.2%。A capillary electrophoresis coupled with electrochemiluminescence detection(CE-ECL)was successfully developed for the chiral separation and determination of a kind of antidepressants racemic drug(venlafaxine) enantiomers by employing sulfated β-cyclodextrin(S-β-CD)as the chiral selector.The determination conditions,including inlet and outlet buffers,injection time and voltage,separation voltage and detection potential were optimized.Unlike the traditional chiral separation method,the buffers used in the capillary inlet and outlet differed from each other.Under the optimum conditions,baseline enantioresolution and highly sensitive detection for the enantiomers of venlafaxine were achieved.The results showed that there was a linear relationship between Luminous intensity(I) and two venlafaxine enantiomers(S,R) concentrations(ρ) in the range of 0.1 μg/L to 1 000 μg/L.And the linear regression equations were IS=321.5ρ+30.1(r=0.999 6) and IR=319.3ρ +28.4(r=0.999 4),respectively.The detection limits(S/N=3) were obtained to be 0.01 μg/L and 0.05 μg/L,respectively,which were lower than the reported value about 3 orders of magnitude.The recoveries were in the range of 94%-100% with relative standard deviations no more than 3.2%.Therefore,the CE-ECL method has the application potential in chiral separation,and could be used to detect drug enantiomers in clinical pharmacology.
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