CN101966210B - Folium llicis latifoliae total glycoside and preparation method thereof - Google Patents
Folium llicis latifoliae total glycoside and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a folium llicis latifoliae total glycoside and a preparation method thereof. The folium llicis latifoliae total glycoside is an extract obtained by carrying out ethanol extraction, water sinking and membrane separating purification on leaves of L.purpurascens Y.C.Yang folium llicis latifoliae or/and L.robustum (Roxb) Blume folium llicis latifoliae as raw materials. The preparation method comprises the following steps of: (1) alcohol extraction: pulverizing the leaves of the L.purpurascens Y.C.Yang folium llicis latifoliae or/and L.robustum (Roxb) Blume folium llicis latifoliae, carrying out heating reflux extraction in ethanol and concentrating extract liquid to obtain an extract; (2) water sinking: dissolving the extract into water for many times to obtain supernatant; and carrying out ultrahigh-speed centrifugal processing on the supernatant to obtain a clear transparent solution; (3) ultrafiltration membrane separating purification: filtering the clear transparent solution by an ultrafiltration membrane and collecting membrane penetrating liquid; and (4) nanofiltration membrane separating purification: carrying out nanofiltration membrane separating purification on the membrane penetrating liquid to obtain purified liquid. The folium llicis latifoliae total glycoside of the invention removes inactive components, retains active components, has auxiliary protecting effect on the chemical liver damage, a sobering function and a fat reducing function, has the advantages of good taste, wider application, simple preparation method and convenient operation and can efficiently extract the active components of the folium llicis latifoliae.
Description
Technical field
The invention belongs to the biological medicine technology field, relate to a kind of plant extract and preparation method thereof, relate in particular to a kind of cornutaside and preparation method thereof.
Background technology
Folium Ilicis is Oleaceae Ligustrum Ligustrum robustum L.robustum (Roxb) Blume or Oleaceae Ligustrum purplestem privet leaf (L.purpurascens Y.C.Yang); Be commonly called as tea fourth, Fu Dingcha, highland Lu's tea; Mainly be distributed in ground such as Yunnan, Guizhou, Sichuan; Folium Ilicis is China's tradition medicinal plants, and is with a long history in use among the people.Folium Ilicis has the merit of clearing away heat and cooling blood, nourishing the liver and kidney, has diffusing wind heat, refresh oneself, relieving thirst and restlessness, goes oily effect, and treatment headache, toothache, conjunctival congestion, calentura excessive thirst, dysentery etc. are had obvious effect.But certain alkaloid component in the Folium Ilicis has the bitter cold characteristic, and therefore not being that everybody is suitable drinks Folium Ilicis, has suffered from people, the people of deficiency and coldness body constitution, chronic gastroenteritis patient's unable to drink usefulness of anemofrigid cold, also unsuitable the drinking of menstrual period women and Xin puerpera.And the Folium Ilicis complicated component, its active constituent content is limited, and the use amount during as drug use is bigger, but the Folium Ilicis bitterness is dense, and mouthfeel is bad, should not be accepted.
In order to remove bitter cold material in the Folium Ilicis; Keep its active component; Need adopt methods such as solvent extraction, macroreticular resin absorbing method, solvent precipitation, solvent precipitation, the cholesterol sedimentation method, lead salt precipitation, chromatography as the extraction of active components of plants to carrying out purification processes in the Folium Ilicis more.But there are some defectives in these methods, for example: solvent extraction length consuming time, be prone to emulsion layer, have a strong impact on the effect of extracting and the purity of total glycosides, this method should not be to the processing of a large amount of samples.Macroreticular resin absorbing method: the oils and fats in the plant, lipotropic component or low polarity component are easy to combine with macroporous resin; Be coated with the last layer oil layer at resin surface; And when the solvent elution of macroporous resin is water or hydrophilic solvent; Will reduce the macroporous resin absorption carrying capacity greatly, have a strong impact on separating effect.Solvent precipitation need add the organic solvent of high power amount, and consumption of organic solvent is big, and environment is had pollution, and concentrates comparatively difficulty, and extract purity is also low, also has the organic solvent residual problem.The cholesterol sedimentation method: the molecular complex less stable that cornutaside and sterol form is not suitable for purifying with the cholesterol sedimentation method.Lead salt precipitation: technology is complicated, and deleading technique is difficult, and content of heavy metal lead is high, and product colour is very dark, is difficult to reach food and drug standard requirement.Chromatography: this method and resin method technology are similar, and the defective the same with macroreticular resin absorbing method also arranged, and chromatography is with the too big inferior separating effect of granularity of aluminium oxide in addition, and the too little solvent flow rate of granularity is slow, makes diffusion of bands easily.
