CN104523777A - Biebersteinia heterostemon total flavone extract as well as extraction method and application thereof - Google Patents
Biebersteinia heterostemon total flavone extract as well as extraction method and application thereof Download PDFInfo
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Abstract
The invention discloses a biebersteinia heterostemon total flavone extract as well as an extraction method and an application thereof. The extraction method comprises the following steps: mixing biebersteinia heterostemon raw material powder with a solvent and carrying out solid-liquid separation after Soxhlet extraction to obtain a filtrate A; concentrating to dry the filtrate A to obtain the biebersteinia heterostemon total flavone extract, wherein the time of the Soxhlet extraction is 2-24h; the solvent is an organic solvent or a mixed solvent of the organic solvent and water; in the mixed solvent of the organic solvent and water, the percent by volume of the organic solvent is above 40%; the organic solvent is one or more of alcohols solvent, chlorinated hydrocarbon solvent, esters solvent and alkanes solvent; the volume mass ratio of the solvent to the biebersteinia heterostemon raw material powder is 1-60mL/g. The extraction method provided by the invention is high in extraction rate, good in antibacterial ability of the total flavone extract, simple to operate and good in equipment universality, recyclable in extraction solvent, low in production cost and more suitable for industrial production.
Description
Technical field
The present invention relates to one and smoke the extractive of general flavone of falling cattle, its extracting method and purposes.
Background technology
Flavonoid substances is extensively present in plant kingdom, and it can be divided into the polytypes such as flavonoid, osajin, flavonols, chalcones.The solvent that dissimilar flavone dissolves also has difference.Such as Radix Scutellariae, the flavone compound therefrom separated has baicalin (containing 4.0%-5.2%), baicalin, wogonoside, wogonin.Wherein baicalin is principle active component, has antibacterial, antiinflammation; In addition, it also has the effect of transaminase lowering.The aglycon of baicalin is baicalin, and the phosphoric acid ester sodium of baicalin can be used for diseases such as treating allergy, pant.Baicalin is water-soluble hardly, is insoluble in methanol, ethanol and acetone equal solvent, dissolves in hot acetic acid.Therefore, in the prior art, baicalin available water decocts and extracts with the way of Acid precipitation.Such as Radix Puerariae again, its flavones ingredient contained is mainly soybean isoflavone, uses alumina column chromatography separation method when being separated Radix Puerariae total flavones.
Smoking down cattle (Biebersteinia heterostem on Maxim) is 1 year raw herbaceous plant, there is strong bad smell, among the people also known as smelly Pericarpium Zanthoxyli, wolf tail, be the plant that Flos Rosae Multiflorae guiding principle Mang cattle Seedling subclass Biebersteiniaceae (Biebersteiniaceae) smokes down Bos.
Smoke down cattle and be mainly distributed in Tibet, Qinghai, the areas such as Gansu, Sichuan, Xinjiang, in the grassland of height above sea level 1000 ~ 3200 meters and river shoal visible.Smoke down cattle and have very high medical value, its acrid in the mouth, hardship, cold in nature, have anti-inflammatory analgetic, heat-clearing and toxic substances removing, clearing away heat from blood, the effect of the poison that dispels the wind, has pharmacologically active widely." Tibetan medicine smokes down the active substance research of cattle " (Acta Pharmaceutica Sinica, nineteen ninety-five; 30 (3): 211-214) had in report and smoked down in cattle containing suitable flavones ingredient.Flavone compound has antiviral, antitumor, heart tonifying, blood pressure lowering, coronary artery dilator reduce cholesterol, diuresis, eliminating phlegm and stopping cough, the effect such as to protect the liver.By retrieving domestic and international related data, not yet find with ethanol to be extract so far, the technique total flavones smoking down cattle extracted with soxhlet extraction, and it is preparing the correlational study and report applied in antibacterial medicines.
Summary of the invention
Technical problem to be solved by this invention is to fill up the blank not smoking the total flavone extracting process of falling cattle in prior art, and provides one to smoke the extractive of general flavone of falling cattle, its extracting method and purposes.The extraction ratio that the present invention smokes the extracting method of the total flavones of falling cattle is high, and the extractive of general flavone antibacterial ability extracted is good, and this extracting method is simple to operate simultaneously, and equipment interoperability is good, and Extraction solvent can be recycled, and production cost is low, is more suitable for suitability for industrialized production.
