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Study On Efficient Separation Technology Of Active Ingredients From Schisandra Chinensis (Turcz.) Baill. And Multistage Utilization Of Medicinal Resources

Posted on:2014-08-31Degree:DoctorType:Dissertation
Country:ChinaCandidate:C H MaFull Text:PDF
GTID:1263330401479572Subject:Botany
Abstract/Summary:PDF Full Text Request
In this study, Schisandra chinensis as raw materials, production process route of comprehensive utilization of S. chinensis medicinal resources, and optimize each segment of the process.Four kinds of different extraction methods were used for extracting S. chinensis essential oil, including hydro-distillation (HD), steam-distillation (SD), microwave assisted hydro-distillation (MHD) and solvent-free microwave assisted distillation (SMD). The extraction kinetic curves showed that the efficiency of MHD and MSD was higher, and the extraction yields were1.20and1.10mL/kg after30min, respectively. DPPH radical scavenging experiments, iron reduction ability test and β-carotene and linoleic acid bleaching experiments were investigated to study the antioxidant activity of essential oil extracted from different extraction methods, and compared with the natural antioxidants Vc and VE. The antioxidant activity of essential oil extracted from SMD was better than that from HD and SD. Through the analysis of the physical characteristics of essential oil, it was found that the refractive index and the density of essential oil obtained by SMD were a little higher than that of essential oil obtained by HD and SD, and the color was darker. S. chinensis fruits after extracting by different methods were observed by scanning electron microscope (SEM), and found that the heat emitted by microwave transfer from the interior of the cell after being heated, and then the partial pressure increased, causing the cell walls rupture, and the essential oil was extracted more completely. S. chinensis fruits after extracting by different methods were analyzed by thermal gravimetric analysis (TGA), the weightlessness of the fruits extracted by SMD was least, showed that the essential oil was extracted more completely. The main component of essential oil was analyzed by GC-MS, more than90%of volatile components were olefins, and there is also a small portion of the alcohols and esters with hydroxyl group, so the antioxidant effect of S. chinensis essential oil is perfect good. SMD as an "environmentally friendly" method for extracting essential oil, showed the higher extraction yield and saved the amount of organic solvents, can also instead of HD and SD.Optimized the conditions of extracting S. chinensis anthocyanins with acidic water stirred at room temperature by response surface method (RSM). Under the optimal conditions, the extraction yield of anthocyanins was up to29.06mg/g. The crude anthocyanins extract was purificated by HPD-300macroporous resin, the purity of anthocyanins increased from5.01%to29.97%, and the antioxidant capacity significantly improved. The iron reduction capacity and the ABTS radical scavenging capacity were respectively1.2times and1.7times more than that before purification. Study on the content and color stability of S. chinensis anthocyanins on the conditions of different pH value, and in acid solution, which pH is1.0, the anthocyanins compound is most stability. The content and color stability of S. chinensis anthocyanins on the conditions of being heated were also investigated, the degradation of anthocyanin was much slow at less than40℃, and the higher temperature, the longer time being heated, the faster degradation rate. Thermal degradation was according to first order kinetics model, and the correlation coefficients were greater than0.99at different temperature. The content and color stability of S. chinensis anthocyanins on the conditions of ultraviolet radiation were also studied. S. chinensis anthocyanins solution was radiated by three wavelength ultraviolet light (UVA, UVB and UVC), the degradation of anthocyanins was more serious at the shorter UV wavelength. The content and color stability of S. chinensis anthocyanins in the process of ultrasound or microwave were investigated, too. The major component of S. chinensis anthocyanins was cyanidin-3-O-xylosylrutinoside, about95%of the total content by LC-MS determination.Compared with different method for extracting S. chinensis polysaccharides, and optimized the single factor of reflux extraction (RE), ultrasound assisted extraction (UAE), and microwave assisted extraction (MAE). Under the optimal conditions, the extraction yields of crude polysaccharides were85.6g/kg,74.4g/kg, and80.2g/kg, respectively. According to the experimental results of the single factor, alternating UAE and MAE of polysaccharides were operated. Under the optimal experiments conditions, the extraction yield of crude polysaccharides was88.7g/kg. The crude polysaccharides was deproteinized by sevag method4times, and the refined polysaccharides yield was51.1g/kg. And then the refined polysaccharides were graded into four kinds of polysaccharides with different volume fractions of ethanol. Study on hydroxyl radical scavenging ability of polysaccharides, and the results showed that the scavenging ability of polysaccharides was similar with Vc, when the