CN104189031A - Method for extracting total flavones of hippophae rhamnoides from hippophae rhamnoides leaves - Google Patents
Method for extracting total flavones of hippophae rhamnoides from hippophae rhamnoides leaves Download PDFInfo
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- CN104189031A CN104189031A CN201410445682.7A CN201410445682A CN104189031A CN 104189031 A CN104189031 A CN 104189031A CN 201410445682 A CN201410445682 A CN 201410445682A CN 104189031 A CN104189031 A CN 104189031A
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Abstract
The invention relates to a method for extracting total flavones of hippophae rhamnoides from hippophae rhamnoides leaves, and particularly relates to a method for extracting total flavones of hippophae rhamnoides by means of synergy of enzyme fermentation and continuous counterflow ultrasound. The method comprises the following steps: a, baking and grinding the hippophae rhamnoides leaves at 60 DEG C, and screening by a 40-mesh screen; b, fermenting by biological enzyme; c, performing continuous counterflow ultrasound assisted extraction; d, passing through a polyamide resin column, eluting by ethanol, collecting eluent, concentrating and drying to obtain the total flavones of hippophae rhamnoides. According to the method, the hippophae rhamnoides leaves are used as raw materials, and the overlaid effect of biological enzyme fermentation and ultrasound is sufficiently used, so that the solubility of total flavones of hippophae rhamnoides can be improved. The method has the advantages of simple process, short extracting time, mild reaction condition and the like, is environmentally friendly, is capable of protecting bioactivity of the total flavones of hippophae rhamnoides from damage, and is easy to realize industrial production.
Description
Technical field
The present invention relates to a kind of method of extracting Fructus Hippophae total flavones from Folium Hippophae, relate in particular to the method for the collaborative continuous flow upstream ultrasonic extraction Fructus Hippophae total flavones of a kind of enzyme fermentation.
Background technology
Fructus Hippophae is a kind of wild acinus plant of Elaeangnaceae Hippophae, has another name called vinegar willow, Fructus Elaeagni Angustifoliae, black thorn, is that the preciousness of generally acknowledging in the world eats and medicinal plants.Research shows, the study on flavonoids in sea buckthorn content of high altitude localities is higher, in leaf, flavone compound mainly exists with the form of glycosides, mainly contain 4 kinds of aglycons such as isorhamnetin, Quercetin, kaempferol and ampelopsin and glycosides compound thereof, there is anti-myocardial ischemina, arrhythmia, reduction serum cholesterol and strengthen the pharmacological actions widely such as immunity.
Flavone is as the main active component of Fructus Hippophae, and common extracting method is as follows: steam distillation, organic solvent extractionprocess, supercritical carbon dioxide extraction method, molecular imprinting technique etc.All there is many deficiencies in these methods; Although steam distillation equipment is simple, cost is low and to environment and mankind's nonhazardous and suitability for industrialized is produced, extraction ratio is low, impurity content is higher, is therefore seldom utilized by people now; Organic solvent extractionprocess cost is higher, has dissolvent residual effect, and the mankind and environment are had to certain influence; Supercritical carbon dioxide extraction method is a new separation, extractive technique, have extract at low temperature, without poisonous residual molten and can Selective Separation etc. feature, but it is for the extraction of Fructus Hippophae flavone, raw material will be processed through early stages such as defat and the depigmentations, and testing process is also more numerous and diverse; Molecular imprinting technique is a kind of new technique just growing up recently, can prepare the MIP that Quercetin is template, carry out extracting flavone experiment from Fructus Hippophae primary extract, experimental result shows that the MIP taking Quercetin as template can extract Quercetin and isorhamnetin effectively from Fructus Hippophae primary extract, but this method cost is too high, process is loaded down with trivial details, now also in the laboratory stage of fumbling.
By literature search, have no and adopt ultrasonic the combining of enzyme fermentation and continuous flow upstream to extract the bibliographical information of Fructus Hippophae total flavones.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, a kind of method of extracting Fructus Hippophae total flavones from Folium Hippophae is provided, the method has the advantages such as technique is simple, easy to operate, extraction time is short, extraction ratio is high, environmentally friendly.