The present invention solves the problems of the technologies described above mainly through following technical scheme.
The invention provides a kind of extracting method smoking the extractive of general flavone of falling cattle, it comprises the following steps: to mix smoking the material powder of falling cattle with solvent, and solid-liquid separation after surname extraction, obtains filtrate A; Described filtrate A is concentrated into dry, must the extractive of general flavone of falling cattle be smoked; Wherein, the time of described surname extraction is 2h ~ 24h; Described solvent is the mixed solvent of organic solvent or organic solvent and water; In described organic solvent and the mixed solvent of water, the percent by volume of organic solvent is more than 40%; Described organic solvent is one or more in alcohols solvent, chlorinated hydrocarbon solvent, esters solvent and alkane solvents; Described solvent compares for 1mL/g ~ 60mL/g with the volume mass smoking the material powder of falling cattle.
The time of described surname extraction is preferably 2h ~ 8h; Be more preferably 2h ~ 6h.The temperature of described surname extraction is generally solvent reflux temperature, is preferably 40 DEG C ~ 100 DEG C; It is more preferably 70 DEG C ~ 80 DEG C.
Described organic solvent is preferably one or more in alcohols solvent and/or esters solvent.Described alcohols solvent is preferably methanol and/or ethanol.Described chlorinated hydrocarbon solvent is preferably dichloromethane and/or chloroform.Described esters solvent is preferably ethyl acetate.Described alkane solvents is preferably petroleum ether and/or normal hexane.In described organic solvent and the mixed solvent of water, the percent by volume of organic solvent is preferably 65% ~ 75%.Described organic solvent and the mixed solvent of water are preferably ethanol water.Described solvent is preferably 10mL/g ~ 40mL/g with the volume mass ratio smoking the material powder of falling cattle; Be more preferably 20mL/g ~ 40mL/g.
Described smoke in the material powder of falling cattle smoke that the raw material of falling cattle can be in root, stem, leaf, flower and the fruit smoking down cattle one or more, preferably for smoking the stem of falling cattle.In the present invention, described smokes the stem of falling cattle for gather voluntarily, and collecting location is Tianzhu Zang Autonomous County, Gansu Province, and acquisition time is annual late August; Also can buy in Tianzhu Zang Autonomous County, Gansu Province and obtain (commercially).
Described smokes the material powder of falling cattle before use, can carry out dried according to the method for this area routine.The method of described drying can be this area and can be the dry conventional method of this area Chinese drugs powder, is preferably vacuum drying.Described vacuum drying method is preferably for adopting the vacuum dryer of this area routine to carry out drying.Wherein, described vacuum drying temperature is preferably 20 DEG C ~ 65 DEG C.Described vacuum drying vacuum is preferably 20kPa ~ 65kPa.
The described grain diameter smoking the material powder of falling cattle can be the grain diameter of this area Chinese drugs powder routine, is preferably 24 ~ 150 orders, is more preferably 50 ~ 120 orders.
The described preparation method smoking the material powder of falling cattle can be the preparation method of this area Chinese drugs powder routine, preferably pulverize for adopting the Chinese medicine grinder of this area routine will smoke the raw material of falling cattle, cross 24 ~ 150 mesh sieves, preferably cross 50 ~ 120 mesh sieves.Described smokes the raw material of falling cattle before pulverizing, preferably through cleaning, re-uses under natural conditions after drying.
The method of described solid-liquid separation can be the method for this area solid-liquid separation routine, as long as can make filtrate A and smoke the residue of falling cattle and separate; The aperture of the filter membrane used in described solid-liquid separation is preferably 0.22 ~ 10 μm.
Described filtrate A is concentrated into the concentrated method described in doing and can be the method that this area filtrate concentrates routine, is preferably distilling under reduced pressure.The temperature of described distilling under reduced pressure is preferably 30 DEG C ~ 80 DEG C.The vacuum of described distilling under reduced pressure is preferably 0 ~ 50kPa.
Described filtrate A is concentrated into the Ethylene recov after doing, in all right recovery to lower batch of extraction process.
