环糊精手性固定相拆分氟西汀对映体
首发时间:2007-01-08
摘要:采用二甲基-β-环糊精手性固定相在反相条件下直接拆分了氟西汀对映异构体。系统考察了流动相的组成与配比、离子强度、pH值、流速及柱温等因素对氟西汀对映体分离的影响。研究发现,以甲醇或乙腈为流动相改性剂,均可很好地拆分氟西汀对映体。优化后的色谱条件为:流动相为乙腈-0.1%醋酸三乙胺缓冲液(15/85,v/v;pH 4.5),柱温35℃;或者流动相为甲醇-0.2%醋酸三乙胺缓冲液(30/70,v/v;pH 3.8),柱温20 ℃。由Van Deemter方程可得最佳流速约为0.3 ml/min;然而,以乙腈和甲醇为改性剂分别在1.0 ml/min和0.8 ml/min以下时已可达基线分离(RS>1.5)。此外,由Van’t Hoff曲线,得到了氟西汀对映体与固定相间相互作用的焓变、焓变差值和熵变差值等热力学参数,并且判定氟西汀对映体的拆分过程为焓控过程。
关键词: 对映体拆分 手性固定相 氟西汀 环糊精衍生物 高效液相色谱
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Resolution of fluoxetine enantiomers on cyclodextrin chiral stationary phase by HPLC
Abstract:Fluoxetine hydrochloride enantiomers were separated by high performance chromatography on dimethylated β-cyclodextrin chiral stationary phase (CSP). The effects of mobile phase composition, ionic strength, pH, flow rate and column temperature on capacity factor, separation factor and resolution were studied systematically. Fluoxetine enantiomers were separated with acetonitrile or methanol as mobile phase modifier. Best separation was obtained with a mobile phase composition of acetonitrile – 0.1% TEAA of 15/85 (v/v, pH 4.5) at 35℃ or methanol – 0.2% TEAA of 30/70 (v/v, pH 3.8) at 20℃. The optimal flow rate was 0.3 ml/min from Van Deemter equation, however, baseline resolution (RS>1.5) was achieved under flow rate of 1.0 ml/min and 0.8 ml/min with acetonitrile and methanol, respectively. Thermodynamic parameters ΔH0, ΔS,RΔH0 and ΔS,RΔS0 were calculated. In general, in the temperature range examined the enthalpic contribution to the enantiomer transfer energy was found to be more significant than the entropic one.
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