氟西汀在二甲基环糊精手性固定相上的拆分

Separation of fluoxetine hydrochloride enantiomers on cyclodextrin chiral stationary phase

为了直接拆分盐酸氟西汀对映体,提出了二甲基-β-环糊精手性固定相高效液相色谱(HPLC)分离方法.采用Φ4.6 mm×250 mm的色谱柱,以质量分数为0.1%的醋酸三乙胺(TEAA)缓冲液为流动相,以乙腈或甲醇为改性剂,紫外检测波长采用226 nm.考察了流动相的组成、缓冲液pH值、体积流量及柱温对氟西汀分离的影响.结果表明,以乙腈和pH 4.5缓冲液质量比为12.1∶87.9的溶液为流动相,在柱温35℃和体积流量为1.0 mL/min下,氟西汀分离度为1.81.以甲醇和pH 3.8缓冲液质量比为25.3∶74.7的溶液为流动相,在柱温20℃和体积流量为0.8 mL/min下,氟西汀分离度为2.22.二甲基-β-环糊精手性固定相可很好地分离氟西汀对映体.

To directly separate fluoxetine hydrochloride enantiomers, high performance liquid chromatography （HPLC） separation method on dimethylated β-cyclodextrin chiral stationary phase was investigated. By adopting the chromatography column of 04. 6 mm × 250 mm, triethylamine acetate （TEAA） buffer with mass fraction of 0.1% was taken as the mobile phase, and acetonitrile or methanol was taken as modifier using ultraviolet detection wavelength of 226 nm. The effects of mobile phase composition, buffer pH, volume flow rate and column temperature on fluoxetine separation were investigated. The results show that when mass ratio of acetonitrile and pH 4.5 buffer in mobile phase is 12.1 ：87.9, fluoxetine resolution is 1.81 at column temperature of 35℃ and volume flow rate of 1.0 mL/min. When mass ratio of methanol and pH 3.8 buffer in mobile phase is 25.3： 74.7, fluoxetine resolution is 2.22 at column temperature of 20 ℃ and volume flow rate of 0.8 mL/min. Dimethylated β-cyclodextrin chiral stationary phase can effectively separate fluoxetine hydrochloride enantiomers.