Summary of the invention
The technical problem that the present invention will solve is; To dense, oral difficult acceptance of Folium Ilicis bitterness and its active constituent content is low, consumption is big problem, provide a kind of remove invalid components retentive activity compositions such as colloid and cellulose, mouthfeel good, use wider, auxiliary protection function is arranged and has anti-alcohol function and the lectuce tea total glycosides of lipid-reducing function for chemical liver injury.
The technical problem that the present invention further will solve is, provides that a kind of technology is simple, cost is low, can high efficiency extracts the Folium Ilicis active component and the effective lectuce tea total glycosides method for preparing of retentive activity composition, solvent-free pollution.
The technical solution adopted for the present invention to solve the technical problems is: a kind of lectuce tea total glycosides is with the purplestem privet leaf Folium Ilicis or/and the blade of Ligustrum robustum Folium Ilicis is a raw material, the extract that obtains through alcohol extraction, water precipitating, membrane separation purification.
In the lectuce tea total glycosides, described alcohol extraction is: adopting ethanol is that solvent carries out heating extraction at least once to raw material, and concentrated extracting solution gets extractum.
In the lectuce tea total glycosides, described water precipitating is: the extractum that alcohol extraction is obtained centrifuging and taking settled solution after at least once water-soluble.
In the lectuce tea total glycosides, said membrane separation purification is: the settled solution behind water precipitating adopts membrane filtration to get the refined solution of lectuce tea total glycosides.
The method for preparing of lectuce tea total glycosides may further comprise the steps:
(1), alcohol extraction: the purplestem privet leaf Folium Ilicis or/and the blade of Ligustrum robustum Folium Ilicis is pulverized, is added alcohol heating reflux and extracts 1～3 time, filter, merge extractive liquid, concentrates and obtains extractum;
(2), water precipitating: the extractum that alcohol extraction is obtained dissolves in the water, fully leaves standstill after the dissolving, gets supernatant; Repeat to merge supernatant behind the water precipitating 2～4 times; The latter incorporated supernatant of water precipitating is carried out the ultrahigh speed centrifugal treating, and wherein centrifugal rotational speed is 15000～20000 rev/mins, discards precipitate and obtains clear solution;
(3), ultrafilter membrane separation and purification: through ultrafiltration membrance filter, the ultrafilter membrane aperture is 0.001～0.02 micron with the centrifugal clear solution that obtains, and the pressure when wherein filtering is controlled at 0.05～0.15MPa, the collection membrane permeate;
(4), nanofiltration membrane separation purification: the film permeate that step (4) obtains pumps into the nanofiltration membrane separation purification again and obtains refined solution, and wherein the NF membrane aperture comprises 0.001 micron below 0.001 micron.
In the lectuce tea total glycosides method for preparing; The alcohol extraction of said step (1) is: the purplestem privet leaf Folium Ilicis or/and the blade of Ligustrum robustum Folium Ilicis is pulverized, is added the ethanol of 5～10 times of leaf weights, heating and refluxing extraction 1～3 time; The time of each reflux is 1～3 hour; Filter merge extractive liquid,, it is 1.05～1.20 that all extracting solution are concentrated to proportion, obtains extractum;
In the lectuce tea total glycosides method for preparing, the water precipitating of said step (2) is: the extractum that alcohol extraction is obtained is dissolved in the purified water of 5～10 times of weight, fully leaves standstill after the dissolving, gets supernatant, repeats to merge supernatant behind the water precipitating 2～4 times.
In the lectuce tea total glycosides method for preparing, before the alcohol extraction of step (1), also be provided with blade is carried out microwave deactivating enzyme Passivation Treatment step.
In the lectuce tea total glycosides method for preparing, also be provided with afterwards in step (4) refined solution is carried out spray-dired step.
