Study On Separation And Preparation Of The Products Deriving From Vinblastine

Technology in mass purification and industrialized production of complex natural resources monomer is bottleneck problem, which restricts the industrialization of activated natural resources from plants. Combination of different effective technologies is one of key technologies to produce complex natural resources monomer with high purity .This paper took Vinorelbine and its intermediate Anhydrovinblastine as example, which were semi-synthesized from vinblastine with complex and activated structure, studying technology about its mass purification and prudction, to provide academic and practical reference for mass purification and industrialized production of other natural resources. Here are the main studying content:1. Purification and separation of intermediate product Anhydrovinblastine. Comparison of different purification techniques for the Anhydrovinblastine was presented. Crystallography was selected out as the best method used to purify anhydrovinblastine in industry. Results showed that the purification of crud Anhydrovinblastine can get from 30% to 65% after the process of crystallization with the yield of 70%.2. Preliminary separating Vinorelbine from liquid hydrolysate. Sephadex LH-20 chromatography and crystallography were taken to preliminary separate Vinorelbine in liquid hydrolysate. Results indicated that the reclaim rate of solid matter is high ,but Sephadex LH-20 chromatography could not separate Vinorelbine from impurities effectively. At last, crystallography was selected out as the best method used to purify anhydrovinblastine in liquid hydrolysate. It can heighten the content of Vinorelbine from 30% to 50%. This process is simple and convenient, and suitable to be magnified in industrialization.3. Further purification of Vinorelbine, which include middling purification and high purification two steps. Normal dry-column manufactured by our-self was used to purify Vinorelbine with developer the same to TLC. After purified by dry-column flash chromatography, the purity of vinorelbine can get to 80% from 55% at the very beginning. The load of dry-column was 12 mg specimen per 1 g silica gel, the best diameter/tallness was 1/10, and the yield of vinorelbine can get to 82%. MCI-GEL CHP-20 reversed-phase chromatography was used in tandem to separate vinorelbine from impurities which were difficult to be separated. The best purification conditions of crud vinorelbine were methanol/water(V:V=80:20), The load of reversed-phase column was 10 mg specimen per 1 g MCI-GEL CHP-20 stuffing. The purity of vinorelbine can get to 98% when MCI-GEL CHP-20 reversed-phase chromatography and crystallization in sequence were used.Technique for high efficient purification of Vinorelbine was investigated in this thesis. A series of feasible process conditions for Purification and separation of Vinorelbine and Anhydrovinblastine were obtained, which are suitable to be used in synthesis of vinorelbine in industry. It gives both academic and practical reference for mass production and purification of other natural resources monomer.