The described extracting method smoking the extractive of general flavone of falling cattle also can comprise refining operation further.Described refining method can be the process for purification of this area routine, preferably comprise the following steps: described to smoke the extractive of general flavone of falling cattle, after organic solvent or water extraction, obtain organic facies, organic facies is concentrated into dry, the extractive of general flavone of falling cattle product must be smoked.Wherein, described organic solvent is one or more in chlorinated hydrocarbon solvent, esters solvent and alkane solvents.Described is concentrated into the method that the concentrated method described in doing can be this area routine by organic facies, be preferably distilling under reduced pressure.The temperature of described distilling under reduced pressure is preferably 30 DEG C ~ 70 DEG C.The vacuum of described distilling under reduced pressure is preferably 20kPa ~ 60kPa.
Present invention also offers a kind of obtained by said extracted method smoke the extractive of general flavone of falling cattle.
Present invention also offers the described extractive of general flavone of falling cattle that smokes and prepare the application in antibacterials.
Described antibacterials are preferably medicament for resisting gram-positive bacteria.Described gram positive bacteria is preferably escherichia coli.
Without prejudice to the field on the basis of common sense, above-mentioned each optimum condition, can combination in any, obtains the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material are all commercially.
Positive progressive effect of the present invention is:
The extraction ratio that the present invention smokes the extracting method of the total flavones of falling cattle is high, simple to operate, and equipment interoperability is good, and Extraction solvent can be recycled, and production cost is low, is applicable to suitability for industrialized production.Extract obtain smoke the extractive of general flavone of falling cattle and effectively can suppress the Gram-positive bacteria growings such as escherichia coli, alternative antibiotic, have good application prospect at drug world.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 smokes the anticolibacillary sensitization test result figure of the extractive of general flavone of falling cattle.
Detailed description of the invention
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, conventionally and condition, or selects according to catalogue.
In following embodiment 1 ~ 4, smoke the stem of falling cattle for gather voluntarily, collecting location is Tianzhu Zang Autonomous County, Gansu Province, and acquisition time is annual late August.The general processing procedure smoking the stem of falling cattle is: choose and smoke the stem of falling cattle, cleans and smokes earth on the stem of falling cattle, dry under natural conditions.
In following embodiment 5, smoke the stem of falling cattle and obtain for buying in Tianzhu Zang Autonomous County, Gansu Province.
The quality of the quality/raw material of extraction ratio=total flavones in following embodiment.
Embodiment 1
(1) drying is pulverized: will smoke the stem of falling cattle and put into Chinese medicine grinder pulverizing, and cross 100 mesh sieves, adopt vacuum desiccator at 25 DEG C, under the condition of vacuum 50kPa, drying under reduced pressure obtains smoking the stem of falling cattle material powder.
(2) surname extraction: get the 15 grams of dry stem of falling cattle material powders that smoke in the filter paper cover rolled well, put into the apparatus,Soxhlet's connected, add the ethanol water 300mL that percent by volume is 75%, 80 DEG C are extracted 2 hours, obtain extraction mixed liquor.
(3) solid-liquid separation: after having extracted, with the extraction mixed liquor in filter paper filtering step (2), filter paper lower floor obtains filtrate A, and filter paper upper strata obtains smoking the stem of falling cattle residue.
(4) filtrate A is concentrated into dry: adopt Rotary Evaporators to be 50kPa in vacuum, and under the condition that temperature is 80 DEG C, concentrated filtrate A is to dry, and recovery volume percentage ratio is the ethanol water of 75%, obtains smoking the stem of falling cattle extractive of general flavone.
(5) refining: to adopt extraction into ethyl acetate to smoke the stem of falling cattle extractive of general flavone, obtain ethyl acetate phase.Then adopt Rotary Evaporators to be 40kPa in vacuum, under the condition that temperature is 30 DEG C, concentrated ethyl acetate mutually to dry, and reclaims ethyl acetate, obtains smoking the stem of falling cattle extractive of general flavone product.Extraction ratio is 2.7%.