In the lectuce tea total glycosides method for preparing, described spray-dired step is: refined solution is pumped into spray cistern carry out spray drying, obtain the dry powder of lectuce tea total glycosides; Wherein the EAT of spray cistern is 185～205 ℃, and leaving air temp is 80～95 ℃.
Lectuce tea total glycosides of the present invention is with the purplestem privet leaf Folium Ilicis or/and the blade of Ligustrum robustum Folium Ilicis is a raw material, the extract that obtains through alcohol extraction, water precipitating, membrane separation purification.This extract is a mixture; Wherein enrichment the active component in the Folium Ilicis; Its active component mainly comprises: Verbascoside, acteoside isomer, and wherein Verbascoside accounts for about 40% of extract total amount, and the action and efficacy of above-mentioned active component is antioxidation, hepatoprotective, blood fat reducing etc.Total glycosides purity of the present invention is high, and has significantly reduced bitterness, and the mouthfeel silk floss is sweet.Lectuce tea total glycosides of the present invention can also be used to make drug injection and oral liquid except being applied to food, beverage etc., and its clarity is high, and the ability long term storage keeps clarity constant in a year and a half.Removed cold composition in the lectuce tea total glycosides, made Product Safety higher, better adaptability is wider.
Only relate to the second alcohol and water in the method for preparing of the present invention, avoid using other poisonous and harmful solvents, safety is good; The operation of preparation is few, with short production cycle, and conservation has especially been saved feed ethanol, has reduced production cost, and process conditions are less demanding, is easy to realize, helps safety in production.Production efficiency is high, and product purity is high, and decontamination is effective, and has kept active component effectively.Purification of the present invention does not adopt heat to concentrate, and has avoided the glycosidic bond fracture in the active component, has guaranteed that active component such as Verbascoside are not destroyed.The filter membrane that adopts in the method for preparing can use repeatedly, and economic benefit is obvious.Work simplification of the present invention, purification process is simple, easy to operate, separation efficiency is high, the optimum industrialization is produced.
The present invention adopts ultrafilter membrane and NF membrane, and wherein ultrafilter membrane is that a kind of aperture specification unanimity, specified pore diameter range are 0.001～0.02 micron micropore filtering film.Side at film imposes suitable pressure, just can sift out the solute molecule less than the aperture, with the isolated molecule amount greater than 500 dalton, particle diameter granule greater than 2～20 nanometers.NF membrane also is a kind of functional semipermeable membrane, can hold back the material of nanoscale (0.001 micron), and it is held back molecular weight of material and is about about 200-800MW.Therefore can pass through ultrafilter membrane depyrogenation and pathogenic microorganism among the present invention, its removal effect can reach the pharmacopeia requirement, and product is safer.
Description of drawings
Fig. 1 is the preparation flow figure of lectuce tea total glycosides.
The specific embodiment
A kind of lectuce tea total glycosides is with the purplestem privet leaf Folium Ilicis or/and the blade of Ligustrum robustum Folium Ilicis is a raw material, the extract that obtains through alcohol extraction, water precipitating, membrane separation purification.Because lectuce tea total glycosides is a mixture, constituent is comparatively complicated, and therefore, the product that the present invention will obtain--lectuce tea total glycosides is exactly through the material behind the said method extraction purification.
Described alcohol extraction is: adopting ethanol is that solvent carries out heating extraction at least once to raw material, and concentrated extracting solution gets extractum.
Described water precipitating is: the extractum that alcohol extraction is obtained centrifuging and taking settled solution after at least once water-soluble.
Said membrane separation purification is: the settled solution behind water precipitating adopts membrane filtration to get the extract of lectuce tea total glycosides.
Below specify the present invention through a plurality of embodiment.
Embodiment 1: according to preparation flow as shown in Figure 1, the preparation of lectuce tea total glycosides may further comprise the steps:
1. the Folium Ilicis blade of plucking adopted DWIM-20MV8 microwave drying sterilization machine in 12 hours, it is carried out the microwave deactivating enzyme Passivation Treatment, set microwave output power: 15KW, transfer rate: 1m/min, the thickness 5cm of charging leaf, continuous feed.The process of microwave deactivating enzyme Passivation Treatment also is to raw material sterilizing, exsiccant process.