The present invention includes following steps:
A. Folium Hippophae, in 60 DEG C of oven dry, pulverizing, is crossed 40 mesh sieves;
B. to the enzyme that adds raw material weight 1 ~ 2% in above-mentioned raw materials, stir, then spray the buffer solution of the citric acid/sodium citrate of pH4.0 ~ 5.0, raw material is reached hold agglomerating, in 40 ~ 50 DEG C of fermentations 5 ~ 7 days;
C. the raw material fermenting is placed in to the continuous flow upstream ultrasonic extractor that frequency is 40kHz, adds 60 ~ 80% the alcoholic solution of 5 ~ 7 times, temperature control, at 45 ~ 60 DEG C, extracts 90 ~ 120min, filters, and obtains filtrate;
D. the filtrate in step c is concentrated into without alcohol taste, proceeding to blade diameter length ratio is that 1:4 ~ 8, particle diameter are 80 ~ 100 object polyamide resin columns, first removes impurity with distilled water eluting, use afterwards 60 ~ 80% the ethanol elution of 4 ~ 8BV, collect eluent, concentrating under reduced pressure, be dried to constant weight, obtain Fructus Hippophae total flavones.
Enzyme described in step b is the cellulase of weight ratio 0.7:0.3 and the mixture of pectase, and the unit of activity of enzyme is 5000U/g.
The present invention compared with prior art, has the following advantages:
(1) general flavone content and yield are higher: the present invention adopts fermented by biological enzyme, the compact texture of destroying cell wall, in conjunction with hyperacoustic cavitation, makes effective ingredient stripping to greatest extent, improve the extraction ratio of total flavones, can realize and working continuously by continuous flow upstream;
(2) the present invention adopts polyamide to carry out separation and purification, and this resin recycling rate of waterused is high, and low price, is applicable to commercial production.
Further illustrate the present invention below in conjunction with detailed description of the invention, but the scope of protection of present invention is not limited to following embodiment.
detailed description of the invention:
Embodiment 1:
Folium Hippophae is in 60 DEG C of oven dry, pulverizing, cross 40 mesh sieves, get 100g powder, (weight ratio is 0.7:0.3 to add the cellulase of raw material weight 1% and pectase, the unit of activity of enzyme is 5000U/g) mixed enzyme, stir, then spray the buffer solution of the citric acid/sodium citrate of pH4.0, raw material is reached hold agglomerating, in 40 DEG C of fermentations 5 days; The raw material fermenting is placed in to the continuous flow upstream ultrasonic extractor that frequency is 40kHz, adds 60% the alcoholic solution of 5 times, temperature control, at 45 DEG C, extracts 90min, filters, and obtains filtrate; Filtrate is concentrated into without alcohol taste, proceeding to blade diameter length ratio is that 1:4, particle diameter are 80 object polyamide resin columns, first remove impurity with distilled water eluting, use afterwards 60% the ethanol elution of 4BV, collect eluent, concentrating under reduced pressure, be dried to constant weight, obtain Fructus Hippophae total flavones extract 1.85g, detect through UV, general flavone content is 51.2%.
Embodiment 2:
Folium Hippophae is in 60 DEG C of oven dry, pulverizing, cross 40 mesh sieves, get 100g powder, add the mixed enzyme of cellulase and the pectase (weight ratio is 0.7:0.3, and the unit of activity of enzyme is 5000U/g) of raw material weight 1.5%, stir, spray again the buffer solution of the citric acid/sodium citrate of pH4.5, raw material is reached hold agglomerating, in 45 DEG C of fermentations 7 days; The raw material fermenting is placed in to the continuous flow upstream ultrasonic extractor that frequency is 40kHz, adds 70% the alcoholic solution of 6 times, temperature control, at 50 DEG C, extracts 100min, filters, and obtains filtrate; Filtrate is concentrated into without alcohol taste, proceeding to blade diameter length ratio is that 1:6, particle diameter are 100 object polyamide resin columns, first remove impurity with distilled water eluting, use afterwards 70% the ethanol elution of 6BV, collect eluent, concentrating under reduced pressure, be dried to constant weight, obtain Fructus Hippophae total flavones extract 1.78g, detect through UV, general flavone content is 55.6%.
Embodiment 3:
Folium Hippophae is in 60 DEG C of oven dry, pulverizing, cross 40 mesh sieves, get 100g powder, add the mixed enzyme of cellulase and the pectase (weight ratio is 0.7:0.3, and the unit of activity of enzyme is 5000U/g) of raw material weight 2%, stir, spray again the buffer solution of the citric acid/sodium citrate of pH5.0, raw material is reached hold agglomerating, in 50 DEG C of fermentations 6 days; The raw material fermenting is placed in to the continuous flow upstream ultrasonic extractor that frequency is 40kHz, adds 80% the alcoholic solution of 7 times, temperature control, at 60 DEG C, extracts 100min, filters, and obtains filtrate; Filtrate is concentrated into without alcohol taste, proceeding to blade diameter length ratio is that 1:8, particle diameter are 90 object polyamide resin columns, first remove impurity with distilled water eluting, use afterwards 80% the ethanol elution of 8BV, collect eluent, concentrating under reduced pressure, be dried to constant weight, obtain Fructus Hippophae total flavones extract 1.96g, detect through UV, general flavone content is 48.1%.
