马钱子碱和士的宁的硅胶柱色谱与半制备高效液相色谱法联用分离纯化  

The seperation and purification of brucine and strychnine from Semen Strychni by silica gel column chromatography combined with semi-preparative HPLC

作　　者：吴小娟[1] 马凤森[1,2] 喻炎 

机构地区：[1]浙江工业大学药学院,浙江杭州310014 [2]浙江中医药大学第三临床医学院,浙江杭州310012

出　　处：《时珍国医国药》2016年第9期2145-2147,共3页Lishizhen Medicine and Materia Medica Research

基　　金：浙江省重大科技专项重点社会发展项目(No.2010C13014);浙江省自然科学基金(No.Y2111194);浙江省重点科技创新团队计划资助(No.2013TD15)

摘　　要：目的通过硅胶柱色谱与半制备高效液相色谱法联用,建立一种高效、快速分离高纯度活性单体马钱子碱和士的宁的方法。方法马钱子总生物碱粗提物经硅胶柱色谱分离,再经半制备高效液相分离纯化,以Silica C18M 10E(250 mm×10 mm,5μm)为色谱柱,乙腈(A)∶水-冰乙酸-氨水(230∶2.4∶0.4)(B)=12∶88为流动相进行等度洗脱2m L/min,检测波长254 nm,柱温25℃,进样量500 u L。结果单次进样50 mg可纯化得到9.65mg马钱子碱和17.91 mg士的宁,纯度分别为98.84%,98.06%,收率分别为73.32%,83.48%。结论该方法简单、快速,可用于高纯度中药活性单体的制备。Objective Silica gel column chromatography and semi-preparation HPLC were employed to establish an efficient and fast method for separation and purification of high purity active monomer of brucine and strychnine. Methods The crude alkaloid extract from the seeds of Semen Strychni was preliminary purified by silica gel column chromatography which was followed by semi-preparative HPLC separation. The semi-preparative HPLC conditions were as follows： column was Silica C18 M 10E（ 250 mm × 10 mm,5 μm）,mobile phase was a mixture of acetonitrile（ A） ： water-glacial acetic acid-ammonium hydroxide（ 230 ： 2. 4 ： 0. 4）（ B） = 12 ： 88,flow rate was 2 m L /min,wavelength was 254 nm,column temperature was 25 ℃,injection volume was 500 μL. Results 9. 65 mg of brucine and 17. 91 mg of strychnine were separated from 50 mg of the crude extracts with the purity of 98. 84% and 98. 06% respectively,the yield rate were about 73. 32% and 83. 48% respectively. Conclusion The method established has the characteristics of simplicity,rapidity and can be used for the preparation of active monomer of traditional Chinese medicine.

关 键 词：硅胶柱色谱 半制备高效液相色谱 马钱子碱 士的宁 活性单体 

分 类 号：R284.1[医药卫生—中药学]