2. Ilex latifolia tea-leaf is pulverized and lixiviate
1) Ilex latifolia tea-leaf is pulverized, and crosses 20 mesh sieves and obtains the Folium Ilicis coarse powder;
2) 50% the edible ethanol that adds 5 times of weight of coarse powder in the above-mentioned coarse powder soaked after 1 hour, and reflux 1 hour is filtered, and medicinal residues add 50% the edible ethanol reflux 1 hour of 5 times of weight of coarse powder again, filter, and merge 2 times ethanol extract, abandon residue;
3) with twice ethanol extract decompression recycling ethanol, and be concentrated to proportion 1.05, obtain extractum.
3. purify
1) extractum is handled: extractum fully is dissolved in the purified water of 5 times of weight, leaves standstill, get supernatant, and subsequent use; Repeat then to merge supernatant behind the water precipitating 3 times, it is centrifugal that the water precipitating supernatant carries out ultrahigh speed, crosses GF-105 type tube centrifuge (north, Liaoyang pharmaceutical machine factory), and 15000 rev/mins of centrifuge speeds obtain clear solution, discard as sedimentary medicinal residues;
2) install ultrafilter membrane, present embodiment is selected polyacrylonitrile filter membrane (model UFbIA160, the aperture is 0.002 μ m) for use, clear filtrating is pumped into, and control operation pressure 0.05MPa, operating temperature is 20 ℃, discards the film stopper, the collection membrane permeate.
3) the film permeate pumps into HNF-90-4040 type NF membrane (aperture is 1nm) again, removes heavy metal and small molecular weight impurity, discards the film stopper, obtains refined solution.
4. concentrate and spray drying treatment
1) refined solution is directly pumped into the spraying head tank;
2) 185 ℃ of control EATs, 85 ℃ of leaving air temps carry out spray drying, control spray velocity, obtain the dry powder of lectuce tea total glycosides.
3) dry powder was pulverized 40 mesh sieves, double-layer plastic bag packing gets the lectuce tea total glycosides powder.
Through detecting, in the present embodiment lectuce tea total glycosides powder, Verbascoside content is 41.38%, acteoside isomer content is 11.65%.
Embodiment 2: the preparation of lectuce tea total glycosides may further comprise the steps:
1. the Folium Ilicis blade of plucking; In 12 hours, adopt DWIM-20MV8 microwave drying sterilization machine to adopt DWIM-20MV8 microwave drying sterilization machine; Blade is carried out the microwave deactivating enzyme Passivation Treatment, set microwave output power: 15KW, transfer rate: 3m/min; The thickness 10cm of charging leaf, continuous feed.The process of microwave deactivating enzyme Passivation Treatment also is to raw material sterilizing, exsiccant process.
2. Ilex latifolia tea-leaf is pulverized and lixiviate
1) Ilex latifolia tea-leaf is pulverized, and crosses 20 mesh sieves and obtains the Folium Ilicis coarse powder;
2) above-mentioned coarse powder 95% the edible ethanol that adds 10.5 times of coarse powder weight soaked after 1 hour, and reflux 3 hours is filtered, and medicinal residues add the edible ethanol reflux 3 hours of 10.5 times of amounts 95% respectively for twice, filter, and merge three times ethanol extract, abandon residue;
3) with three ethanol extract decompression recycling ethanols, and be concentrated to proportion 1.20, obtain extractum.
3. purify
1) extractum is handled: extractum is dissolved in the purified water of 15 times of amounts, leaves standstill, get supernatant, and subsequent use; Repeat to merge supernatant behind the water precipitating 4 times, it is centrifugal to carry out ultrahigh speed, crosses GF-105 type tube centrifuge (north, Liaoyang pharmaceutical machine factory), and 20000 rev/mins of centrifuge speeds obtain clear solution, discard as sedimentary medicinal residues;
2) install ultrafilter membrane, present embodiment is selected the polyacrylonitrile filter membrane for use, and the aperture is 0.001 μ m, clear solution is pumped into, and control operation pressure 0.15MPa, 5 ℃ of operating temperatures, the collection membrane permeate discards the film stopper.
3) the film permeate pumps into NF membrane again, and the NF membrane aperture is 0.1nm, removes heavy metal and small molecular weight impurity, discards the film stopper, obtains refined solution.
