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Extraction And Separation Of Active Components From T. Wilfordii And Utilization Of The Seeds Of J. Curcas

Posted on:2012-10-06Degree:DoctorType:Dissertation
Country:ChinaCandidate:J MinFull Text:PDF
GTID:1221330362953754Subject:Pharmaceutical Engineering
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Supercritical fluid extraction (SFE) is an environmentally friendly chemical separation technology, which is considered as one of the key technologies in the modernization of extracting and separating natrual products and traditional Chinese medicine. In this paper, SFE combined with other advanced technologies was used to make both the extraction and separation of active components from Tripterygium Wilfordii Hook.f. (T. Wilfordii) and the utilization of the seeds of Jatropha curcas (J. curcas).T. Wilfordii is a traditional Chinese medicine, which has many pharmacological actions such as anti-inflammatory, antibacterial, immunosuppressive and antifertility. Triptolide is considered as the main active component while tripterine as the main toxic component. Besides, tripterine is reported to be strongly anticancer.Based on the results of preliminary studies, industrial SFE equipment was used for the sacle-up of SFE processes of T. Wilfordii. The peeled roots of T. Wilfordii were extracted with supercritical CO2 (SC-CO2) +75% ethanol, aiming to increase the yield of triptolide and decrease the yield of tripterine. The yields of triptolide and tripterine were 1.56 and 2.27 times as much as those of traditional methods, respectively. The yeilds were lower but still in the same magnitude compared to those of pilot experiments, indicating the scale-up process was feasible. The root bark of T. Wilfordii was extracted with SC-CO2 + ethanol, aiming to increase the yield of tripterine. The yield of tripterine was 1.28-2.56 and 1.02 times as much as those of traditional methods and pilot experiments, respectively. The results were consistent to pilot experiments, indicating the feasibility of the scale-up process.An“acidification–alkalization–organic solvent extraction”process was designed and investigated for further separation of triptolide and tripterine in the extracts obtained from the scale-up SFE experiments. High performance liquid chromatography was performed for the detection of triptolide and tripterine in the products. Under optimal separation condtions, the following results could be obtained: no triptolide was detectable in the product of tripterine, no tripterine was detectable in the product of triptolide, and neither triptolide nor tripterine was detectable in the product of total alkaloids. Therefore triptolide, tripterine and total alkaloids were well separated and enriched with the optimal separation process.Above results showed the process of“SFE-acidification-alkalization-organic solvent extraction”can efficiently extract triptolide and tripterine, and well separate triptolide, tripterine and total alkaloids in the extracts. It provided a new approach and technology support for the appropriate utilization of T. Wilfordii. With a high content of non-edible seed oil, J. curcas is world recognized as the most potential plant to be the substitute of fossils. In this study, jatropha seed oil was extracted with SC-CO2 and the extraction of molluscacidal saponins from the seeds was explored.Firstly, seed oil was extracted from the seed kernels of J. curcas by SC-CO2. The effect of some factors such as particle size, extraction temperature and pressure on the yield of seed oil was investigated. A maximum yield of 51.5% (recovery 92.1%) can be obtained under the optimal conditions (particle size: 250-380μm, 55℃and 40MPa). The scale-up experiment of the optimal conditions gave a yield of 47.25% (recovery 84.5%), which was lower than that of pilot experiemnts but higher than that of traditional methods, indicating the SC-CO2 extraction process was feasible.Secondly, saponins were extracted from the de-oiled seed kernels by heat reflux extraction with ethanol solution. The influences of water temperature, concentration of ethanol solution, solid-liquid ratio and extraction times on the yield of total saponins were investigated by an orthogonal design. The range analysis showed the factors were in an order of extraction times > solid-liquid ratio > concentration of ethanol solution > water temperature. And the optimal extraction conditions were extraction with 80% ethanol with a solid-liquid ratio of 1:10 under the water temperature of 80℃for 3 times. The maximum yield of total saponins was 1.955% (recovery 88.64%) among the experiments.Lastly, the solubilities of jatropha seed oil in SC-CO2 at definite temperatures and pressures were caculated from the initial slope of the extraction curve of yield versus volumes of SC-CO2 and correlated with the Chrastil equation and modified Chrastil equation with AARDs of 10.10 % and 3.468 %, respectively. In addition, the SC-CO2 extraction process of jatropha seed oil was simulated with the broken and intact cell model and two-stage diffusion model, respectively. The values of AARDs were in the range of 1.08-3.67 % and 3.01%-10.24%, respectively, indicating that both models had good simulation results. The above theoretical studies therefore provide basic data and technoglogy support for the industrial scale-up and process design of the SC-CO2 extraction of jatropha seed oil.
Keywords/Search Tags:supercritical CO2 extraction, triptolide, tripterine, jatropha seed oil, saponin, solubility, mass transfer model
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