concentration of polysaccharides was less than0.2mg/mL. When the concentration of polysaccharides was higher than0.2mg/mL, the scavenging ability of polysaccharides was nearly2times better than Vc. The in vitro activity test of polysaccharides showed that200μg/mL was the optimal concentration of S. chinensis polysaccharides to promote cell growth and in combination with ConA and Lps, the synergism of Lps was better than that of ConA about1.5times.UPLC-MS/MS and HPLC-UV detection method of S. chinensis biphenyl cyclooctene lignans were set up. Comparisons of different methods for extracting lignans:the extraction yield of lignans with Soxhlet extraction was the highest of all, but the dissolution yield of impurity was also higher due to the prolonged being heated. Because of too time-consuming,50℃hot-dip and cold soaking at room temperature were not suitable apply to industrial production. Though the yield of lignans was not high with ultrasound assisted extraction (UAE) and microwave assisted extraction (MAE), the purity of extract was relatively higher, can be used as a laboratory preparation method of lignans.80%ethanol reflux extracted2.5h was suitable for large-scale production to prepare lignans crude extract, the lignans yield was0.344mg/g and the purity of extract was1.60%. Ionic liquid MAE method can be obtained essential oil and lignans simultaneously. The ester-bond lignans was hydrolyzed under being heated alkaline conditions by hydrolysis in situ extraction method. The increased content of free-state lignans was enriched in the organic solvent at the same time with hydrolysis, then the organic phase was concentrated and the lignans crude extract was obtained. The lignans yield was0.506mg/g, and the purity of lignans extract was5.46%. After201*7basic anion exchange resin hydrolysis in combination with HPD-5000macroporous resin enrichment, the lignans yield was0.454mg/g, and the purity of lignans extract was27.5%. Purified the Lignans extract using silica gel column chromatography, the purity of lignans was96.5%, and the recovery was more than95%.Extracted S. chinensis seed oil with different solvent and different methods. Petroleum ether as the extraction solvent, ultrasound assisted extraction (UAE) of seed oil, the yield of seed oil was the highest11.39%, light in color and transparent. The apparent color of seed oil extracted with the ethyl acetate was dark and muddy. Chemical indexes of seed oil extracted by the different solvent and methods were detected, the acid value, saponification value and peroxide value of seed oil extracted by microwave-assisted extraction (MAE) was slightly lower, compared with that by UAE. The acid value (11.2mg KOH/g oil) and saponification value (109.0mg KOH/g oil) of seed oil extracted with petroleum ether was minimum. The iodine value (107.6mg KI/g oil) was also lowest, that to say the unsaturated degree was the lowest. Therefore, the seed oil extracted with petroleum ether by UAE was selected as the raw material for preparation of biodiesel. The seed oil was heated for preparation of biodiesel, with concentrated sulfuric acid, an ion exchange resin, or an ionic liquid as a catalyst, respectively. FT-IR and TG were used to analysis the seed oil and biodiesel. The content of saturated and unsaturated fatty acids in seed oil, and fatty acid methyl esters in biodiesel were measured by GC-MS, high sensitivity, good repeatability, also quantitative accuracy.In the thermochemical conversion process of S. chinensis residues, under the optimal conditions, the discharging speed was1.9-2.1kg/min, the residues rod bar was high density, no cracks on the surface, no significant carbonization, and no spray phenomenon. In the pyrolysis reaction of S. chinensis residues, the forming rod bar was200g, pyrolysis power was200W, the final temperature was about350℃, and the pyrolysis time was120min. Under the above conditions, the yields of gas, vinegar, tar, and biomass carbon were13-17%,28-32%,18-23%, and13-17%, respectively. The distillate liquid after pyrolysis was separated into vinegar and tar with the rapid low-temperature deposition method. The vinegar was dried by anhydrous sodium sulfate, and then extracted by organic solvent, not only can remove water, also can be enriched polyphenol antioxidants. The radical scavenging ability and iron reducing power of vinegar ethyl formate extract were similar with that of synthetic antioxidants BHA. And then the composition of vinegar and bio-oil was analyzed by GC-MS. BET informed that the surface area, the pore volume, and the average pore size of the activated biomass carbon were690.47m2/g,0.31cm3/g,1.88nm, respectively.Process diagram of the comprehensive utilization of S. chinensis medicinal resources was set up, enlarged the raw materials amount, and the experimental results were basically consistent with the small test results. The process realized the full advantage of the natural active products in S. chinensis fruits, and zero emissions to the environment. And strive to get the maximum output and economic benefits, with the minimum raw materials input and energy consumption.
Keywords/Search Tags:Schisandra chinensis (Turcz.) Baill., essential oil, anthocyanins, polysaccharide, biphenyl cyclooctene lignans, seed oil, residues
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