4. concentrate and spray drying treatment
1) refined solution is directly pumped into the spraying head tank;
2) 205 ℃ of control EATs, 95 ℃ of leaving air temps carry out spray drying, control spray velocity, make it to obtain the dry powder of lectuce tea total glycosides.
3) dry powder was pulverized 40 mesh sieves, double-layer plastic bag packing gets the lectuce tea total glycosides powder.
Through detecting, in the present embodiment lectuce tea total glycosides powder, Verbascoside content is 42.15%, acteoside isomer content is 12.92%.
Embodiment 3: the preparation of lectuce tea total glycosides may further comprise the steps:
1. the Folium Ilicis blade of plucking adopted DWIM-20MV8 microwave drying sterilization machine to adopt DWIM-20MV8 microwave drying sterilization machine in 12 hours, blade is carried out killing enzyme and inactivation handle; Set microwave output power: 15KW; Transfer rate: 2m/min, the thickness 8cm of charging leaf, continuous feed.The process of microwave deactivating enzyme Passivation Treatment also is to raw material sterilizing, exsiccant process.
2. treated Ilex latifolia tea-leaf is pulverized and lixiviate
1) Ilex latifolia tea-leaf is pulverized, and crosses 20 mesh sieves and obtains the Folium Ilicis coarse powder;
2) 80% of 10 times of weight of above-mentioned coarse powder adding coarse powder edible ethanol soaked after 1 hour, and reflux 2 hours is filtered, and abandons residue;
3) with the ethanol extract decompression recycling ethanol, and be concentrated to proportion 1.10, obtain extractum.
3. purify
1) extractum is handled: extractum is dissolved in the purified water of 10 times of amounts, leaves standstill, get supernatant, and subsequent use; Repeat to merge supernatant behind the water precipitating 2 times, it is centrifugal to carry out ultrahigh speed, crosses GF-105 type tube centrifuge (north, Liaoyang pharmaceutical machine factory), and 18000 rev/mins of centrifuge speeds obtain clear solution, discard as sedimentary medicinal residues;
2) install ultrafilter membrane, present embodiment is selected the polyacrylonitrile filter membrane for use, and the ultrafilter membrane aperture is 0.02 μ m.Clear solution is pumped into, control operation pressure 0.10MPa, 45 ℃ of operating temperatures discard the film stopper, the collection membrane permeate.
3) the film permeate pumps into NF membrane again, and the NF membrane aperture is 0.5nm, removes heavy metal and small molecular weight impurity, discards the film stopper, obtains refined solution.
4. concentrate and spray drying treatment
1) refined solution is directly pumped into the spraying head tank;
2) 195 ℃ of control EATs, 80 ℃ of leaving air temps carry out spray drying, control spray velocity, make it to obtain the dry powder of lectuce tea total glycosides.
3) will pulverize 40 mesh sieves, double-layer plastic bag packing gets the lectuce tea total glycosides powder.
Through detecting, in the present embodiment lectuce tea total glycosides powder, Verbascoside content is 41.88%, acteoside isomer content is 13.17%.
In the foregoing description, can the Folium Ilicis blade not carried out the microwave deactivating enzyme Passivation Treatment, directly with the lixiviate of blade drying and crushing yet.
Also can directly use through the filtering refined solution of NF membrane, not process dry powder.
Lectuce tea total glycosides can be applied to the manufacturing of bitter leaves tea beverage, also can do to process injection or oral agents with medicine material.The contrast test of Folium Ilicis and lectuce tea total glycosides:
One, mouthfeel: 10g Folium Ilicis prophyll 200ml boiled water is brewed; 0.16g lectuce tea total glycosides dry powder adds 200ml water, supply 10 people to drink the result respectively: 10 people think that all lectuce tea total glycosides dry powder beverage delicate fragrance is good to eat; Back sugariness is outstanding; Directly mouthfeel is not good and puckery with Folium Ilicis prophyll bubble too bitter, is difficult to drink one glass.
Two, drink effect:
The test-meal method
10g Folium Ilicis prophyll 200ml boiled water brews, and drinks every day 3 times;
16g lectuce tea total glycosides dry powder adds 200ml water, drinks every day 3 times;
Study subject meets 30 university student volunteers of requirement of experiment through health check-up, and the body weight degree is all above more than 20%, and the own control design is adopted in experiment.
