D-10-樟脑磺酸铵-薄层色谱法拆分普萘洛尔对映体

Enantioseparation of racemic Propranolol using D-10-camphor ammonium sulphonate by TLC

目的研究薄层色谱拆分普萘洛尔对映体的新方法。方法采用D-10-樟脑磺酸铵手性离子对试剂-薄层色谱法,在硅胶GF254板上拆分普萘洛尔对映体;考察展开体系、温度、预饱和时间、pH、手性离子对试剂浓度以及湿度对拆分效果的影响。结果最佳分离条件为D-10-樟脑磺酸铵溶液(0.85 mmo.lL-1,pH8.0)-二氯甲烷-甲醇(0.3:1.95:0.75)在8℃下预饱和30 min,样品溶液的pH7.0,以1%香草醛浓硫酸溶液显色。结论所用方法可拆分普萘洛尔。

OBJECTIVE To establish a new method for enantioseparation of racemic Propranolol hydrochloride by TLC. METHODS The separation was carried out on silica gel GF254 plate, using D - 10 - camphor ammonium sulfonate as chiral ion - pair agent in the mobile phase. The effects of the mobile phase, temperature, presaturation time, pH, the concentration of ion - pair agent and humidity on separation were investigated. RESULTS The optimal separation condition was D - 10 - camphor ammonium sulfonate （0. 85 mmol·L^-1 ,pH 8.0） - dichloromethane -methanol（0. 3 ： 1.95 ： 0. 75）, presaturated for 30 rain at 8℃ in advance, the pH of sample was 7.0, taking 1% vanillin/sulfuric acid as chromogenic agent. CONCLUSION Propranolol enantiomer is successfully separated in this way.