在卵类粘蛋白手性柱上拆分药物对映体西替利嗪的研究

Study on Enantiomeric Separation of Cetirizine on HPLC with a Chiral Ovomucoid Column

目的:建立利用卵类粘蛋白手性固定相拆分西替利嗪对映异构体的反相高效液相色谱分析方法,研究色谱条件对拆分结果的影响和该蛋白柱的部分拆分机理。方法:西替利嗪溶解在流动相中配成浓度为22μg·mL-1的溶液,用Ultron Es-OVM柱(5μm,150 mm×4.6 mm),流动相为磷酸二氢钾缓冲溶液与有机改进剂(甲醇或乙醇或乙腈)的混合溶液,紫外器波长230 nm,柱温25℃。结果:首次利用卵类粘蛋白手性柱成功拆分了西替利嗪药物对映体,最佳分离条件:乙腈-20 mmol·L-1磷酸二氢钾(pH 6.20,用磷酸和氢氧化钾溶液调节)(18:82),流速0.5 mL·min-1,出峰时间在20 min内,分离度达到1.68。结论:本方法简单、快速,无需柱前衍生,可方便用来拆分和检测西替利嗪对映体。

Objective: To establish an HPLC method for the enantiomeric separation of cetirizine with a chiral ovo mucoid column. To investigate the affection of chromatographic conditions on the enantiomeric separation and chiral recognition mechanism of ovomucoid column. Methods:The sample of cetirizine was dissolved in mobile phase with concentration of 22μg·mL-1. Ultron ES - OVM (5μm,150 mm×4. 6 mm) was used as analytical column with mobile phase consisted of three different organic modifiers (methanol, ethanol and acetonitrile respectively) and phosphate buffer solution. The chromatograms were monitored by UV detection and the wavelength of 230 nm was selected. The column temperature was fixed on 25℃. Results: The enantiomers of cetirizine were separated on a ovomucoid column firstly and successfully with resolution 1.68 and elution time in 20 minutes under the optimum separation conditions:CH3CN-20 mmol·L-1KH2PO4(pH 6.20,adjusted by H3PO4and KOH) (18:82) ,flow rate was 0. 5 mL·min-1. Conclusion:The method is simple,quick and without derivation and can be used for separation and determination enantiomers of cetirizine conveniently.