Clinical health check-up:
1, blood test: experimenter red-cell count before and after the experiment, hematochrome, the leukocytic result that measures for twice all in range of normal value, SAIT (ALT), aspartate transaminase (AST), T-CHOL TC, triglyceride TG, high density lipoprotein LDL-C level determination.
2, biochemical indicator is measured: experimenter's each item biochemical indicator is all in normal range before and after the experiment.
3, electrocardiogram, B ultrasonic, Chest X-rays, blood pressure, heart rate: experimenter electrocardiogram before and after the experiment, the fluoroscopy of chest of X line, B ultrasonic (liver, gallbladder, pancreas, spleen, kidney), blood pressure, twice check result of heart rate are all normal.
4, result:
The edible continuously beverage of experimenter is after 2 weeks; Carry out SAIT (ALT), aspartate transaminase (AST), T-CHOL TC, triglyceride TG, high density lipoprotein LDL-C level determination; Result: ALT on average reduces by 20.3%; AST on average reduces by 35.4%, and TC on average reduces 28.4%TG and on average reduces 21.3%LDL-C and on average reduce by 17.2%.Conclusion can think that the present invention's beverage has blood fat reducing and chemical liver injury is had auxiliary protection function.
The experimenter representes: after the edible beverage, drinking amount obviously increases.The edible beverage in drunk back can quicken to sober up.
Claims (7)
1. lectuce tea total glycosides; It is characterized in that; With the purplestem privet leaf Folium Ilicis or/and the blade of Ligustrum robustum Folium Ilicis is a raw material; The extract that obtains through alcohol extraction, water precipitating, ultrafilter membrane separation and purification, nanofiltration membrane separation purification, in this extract enrichment the active component in the Folium Ilicis, its active component mainly comprises: Verbascoside, acteoside isomer; Described alcohol extraction is: the purplestem privet leaf Folium Ilicis or/and the blade of Ligustrum robustum Folium Ilicis is pulverized, is added alcohol heating reflux and extracts 1～3 time, filter, merge extractive liquid, concentrates and obtains extractum; Described water precipitating is: the extractum that alcohol extraction is obtained dissolves in the water, fully leaves standstill after the dissolving, gets supernatant; Repeat to merge supernatant behind the water precipitating 2～4 times; The latter incorporated supernatant of water precipitating is carried out the ultrahigh speed centrifugal treating, and wherein centrifugal rotational speed is 15000～20000 rev/mins, discards precipitate and obtains clear solution; Described ultrafilter membrane separation and purification is: through ultrafiltration membrance filter, the pressure when wherein filtering is controlled at 0.05～0.15MPa with the centrifugal clear solution that obtains, and the ultrafilter membrane aperture is 0.001～0.02 micron, the collection membrane permeate; Described nanofiltration membrane separation purification is: said film permeate pumps into the nanofiltration membrane separation purification again and obtains refined solution, and wherein the NF membrane aperture is below 0.001 micron.
2. the method for preparing of the described lectuce tea total glycosides of claim 1 is characterized in that, may further comprise the steps:
(1), alcohol extraction: the purplestem privet leaf Folium Ilicis or/and the blade of Ligustrum robustum Folium Ilicis is pulverized, is added alcohol heating reflux and extracts 1～3 time, filter, merge extractive liquid, concentrates and obtains extractum;
(2), water precipitating: the extractum that alcohol extraction is obtained dissolves in the water, fully leaves standstill after the dissolving, gets supernatant; Repeat to merge supernatant behind the water precipitating 2～4 times; The latter incorporated supernatant of water precipitating is carried out the ultrahigh speed centrifugal treating, and wherein centrifugal rotational speed is 15000～20000 rev/mins, discards precipitate and obtains clear solution;
(3), ultrafilter membrane separation and purification: through ultrafiltration membrance filter, the pressure when wherein filtering is controlled at 0.05～0.15MPa with the centrifugal clear solution that obtains, and the ultrafilter membrane aperture is 0.001～0.02 micron, the collection membrane permeate;
(4), nanofiltration membrane separation purification: the film permeate that step (3) obtains pumps into the nanofiltration membrane separation purification again and obtains refined solution, and wherein the NF membrane aperture is below 0.001 micron.
