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出 处:《应用化学》2009年第3期355-357,共3页Chinese Journal of Applied Chemistry
基 金:教育部高等学校博士学科点专项科研基金(20040335045)资助项目
摘 要:采用分步法制备了全苯异氰酸酯化β-环糊精键合硅胶手性固定相,并采用高效液相色谱分析技术对外消旋氟西汀、帕罗西汀、萘普生、普萘洛尔和阿普洛尔进行了拆分。实验结果发现,5种手性药物在自制的手性固定相上均获得基线分离,并且得到了最佳的色谱条件:帕罗西汀、萘普生为甲醇-0.15%TEAA(体积比35∶65,pH=4.0);氟西汀为甲醇-0.15%TEAA(体积比30∶70,pH=4.0);普萘洛尔、阿普洛尔为甲醇-0.15%TEAA(体积比40∶60,pH=5.0)。Several chiral medicines were separated on a new home-made β-cyclodextrins chiral stationary phase. The perphenylcarbamoylated β-cyclodextrin bonded silica CSP was prepared step by step, from synthesized and purified mono-6-p-toluenesulfonyl-β-eyclodextrin, mono-6-N-allylamino-β-cyclodextrin and mono-6-N-allylamino-perphenylcarbamoylated-β-eyclodextrin. By this CSP, baseline separation of five racemie medicines ( fluoxetine, paroxetine, naproxen, propranolol and alprenolol) was realized. The optimal conditions were determined. The mobile phase was methanol-0. 15% TEAA ( 35: 65, V/V, pH = 4, 0) for paroxetine and naproxen, methanol-0. 15% TEAA ( 30 : 70, WV, pH = 4. 0 ) for fluoxetine, and methanol-0. 15% TEAA (40:60, V/V, pH = 5.0 ) for propranolol and alprenolol, respectively; the flowrate was 0. 5 mL/min, the temperature 20℃, and UV-deteetor was used(254 nm).
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