Embodiment 2
(1) pulverize dry: the stem of falling cattle that smokes cleaned is put into Chinese medicine grinder and pulverized, and cross 50 mesh sieves, employing vacuum desiccator is at 25 DEG C, and under the condition of vacuum 50kPa, drying under reduced pressure obtains smoking the stem of falling cattle material powder.
(2) surname extraction: get the 15 grams of dry stem of falling cattle material powders that smoke in the filter paper cover rolled well, put into the apparatus,Soxhlet's connected, add ethyl acetate 300mL, 75 DEG C are extracted 4 hours, obtain extraction mixed liquor.
(3) solid-liquid separation: after having extracted, with the extraction mixed liquor in filter paper filtering step (2), filter paper lower floor obtains filtrate A, and filter paper upper strata obtains smoking the stem of falling cattle residue.
(4) filtrate A is concentrated into dry: adopt Rotary Evaporators to be 50kPa in vacuum, under the condition that temperature is 40 DEG C, filtrate A is concentrated into dry, and reclaims ethyl acetate, obtains smoking the stem of falling cattle extractive of general flavone.Extraction ratio is 1.8%.
Embodiment 3
(1) drying is pulverized: will smoke the stem of falling cattle and put into Chinese medicine grinder pulverizing, and cross 150 mesh sieves, adopt vacuum desiccator at 25 DEG C, under the condition of vacuum 65kPa, drying under reduced pressure obtains smoking the stem of falling cattle material powder.
(2) surname extraction: surname extraction condition is: get the 15 grams of dry stem of falling cattle material powders that smoke in the filter paper cover rolled well, put into the apparatus,Soxhlet's connected, add normal hexane 300mL, 70 DEG C are extracted 8 hours, obtain extraction mixed liquor.
(3) solid-liquid separation: after having extracted, with the extraction mixed liquor mixed liquor in filter paper filtering step (2), filter paper lower floor obtains filtrate A, and filter paper upper strata obtains smoking the stem of falling cattle residue.
(4) filtrate A is concentrated into dry: adopt Rotary Evaporators to be 5kPa in vacuum, and under the condition of temperature 70 C, concentrated filtrate A to dry, and reclaims normal hexane solvent, obtains smoking the stem of falling cattle extractive of general flavone.
(5) refining: to adopt extraction into ethyl acetate to smoke the stem of falling cattle extractive of general flavone, obtain ethyl acetate phase.Then adopt Rotary Evaporators to be 60kPa in vacuum, under the condition that temperature is 40 DEG C, concentrated ethyl acetate mutually to dry, and reclaims ethyl acetate, obtains smoking the stem of falling cattle extractive of general flavone product.Extraction ratio is 1.3%.
Embodiment 4
(1) pulverize dry: the stem of falling cattle that smokes cleaned is put into Chinese medicine grinder and pulverized, and cross 24 mesh sieves, employing vacuum desiccator is at 60 DEG C, and under the condition of vacuum 20kPa, drying under reduced pressure obtains smoking the stem of falling cattle material powder.
(2) surname extraction: get the 15 grams of dry stem of falling cattle material powders that smoke in the filter paper cover rolled well, put into the apparatus,Soxhlet's connected, add the ethanol water 300mL that percent by volume is 45%, 80 DEG C are extracted 2 hours, obtain extraction mixed liquor.
(3) solid-liquid separation: after having extracted, with the extraction mixed liquor in filter paper filtering step (2), filter paper lower floor obtains filtrate A, and filter paper upper strata obtains smoking the stem of falling cattle residue.
(4) filtrate A is concentrated into dry: adopt Rotary Evaporators to be 30kPa in vacuum, under the condition that temperature is 40 DEG C, filtrate A is concentrated into dry, and recovery volume percentage ratio is the ethanol water of 45%, obtains smoking the stem of falling cattle extractive of general flavone.Extraction ratio is 1.9%.
Embodiment 5
(1) drying is pulverized: will smoke the stem of falling cattle and put into Chinese medicine grinder pulverizing, and cross 100 mesh sieves, adopt vacuum desiccator at 25 DEG C, under the condition of vacuum 50kPa, drying under reduced pressure obtains smoking the stem of falling cattle material powder.
