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Study on High Effective Seperation and Purification Process of Ursolic Acid and Oleanolic Acid from Waste Residue of Catharanthus Roseus

Author: NiuHuiYing
Tutor: YangLei；ZuYuanGang
School: Northeast Forestry University
Course: Botany
Keywords: Vinca alkaloids extracted residues Ursolic acid Oleanolic acid Separate Purification
CLC: R284
Type: Master's thesis
Year: 2008
Downloads: 106
Quote: 0
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Abstract


Ursolic acid and oleanolic acid pentacyclic triterpenoids, have anti-tumor, anti-oxidation, anti-inflammatory, hepatoprotective, hypolipidemic and whitening. This study and explore from vinca alkaloids extracted residues in the separation and purification of ursolic acid and oleanolic acid process. The main conclusions are as follows: identified high-performance liquid chromatographic determination of ursolic acid and oleanolic acid: Column: HiQsil C to 18 (250mm × 4.6mm, 5μm), mobile phase: acetonitrile : methanol: 0.5% ammonium acetate = 67:12:21 (V: V: V), flow rate: 1mL/min, detection wavelength: 210 nm, column temperature: room temperature. Identified ursolic acid and oleanolic acid separation and purification process route specific process parameters are as follows: (1) to determine the process parameters of ursolic acid and oleanolic acid extraction: extraction methods for negative pressure mixed vacant of extracted ventilation 0.2m 3 / h, extraction solvent 90% ethanol, solid-liquid ratio of 1:10, extraction time 25 min, extraction times 3 times. (2) 100g dried vinca alkaloids extracted residues by 90% ethanol extract extract 19.0g extract ursolic acid in a purity of 11.00%, 97.57% of the extraction rate; purity of oleanolic acid 3.01%, 99.72% extraction rate. (3) using ethyl acetate extraction from the 90% ethanol extract ursolic acid and oleanolic acid extraction method plus ultrasonic agitation, extraction for 3 times. 19.0g ethanol extract by ethyl acetate extraction of crude 4.84g, crude ursolic acid purity of 37.32%, the recovery rate was 86.36%; oleanolic acid, a purity of 10.33%, the recovery rate was 87.26%. Further purified by column chromatography (4) ursolic acid and oleanolic acid, specific process parameters are as follows: column chromatography packing 300-400 mesh silica, The sample volume 0.2g/10g silica gel, elution solvent for n-hexyl hexane: ethyl acetate = 5:4, flow rate of 3ml/min, and collect the appropriate eluting component. Sample 2.28g, 4.84g ethyl acetate extract column chromatography the ursolic acid column chromatography product purity of 68.14%, 86.05% recovery of: oleanolic acid, a purity of 17.79%, and the recovery rate was 81.21 %. (5) column chromatography ursolic acid and oleanolic acid mixture 2.28g dissolved with anhydrous ethanol, and recrystallized at 4 ℃. Crystallization of ursolic acid and oleanolic acid crystal mixture 1.505g ursolic acid purity of 74.15%, the recovery rate was 76.39%; oleanolic acid purity of 19.91%, 78.56% recovery. (6) from 90% ethanol extract → ethyl acetate → silica gel column chromatography → ethanol recrystallization process, the total recovery of ursolic acid 55.39% 55.53% total recovery of oleanolic acid.

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