3. the method for preparing of lectuce tea total glycosides according to claim 2 is characterized in that, the alcohol extraction of said step (1) is: with the purplestem privet leaf Folium Ilicis or/and the blade of Ligustrum robustum Folium Ilicis pulverize; The ethanol that adds 5～10 times of leaf weights; Heating and refluxing extraction 1～3 time, the time of each reflux is 1～3 hour, filters merge extractive liquid; It is 1.05～1.20 that all extracting solution are concentrated to proportion, obtains extractum.
4. the method for preparing of lectuce tea total glycosides according to claim 2; It is characterized in that the water precipitating of said step (2) is: the extractum that alcohol extraction is obtained is dissolved in the purified water of 5～10 times of weight, fully leaves standstill after the dissolving; Get supernatant, repeat to merge supernatant behind the water precipitating 2～4 times.
5. according to the method for preparing of any described lectuce tea total glycosides of claim 2～4, it is characterized in that, before the alcohol extraction of step (1), also be provided with blade is carried out microwave deactivating enzyme Passivation Treatment step.
6. according to the method for preparing of any described lectuce tea total glycosides of claim 2～4, it is characterized in that, also be provided with afterwards in step (4) refined solution is carried out spray-dired step.
7. the method for preparing of lectuce tea total glycosides according to claim 6 is characterized in that, described spray-dired step is: refined solution is pumped into spray cistern carry out spray drying, obtain the dry powder of lectuce tea total glycosides; Wherein the EAT of spray cistern is that 185～205 ℃, leaving air temp are 80～95 ℃.
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| CN102670672A (en) * | 2011-03-11 | 2012-09-19 | 中国医学科学院药用植物研究所 | Application of broadleaf holly leaf extract in preparation of medicine for reducing content of triglyceride in liver |
| CN104688828B (en) * | 2015-02-14 | 2018-05-01 | 深圳大学 | The application of the total glycosides induction antiviral cell factor of purplestem privet leaf |
| CN105294788A (en) * | 2015-10-27 | 2016-02-03 | 深圳大学 | Lipase inhibitor, extraction method thereof and application thereof |
| CN107897486A (en) * | 2017-11-20 | 2018-04-13 | 深圳大学 | A kind of chewing gum |
| CN108200838A (en) * | 2017-12-18 | 2018-06-26 | 杨军贤 | A kind of cultivation implantation methods of hardship Sweet tea tree |
| CN111773273A (en) * | 2020-08-14 | 2020-10-16 | 遵义医科大学 | Ligustrum robustum total flavone, preparation method and application |
| CN114766672A (en) * | 2022-05-25 | 2022-07-22 | 贵州泰和现代生态农业科技有限公司 | Old lobular broadleaf holly leaf extract and application thereof in preparing food for relieving alcohol-induced liver injury |
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| CN1508149A (en) * | 2002-12-18 | 2004-06-30 | 中南大学 | Method for extracting total triterpenic acid, ursolic acid and oleanolic acid from Taiwan lectuce herb tea |
| CN101254222A (en) * | 2007-03-02 | 2008-09-03 | 重生源生物科技（深圳）有限公司 | Applications of lectuce tea total glycosides and method of preparing the same |
| CN101361766A (en) * | 2007-08-10 | 2009-02-11 | 贺震旦 | Use of ilexlutifolia thumb total glycosides and preparation method thereof |
| CN101558803A (en) * | 2008-04-16 | 2009-10-21 | 张大卫 | Extracting and purifying method of extract of bitter leaves |
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| CN1508149A (en) * | 2002-12-18 | 2004-06-30 | 中南大学 | Method for extracting total triterpenic acid, ursolic acid and oleanolic acid from Taiwan lectuce herb tea |
| CN101254222A (en) * | 2007-03-02 | 2008-09-03 | 重生源生物科技（深圳）有限公司 | Applications of lectuce tea total glycosides and method of preparing the same |
| CN101361766A (en) * | 2007-08-10 | 2009-02-11 | 贺震旦 | Use of ilexlutifolia thumb total glycosides and preparation method thereof |
| CN101558803A (en) * | 2008-04-16 | 2009-10-21 | 张大卫 | Extracting and purifying method of extract of bitter leaves |
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