(2) surname extraction: get the 20 grams of dry stem of falling cattle material powders that smoke in the filter paper cover rolled well, put into the apparatus,Soxhlet's connected, add 200 milliliters of chloroform, 75 DEG C are extracted 4 hours, obtain extraction mixed liquor.
(3) solid-liquid separation: after having extracted, with the extraction mixed liquor in filter paper filtering step (2), filter paper lower floor obtains filtrate A, and filter paper upper strata obtains smoking the stem of falling cattle residue.
(4) filtrate A is concentrated into dry: adopt Rotary Evaporators to be 50kPa in vacuum, and under the condition that temperature is 80 DEG C, concentrated filtrate A to dry, and reclaims chloroform soln, obtains smoking the stem of falling cattle extractive of general flavone.
(5) refining: to adopt extraction into ethyl acetate to smoke the stem of falling cattle extractive of general flavone, obtain ethyl acetate phase.Then adopt Rotary Evaporators to be 40kPa in vacuum, under the condition that temperature is 30 DEG C, concentrated ethyl acetate mutually to dry, and reclaims ethyl acetate, obtains smoking the stem of falling cattle extractive of general flavone product.Extraction ratio is 1.3%.
Embodiment 6
(1) drying is pulverized: will smoke the stem of falling cattle and put into Chinese medicine grinder pulverizing, and cross 100 mesh sieves, adopt vacuum desiccator at 25 DEG C, under the condition of vacuum 50kPa, drying under reduced pressure obtains smoking the stem of falling cattle material powder.
(2) surname extraction: get the 15 grams of dry stem of falling cattle material powders that smoke in the filter paper cover rolled well, put into the apparatus,Soxhlet's connected, add the ethanol water 300mL that percent by volume is 75%, 80 DEG C are extracted 24 hours, obtain extraction mixed liquor.
(3) solid-liquid separation: after having extracted, with the extraction mixed liquor in filter paper filtering step (2), filter paper lower floor obtains filtrate A, and filter paper upper strata obtains smoking the stem of falling cattle residue.
(4) filtrate A is concentrated into dry: adopt Rotary Evaporators to be 50kPa in vacuum, and under the condition that temperature is 80 DEG C, concentrated filtrate A is to dry, and recovery volume percentage ratio is the ethanol water of 75%, obtains smoking the stem of falling cattle extractive of general flavone.
(5) refining: to adopt extraction into ethyl acetate to smoke the stem of falling cattle extractive of general flavone, obtain ethyl acetate phase.Then adopt Rotary Evaporators to be 40kPa in vacuum, under the condition that temperature is 30 DEG C, concentrated ethyl acetate mutually to dry, and reclaims ethyl acetate, obtains smoking the stem of falling cattle extractive of general flavone product.Extraction ratio is 2.6%.
Comparative example 1 restricted-access media smokes the total flavones of falling cattle and smokes the extractive of general flavone of falling cattle
The stem of falling cattle will be smoked and place 60 DEG C of oven dry in constant incubator, pulverize.Cross 10 mesh sieves, 70% alcoholic solution and the ratio smoking down cattle are 1:20, and at 35 DEG C, lixiviate 60 minutes, uses 4 layers of filtered through gauze 2 times, obtain filtrate.Filtrate is concentrated into dry, and recovery volume percentage ratio is the ethanol water of 70%, obtains smoking the stem of falling cattle extractive of general flavone I (being called for short JTFI).Extraction ratio is 1.18%.
