| In this treatise,we made the use of ethanol and petroleum as an extraction solvent to extract aucubin,gutta;percha,samara oil from Eucommia ulmoides samara.The vacuum microwave-assisted extraction method extract target compounds from the Eucommia ulmoides samara.At the same time,we optimized the extraction method and applied high-speed countercurrent chromatography(HSCCC)to seperate and enrich the aucubin from the samara of Eucommia ulmoides.The specific depiction is as followed:1.The analysis method of aucubin,gutta percha,samara oil was established and the aucubin detection conditions are as followed:the detected wavelength;205 nm;mobile phase composition:methanol:0.2%phosphoric acid solution(15:85,v/v);mobile phase flow rate:1 mL/min,injection volume of 10 ?L;column:Curosil-PFP C18(250 × 4.6 mm,5 ?m),column temperature:25?,isocratic elution of 15 min.The yield calculation method of gutta-percha was established.The samara oil were analyzed by GC-MS method and the results of the analysis showed that the main component of seed oil is ?-linolenic acid,linoleic acid,palmitic acid,oleic acid.The a-linolenic acid the highest content that is up to 64.55%.2.Confirming the effect of vacuum microwave-assisted extraction method extract samara oil and gutta percha from Eucommia ulmoides samara.single factor experiments,including soaked time,vacuum,liquid to solid ratio,microwave power,were investigated and the optimized result were microwave irradiation power 450 W,the degree of vacuum 0.09 MPa,liquid to solid ratio 20 mL/g,microwave irradiation time 25 min.The yields of gutta percha and samara oil are 91.2 mg/g and 73.4 mg/g by optimized extraction conditions.3.In the work,the vacuum microwave-assisted extraction method was applied to extract aucubin from Eucommia ulmoides samara and single factor experiments including vacuum,soak time,liquid to solid ratio,vacuum microwave power were investigated.The optimized results were the concentration of ethanol was 40%,the degree of vacuum 0.09 MPa,liquid to solid ratio of 15 mL,soaking time of 6 h,microwave power of 450 W,microwave irradiation time 15 min.Based on the single factor experiment result,the response surface method was used to optimize the extraction process.Applied the software Expert Design 7.0 to optimize three factors including vacuum degree,microwave irradiation power and liquid material ratio.The optimize result was as followed:the degree of vacuum 0.05 MPa,liquid to solid ratio 15 mL/g and microwave irradiation power 450 W.The predicted of extraction rate 54.31 mg/g.Under the optimal conditions,the average yield was 55.98 mg/g(n=3),the relative standard deviation of the predicted value was within 5%range,which showed that the predicted value of the regression equation of the model was basically consistent with the actual value.4.Aucubin was separated and enriched by using High-Speed Countercurrent Chromatography(HSCCC)from Eucommia ulmoides samara.Selection of the two-phase solvent system is ethyl acetate-n-butanol-water(2:1:2,v/v/v).the partition coefficient of 0.87.The inject conditions,including revolution speed,flow rate of the mobile phase,water bath temperature,were optimized for HSCCC system.The opimal results were revolution speed 900 r/min,flow rate of the mobile phase 1.5 mL/min,water bath temperature 40?.By the above conditions,The purity of aucubin is 97.1%after separation and purification.The separation and enrichment of aucubin were identified by analysis of 13C-NMR,1H-NMR,ESI-MS. |
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