Claims (2)
1. a method of extracting Fructus Hippophae total flavones from Folium Hippophae, is characterized in that, comprises the following steps:
A. Folium Hippophae, in 60 DEG C of oven dry, pulverizing, is crossed 40 mesh sieves;
B. to the enzyme that adds raw material weight 1 ~ 2% in above-mentioned raw materials, stir, then spray the buffer solution of the citric acid/sodium citrate of pH4.0 ~ 5.0, raw material is reached hold agglomerating, in 40 ~ 50 DEG C of fermentations 5 ~ 7 days;
C. the raw material fermenting is placed in to the continuous flow upstream ultrasonic extractor that frequency is 40kHz, adds 60 ~ 80% the alcoholic solution of 5 ~ 7 times, temperature control, at 45 ~ 60 DEG C, extracts 90 ~ 120min, filters, and obtains filtrate;
D. the filtrate in step c is concentrated into without alcohol taste, proceeding to blade diameter length ratio is that 1:4 ~ 8, particle diameter are 80 ~ 100 object polyamide resin columns, first removes impurity with distilled water eluting, use afterwards 60 ~ 80% the ethanol elution of 4 ~ 8BV, collect eluent, concentrating under reduced pressure, be dried to constant weight, obtain Fructus Hippophae total flavones.
2. a kind of method of extracting Fructus Hippophae total flavones from Folium Hippophae according to claim 1, is characterized in that, the enzyme described in step b is the cellulase of weight ratio 0.7:0.3 and the mixture of pectase, and the unit of activity of enzyme is 5000U/g.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104663956A (en) * | 2015-02-02 | 2015-06-03 | 吉木萨尔县生产力促进中心(有限公司) | Preparation method of frozen-dried quick-dissolving tea powder with red flowers and sea buckthorn |
| CN104857108A (en) * | 2015-06-01 | 2015-08-26 | 湖北中烟工业有限责任公司 | Method for preparing hawthorn extractive through continuous countercurrent ultrasonic equipment |
| CN104974851A (en) * | 2015-07-06 | 2015-10-14 | 湖北中烟工业有限责任公司 | Preparation method for black plum extract for cigarette |
| CN105748590A (en) * | 2015-04-01 | 2016-07-13 | 司红康 | Method for extracting total flavonoids compounds from fruits of Ficus erecta |
| CN108244295A (en) * | 2018-03-23 | 2018-07-06 | 青海康普生物科技股份有限公司 | A kind of preparation method of sea-buckthorn Fu tea |
| CN115054620A (en) * | 2022-03-24 | 2022-09-16 | 石河子大学 | Method for extracting flavones from seabuckthorn leaves by using cellulase-ultrasonic cavitation assistance |
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2014
- 2014-09-04 CN CN201410445682.7A patent/CN104189031A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104663956A (en) * | 2015-02-02 | 2015-06-03 | 吉木萨尔县生产力促进中心(有限公司) | Preparation method of frozen-dried quick-dissolving tea powder with red flowers and sea buckthorn |
| CN104663956B (en) * | 2015-02-02 | 2018-04-03 | 吉木萨尔县生产力促进中心(有限公司) | Safflower seabuckthorn freeze-dried instant tea powder |
| CN105748590A (en) * | 2015-04-01 | 2016-07-13 | 司红康 | Method for extracting total flavonoids compounds from fruits of Ficus erecta |
| CN104857108A (en) * | 2015-06-01 | 2015-08-26 | 湖北中烟工业有限责任公司 | Method for preparing hawthorn extractive through continuous countercurrent ultrasonic equipment |
| CN104974851A (en) * | 2015-07-06 | 2015-10-14 | 湖北中烟工业有限责任公司 | Preparation method for black plum extract for cigarette |
| CN104974851B (en) * | 2015-07-06 | 2018-06-08 | 湖北中烟工业有限责任公司 | A kind of preparation method of black cloth woods cigarette extract |
| CN108244295A (en) * | 2018-03-23 | 2018-07-06 | 青海康普生物科技股份有限公司 | A kind of preparation method of sea-buckthorn Fu tea |
| CN115054620A (en) * | 2022-03-24 | 2022-09-16 | 石河子大学 | Method for extracting flavones from seabuckthorn leaves by using cellulase-ultrasonic cavitation assistance |
| CN115054620B (en) * | 2022-03-24 | 2023-09-01 | 石河子大学 | Method for extracting sea buckthorn leaf flavonoid with assistance of cellulase-ultrasonic cavitation |
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Application publication date: 20141210 |