Comparative example 2 ultrasonic extraction extracts and smokes the total flavones of falling cattle and smoke the extractive of general flavone of falling cattle
To smoke the stem of falling cattle and put into Chinese medicine grinder pulverizing, and cross 100 mesh sieves, adopt vacuum desiccator at 25 DEG C, under the condition of vacuum 50kPa, drying under reduced pressure obtains smoking the stem of falling cattle material powder.Conical flask is put into ultrasonic washing instrument, selects ethanol ultrasonic extraction to smoke the stem of falling cattle total flavones.Ultrasonic extraction conditions is: percent by volume is the ethanol water of 75%, supersound extraction time 55min, and supersound extraction temperature is 35 DEG C, supersound extraction power 600W, ethanol water and smoke the stem of falling cattle powder volume mass ratio 37:1mL/g.After extraction completes, smoke the mixed liquor of the stem of falling cattle powder and alcoholic solution with filter paper filtering, filter paper lower floor obtains filtrate, and filter paper upper strata obtains smoking the stem of falling cattle residue.Adopt Rotary Evaporators to be 50kPa in vacuum, under the condition that temperature is 40 DEG C, concentrated filtrate is to dry, and recovery volume percentage ratio is the ethanol water of 75%, obtains the extract II smoking the stem of falling cattle total flavones.Adopt extraction into ethyl acetate to smoke the crude extract of the stem of falling cattle total flavones, obtain ethyl acetate phase.Then adopt Rotary Evaporators to be 40kPa in vacuum, under the condition that temperature is 30 DEG C, concentrated ethyl acetate mutually to dry, and reclaims ethyl acetate, obtains smoking the stem of falling cattle extractive of general flavone product I I (being called for short CSFII).Extraction ratio is 2.2%.
Effect example antibacterial experiment
(1) preparation of bacterium liquid
Respectively several single bacterium colony on picking LB flat board, is suspended from physiological saline solution, turbula shaker shakes 15s and fully mix, and to correct its turbidity be 0.5 Maxwell, and now Bacteria suspension concentration is 1.5*10
8cFU/mL.
(2) preparation of medicinal liquid
Experimental group: that gets that same volume inventive embodiments 1, comparative example 1 and comparative example 2 obtain smokes the extractive of general flavone of falling cattle and DMSO, is put in EP pipe, makes fully to dissolve mixing both it;
Matched group: the normal saline and the DMSO that get same volume, be put in EP pipe, makes fully to dissolve mixing both it.
(3) drug sensitivity assay
Adopt Oxford cup experiment, draw on certain density indicator bacteria bacteria suspension 0.4mL LB agar plate extremely, even with the coating of aseptic glass rake, and with tweezers, aseptic Oxford cup is put into culture dish gently, in the plate of horizontal positioned, place 4 Oxford cups equably.Draw that the embodiment of the present invention 1 smokes the extract of falling cattle, extraction obtains respectively and smoke the extractive of general flavone of falling cattle (JTFI), ultrasonic extraction obtains smokes the extractive of general flavone of falling cattle (CSFII) and each 0.20mL of DMSO matched group puts into Oxford cup.Above-mentioned Oxford cup is placed in 37 DEG C to cultivate 18 ~ 24 hours, measures antibacterial circle diameter, repeat experiment 3 times, average.
(4) result
Data show, the embodiment of the present invention 1 smoke the extract of falling cattle, what extraction obtained smokes the extractive of general flavone of falling cattle (JTFI), what ultrasonic extraction obtained smokes the extractive of general flavone of falling cattle (CSFII) has inhibitory effect to escherichia coli, and matched group does not produce bacterial restrain, and the inhibition zone diameter 1.71 ± 0.1 centimetres smoking the extract of falling cattle generation of the embodiment of the present invention 1, what be obviously greater than that extraction obtains smokes the extractive of general flavone of falling cattle (JTFI), the diameter 1.01 ± 0.1 centimetres of what ultrasonic extraction obtained the smoke bacterial restrain that the extractive of general flavone of falling cattle (CSFII) produces, specifically see Fig. 1, wherein, 1 obtain for extraction smoke the extractive of general flavone of falling cattle (JTFI), 2 obtain for ultrasonic extraction smoke the extractive of general flavone of falling cattle (CSFII), 3 smoke for the embodiment of the present invention 1 extract of falling cattle, 4 is matched group.There is the above results to find out: of the present inventionly to smoke the alternative antibiotic of the extractive of general flavone of falling cattle, thus overcome the problem that antibiotic causes multi drug resistant bacterial pathogens to produce, have broad application prospects at drug world.
Claims (10)
1. smoke an extracting method for the extractive of general flavone of falling cattle, it is characterized in that, it comprises the following steps: to mix smoking the material powder of falling cattle with solvent, and solid-liquid separation after surname extraction, obtains filtrate A; Described filtrate A is concentrated into dry, must the extractive of general flavone of falling cattle be smoked; Wherein, the time of described surname extraction is 2h ~ 24h; Described solvent is the mixed solvent of organic solvent or organic solvent and water; In described organic solvent and the mixed solvent of water, the percent by volume of organic solvent is more than 40%; Described organic solvent is one or more in alcohols solvent, chlorinated hydrocarbon solvent, esters solvent and alkane solvents; Described solvent compares for 1mL/g ~ 60mL/g with the volume mass smoking the material powder of falling cattle.
