Study On Extraction Technology Of Effective Components From Lonicera Japonica

Honeysuckle（Lonicera japonica Thunb.）is the dried flower bud of Lonicera japonica.Honeysuckle has heat-clearing and detoxifying,collarerals-clearing and activating,broad-spectrum anti-viral effects and so on.At present,more than 70% of the anti-inflammatory and cold proprietary Chinese medicine contains honeysuckle.With the thorough research on honeysuckle,people gradually realize that honeysuckle is covered with treasure,its application is becoming more and more widely,in the pharmaceutical industry,beverage and food industry,health care products industry and daily chemical industry.Yet the extraction,separation and application of the effective components of honeysuckle have not reached the stage of large-scale production.Therefore,it is necessary to study the extraction,separation and application of its effective components and carry out thorough research on the industrialization.Therefore,according to the maturity of technology,the input-output ratio and the feasibility of industrialization,this study selected the extraction process of volatile oil and active components to optimize and compare.The extraction and determination of process optimization and comparative analysis on the effective components of honeysuckle on small-scale tests and pilot experiments was conducted by water distillation,supercritical extraction,water extraction and alcohol precipitation and ultrasonic assisted ethanol extraction and GC-MS,HPLC and other means of modern technology,and obtained the optimal technological conditions and the evaluation index system.1.Volatile oil was extracted from honeysuckle by coeno-water distillation.Based on single factor and orthogonal test,the optimum extraction condition was studied,results showed that the optimum condition were: honeysuckle crushing level of 20 mesh,soak time of 28 h with 5 % salt solution,solid-liquid ratio of 1:10（g:mL）,extraction time of 42 h,the yield of volatile oil is 0.17 %.the product is light yellow solid with heavy taste of wax;79 components of volatile oil were detected by GC-MS,in which9 types of fatty acids（69.1%）,17 types of lipids（16.83%）and 15 types of alkane components（5.37%）accounted for a large proportion,which accounted for 91.3% of the total product.2.The essential oil from honeysuckle was extracted by supercritical CO₂ extraction.The bestextraction techniques were obtained through single factor trials and orthogonal experiments,the best extraction conditions was: extraction pressure of 45 MPa,temperature of 45 ℃,static extraction time of 0.5h,dynamic extraction time of 1 h,CO₂ fulx of 4 L/min,the yield is 2.0687% and the product is light yellow to pale green paste with delicate fragrance;Products was analyzed by GC-MS,and 57 ingredients were separated.The main components are 9 types of fatty acids（55.59%）,11 types of alkanes（21.66 %）and 11 types of lipids（5.13 %）,which accounted for 82.38% of the total extracts.Conclusion: The extraction yield can be improved by optimizing extraction conditions.3.The active ingredient of honeysuckle was extracted by water extract-alcohol precipitation,by single factor tests and response surface test,optimum extraction technology of water extract-alcohol precipitation of honeysuckle was: solid-liquid ratio of 1:30（g:m L）,extraction temperature 90 ℃,extracting2 times,each time 45 min,sank alcohol concentration 75%,chlorogenic acid extraction yield of 73.72%.Water extract-alcohol precipitation process in amplifier stage was conducted in 10 L reaction kettle,the negative pressure was added,the rest of the conditions was the same as small-scale tests,the process was measured by the ratio of the chlorogenic acid and luteoloside,the best process for vacuum degree was about 0.06 MPa,extraction temperature of 75 ℃ 77 ℃,chlorogenic acid extraction yield was91.43%,luteoloside extraction yield was 23.12%,through spray drying（optimization of spray drying conditions: Inlet air temperature of 87 ℃,material flow 460 ml/h）,chlorogenic acid content was 7.765%,and luteoloside content was 0.077% in spray drying product.The pilot experiment was conducted in 50 L extracting and concentration set,considering the extraction rate of of active ingredients,product yield and index component content in product,the vacuum degree of 0.06 MPa,temperature of 76 ℃ was selected as the optimum condition,under this condition,the product yield is 39.887%,the extraction rate of chlorogenic acid was 88.583%,the extraction rate of luteoloside was 22.838%,the chlorogenic acid content in product was 6.418%,luteoloside content was0.057%;yield of spray drying product was 22.924%,chlorogenic acid content was 7.177%,galuteolin content was 0.071%.4.The active ingredient of honeysuckle was extracted by ultrasonic assisted ethanol extraction,in laboratory test,through single factor test and orthogonal test,we obtained the optimum extractionconditions of chlorogenic acid : 50% ethanol as extraction solution,solid-liquid ratio was 1:15（g:mL）,temperature of ultrasonic extraction was 50 ℃,extracting 2 times,every time 20 min,the extraction rate of chlorogenic acid was 88.3%.The pilot experiment of alcohol extraction process was conducted in 50 L extracting and concentration set,comparison was made on the extraction of active ingredients between four ethanol concentrations of 40%,50%,60% and 70%,the best process of alcohol extract was obtained by 60%ethanol concentration,other conditions was the same as laboratory test,under this condition,the product yield was 32.94%,the extraction rate of the chlorogenic acid was 82.097%,extraction rate of galuteolin was 72.720%,content of chlorogenic acid was 7.841%,content of galuteolin was 0.239%.5.Through comprehensive comparison of the two volatile oil extraction process of honeysuckle,supercritical extraction process is superior to water distillation,volatile oil yield of supercritical extraction of was 12 times higher than water distillation,when the volatile oil is completely extracted,extraction time is shortened by more than 26 times,extraction and the separation step of supercritical extraction process was conducted in the same time with the advantages of simple operation,energy saving,,no residual organic solvent and soft delicate fragrance of the product.6.Through comprehensive comparison of the two active components extraction process of honeysuckle,alcohol extraction process was better than water extraction and alcohol precipitation process.The extraction effect of chlorogenic acid and luteoloside were both good by alcohol extraction process,the extraction temperature was lower with little damage to the active component,extraction time was short by alcohol extraction process with simpler operation.In this study,through the optimization of volatile oil and active ingredient extraction technology of honeysuckle,which can provide theoretical support for industrialized extraction of honeysuckle,in the same time,the optimized process has important significance to improve the added value of honeysuckle and enhance the core competitiveness of geoherbs in Henan.