Fanali S, Cotichini V, Porrà R
Istituto di Cromatografia del C.N.R., Area della Ricerca di Roma, Italy.
J Capillary Electrophor. 1997 Jan-Feb;4(1):21-6.
Capillary electrophoresis has been used for the separation of venlafaxine and two of its impurities deriving from the synthesis process. The electrophoretic experiments were performed using background electrolytes at different pHs in the 2.5-9.2 range in order to study the effective mobilities and resolution of the three examined compounds. The optimum experimental conditions for the baseline resolution of the three analytes was found at pH 6.5. Very good repeatability for both migration time and corrected peak areas was achieved. The calibration curve was studied for venlafaxine (concentration range 26-224 micrograms/mL), and the plot of the peak area ratio (sample/internal standard [IS]) versus venlafaxine concentration was linear with a correlation coefficient of 0.9991. The effect of different cyclodextrins (CDs), namely, gamma-cyclodextrin (gamma-CD), hydroxypropyl-beta-CD (HP-beta-CD), and alpha-cyclodextrin (alpha-CD), on effective mobility and enantiomeric resolution (R) of venlafaxine (Wy45030) and its impurities (imp1 and imp2) was studied at different pHs, and the best results were obtained at pH 9.2. Venlafaxine was baseline resolved in its enantiomers using gamma-CD or HP-beta-CD, while imp1 (Wy45494) was baseline resolved using alpha-CD.
毛细管电泳已用于分离文拉法辛及其合成过程中产生的两种杂质。为了研究三种被测化合物的有效迁移率和分离度,使用pH值在2.5 - 9.2范围内的不同背景电解质进行电泳实验。在pH 6.5时发现了三种分析物基线分离的最佳实验条件。迁移时间和校正峰面积均具有非常好的重复性。研究了文拉法辛(浓度范围为26 - 224微克/毫升)的校准曲线,峰面积比(样品/内标[IS])与文拉法辛浓度的关系图呈线性,相关系数为0.9991。在不同pH值下研究了不同环糊精(CDs),即γ-环糊精(γ-CD)、羟丙基-β-环糊精(HP-β-CD)和α-环糊精(α-CD)对文拉法辛(Wy45030)及其杂质(imp1和imp2)有效迁移率和对映体分离度(R)的影响,在pH 9.2时获得了最佳结果。使用γ-CD或HP-β-CD时,文拉法辛的对映体实现了基线分离,而使用α-CD时,imp1(Wy45494)实现了基线分离。