2. extracting method as claimed in claim 1, it is characterized in that, the time of described surname extraction is 2h ~ 8h, is preferably 2h ~ 6h; And/or the temperature of described surname extraction is 40 DEG C ~ 100 DEG C; It is preferably 70 DEG C ~ 80 DEG C.
3. extracting method as claimed in claim 1, is characterized in that,
Described alcohols solvent is methanol and/or ethanol;
Described chlorinated hydrocarbon solvent is dichloromethane and/or chloroform;
Described esters solvent is ethyl acetate;
Described alkane solvents is petroleum ether and/or normal hexane;
In described organic solvent and the mixed solvent of water, the percent by volume of organic solvent is 65% ~ 75%;
Described organic solvent and the mixed solvent of water are preferably ethanol water;
And/or described solvent compares for 10mL/g ~ 40mL/g with the volume mass smoking the material powder of falling cattle; Be preferably 20mL/g ~ 40mL/g.
4. extracting method as claimed in claim 1, is characterized in that, described smoke in the material powder of falling cattle smoke the raw material of falling cattle be smoke down in the root of cattle, stem, leaf, flower and fruit one or more, preferably for smoking the stem of falling cattle.
5. extracting method as claimed in claim 1, it is characterized in that, the described material powder of falling cattle that smokes carries out dried before use; The method of described drying is preferably vacuum drying; Wherein, described vacuum drying temperature is preferably 20 DEG C ~ 65 DEG C; Described vacuum drying vacuum is preferably 20kPa ~ 65kPa.
6. extracting method as claimed in claim 1, it is characterized in that, the described grain diameter smoking the material powder of falling cattle is 24 ~ 150 orders, is preferably 50 ~ 120 orders;
And/or the described preparation method smoking the material powder of falling cattle is pulverized for adopting Chinese medicine grinder will smoke the raw material of falling cattle, crosses 24 ~ 150 mesh sieves, preferably crosses 50 ~ 120 mesh sieves.
7. extracting method as claimed in claim 1, it is characterized in that, the aperture of the filter membrane used in described solid-liquid separation is preferably 0.22 ~ 10 μm;
It is distilling under reduced pressure that described filtrate A is concentrated into the concentrated method described in doing; The temperature of described distilling under reduced pressure is preferably 30 DEG C ~ 80 DEG C; The vacuum of described distilling under reduced pressure is preferably 0 ~ 50kPa;
And/or described filtrate A is concentrated into the Ethylene recov after doing, also in further recovery to lower batch of extraction process.
8. extracting method as claimed in claim 1, it is characterized in that, the described extracting method smoking the extractive of general flavone of falling cattle also comprises refining operation further; Described refining method preferably comprises the following steps: described to smoke the extractive of general flavone of falling cattle, after organic solvent or water extraction, obtains organic facies, organic facies is concentrated into dry, must smoke the extractive of general flavone of falling cattle product; Wherein, described organic solvent is one or more in chlorinated hydrocarbon solvent, esters solvent and alkane solvents; The described concentrated method described in doing that organic facies is concentrated into is preferably distilling under reduced pressure; The temperature of described distilling under reduced pressure is preferably 30 DEG C ~ 70 DEG C; The vacuum of described distilling under reduced pressure is preferably 20kPa ~ 60kPa.
9. one kind obtained by the extracting method described in any one of claim 1 ~ 8 smoke the extractive of general flavone of falling cattle.
10. one kind smokes the application of the extractive of general flavone of falling cattle in preparation antibacterials as claimed in claim 9; Described antibacterials are preferably medicament for resisting gram-positive bacteria; Described gram positive bacteria is preferably escherichia coli.
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| CN109045077A (en) * | 2018-08-30 | 2018-12-21 | 青海大学 | The anticancer usage of Heterostemonous Biebersteinia fat-soluble extract |
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