CN104083505B - A kind of extracting method of acid Fructus Litchi ethanol position active component - Google Patents
A kind of extracting method of acid Fructus Litchi ethanol position active component Download PDFInfo
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Abstract
The invention discloses the extracting method of a kind of acid Fructus Litchi ethanol position active component, comprise step: acid Fructus Litchi is dried and pulverized, and concentration is 95% soak with ethanol O.2 0.4 hour, microwave power 400 6OOW, extract 80 100 seconds, be concentrated to give extractum, reclaim ethanol, use n-Butanol soluble extractum, filter, concentrating under reduced pressure, make clear paste, obtain sour Fructus Litchi Active principals, reclaim n-butyl alcohol；Acid Fructus Litchi is acid Semen Litchi, acid Folium Litchi, acid Fructus Litchi bar, acid Fructus Litchi bark and acid Fructus Litchi.This method extraction purification has simple, efficient, and extraction ratio is high, and extract component is clear and definite and purity is high, can prepare higher curative effect and be easy to the preparation taken；Solvent used by extraction is dehydrated alcohol, decreases this procedure of configuration concentration, saves the time, simultaneously by recycling design for other side, economical, energy-conservation, environmental friendliness, is conducive to the carrying out produced, has preferable economic benefit, social benefit and ecological benefits.
Description
Technical field
The invention belongs to technical field of extraction of Chinese traditional medicine, relate to the extracting method of a kind of acid Fructus Litchi ethanol position active component.
Background technology
Acid Fructus Litchi be sapindaceous plant acid Fructus Litchi (Litchi Chinensis Sonn) plant, main product in the ground such as Guangdong, Guangxi,
Its nature and flavor hardship sweet, micro-, warm in nature, return liver, kidney channel, there is effect of promoting the circulation of blood eliminating stagnation, cold-dispelling pain-relieving, many for " Chinese Pharmacopoeia "
Version is recorded.May separate out polysaccharide, total saponins and flavone compound isoreactivity composition from Fructus Litchi and Semen Litchi, research proves,
Fructus Litchi and Semen Litchi and active component thereof are except having blocking synthesis of nitrosamine and removing nitrite ion, antioxidation and removing freely
Outside the biological activity of base and suppression HBsAg, HBeAg and HBV-DNA etc., also antiinflammatory, pain relieving, bring down a fever and suppress mice to move
Planting property tumor, to anti-immune and acute liver damage, blood sugar lowering, Adjust-blood lipid, antioxidation and enhancing insulin resistant model rat
The pharmacological actions such as insulin sensitivity.Particularly in Semen Litchi, saponin component has antitumor, antibacterial, antiviral, treatment sugar
The biological activitys such as urine disease and cardiovascular disease.Experiment and clinical treatment display Semen Litchi total saponins can significantly blood sugar lowering, Adjust-blood lipid,
Effective treatment diabetes and metabolic syndrome.And the spies such as Chinese native medicine security is good, raw material is easy to get, price material benefit, toxic and side effects is little
Point, needs long-term prescription, the total saponins composition blood sugar lowering in exploitation acid Fructus Litchi to have certain meaning particularly with respect to diabetes.
And at present main pharmacodynamics material research known to Semen Litchi being remained on runic thing, the confirmation of effective site lacks system with purifying
System and standardization.And in terms of acid Fructus Litchi blood sugar lowering, still lack experiment and clinical research, so promote that acid Fructus Litchi is from merely
Edible fruits, change into high value added product and Chinese medicine preparation still need to research.Make full use of acid Fructus Litchi, develop treatment further
Diabetes medicament has important social meaning and value, and then improves the quality of life of people.So the fall in exploitation acid Fructus Litchi
Blood glucose constituents has the biggest prospect.
The Chinese patent CN200410013168.2 of the applicant National Medical College Of Right Rivers, treatment diabetes Chinese medicine preparation and
Production method.It is made up of the raw material of following parts by weight: Fructus Citri grandis 5-15, Fructus Litchi 5-10, Fructus psidii guajavae immaturus-10, Semen Mori 3-8,
Fructus Lycii 3-10, described Fructus Litchi is acid Fructus Litchi.Its production stage is: (1), by acid Fructus Litchi, grapefruit flesh, squeezes the juice with juice extractor,
Fruit juice filters, and heating concentrates, and obtains A liquid；Semen Mori, Fructus Citri grandis, Fructus psidii guajavae immaturus, add water 5 times, and heated and boiled water carries twice, every time
2-3 hour, Aqueous extracts heating concentrated, and filters, obtains Aqueous extracts B；(2) being mixed with B liquid by A liquid, mixed liquor adds 70-95%
Ethanol precipitates, its volume ratio, mixed liquor: 70-95% ethanol=1: 3, after mixing, puts 4 DEG C-8 DEG C standing 16-24 little
Time, cross and filter off precipitation, obtain C liquid；(3) ethanol is reclaimed.Ethanol, the medicinal liquid of recovery is reclaimed in C liquid is placed on the liquor-saturated retracting device of second
Heating is concentrated to give D liquid, takes D liquid, adds appropriate syrup and adjuvant, obtains oral liquid, or D liquid continues heating concentration, must flow leaching
Cream E, is spray-dried, and get dry extract powder, takes dried cream powder F, mixes with appropriate amount of auxiliary materials, granule processed, or adds appropriate amount of auxiliary materials, makes
Capsule, tablet, spansule and pharmaceutically can dosage form product.The activity one-tenth that technical problem is that acid Fructus Litchi of this production method
Divide and could not effectively extract.
Existing Chinese medicine extraction has the methods such as alcohol reflux, microwave extraction, purification by macroporous resin, is directed to certain single effectively more
Composition or position, removed its unwanted composition.It is with strong points, and effective ingredient is concrete, expends few, is not required to through it
Its technique is gone the removal of impurity.Compared with crude drug, it is enriched effective ingredient, and not only taking dose is few, effectively acts on
Specific target position, taking convenience, curative effect are good.And middle medical drugs have one characteristic that polypharmacy, be characterized in Mutiple Targets, many
Position, multi-level comprehensive function, curative effect is slowly and concrete, and pharmacological action is unintelligible, corresponding corresponding according to the concrete state of an illness
Effective component extracting.In acid Semen Litchi, flavone compound has blood sugar lowering, Adjust-blood lipid, antioxygen, anti-hepatitis virus, protects the liver
Effect.Total saponins can suppress virus activity blood sugar lowering, Adjust-blood lipid and increase insulin sensitivity, and polysaccharide is at antitumor, anti-
The aspects such as inflammation, antiviral, blood sugar lowering, defying age, anticoagulation and immunological enhancement play biological action.By to Chinese medicine
In clear and definite effective ingredient carry out Study on extraction, do not only reach distinctive effect in Chinese medicine, and by production, solve
The problem that Chinese medicine content is not enough, is allowed to more to modernize and industrialization.
Summary of the invention
Present invention aims to above to solve the technical problem that, it is provided that a kind of extraction ratio is high, purity is high, technological process
The extracting method of simple acid Fructus Litchi ethanol position active component.
The present invention is achieved in that
The extracting method of a kind of acid Fructus Litchi ethanol position active component, it is characterised in that comprise the steps of
(1) dry pulverizing: dried according to a conventional method by acid Fructus Litchi medical material, pulverize 40 mesh, obtain acid litchi powder standby；
(2) microwave extraction: acid litchi powder is added in extractor, adds soak with ethanol, carry out microwave extraction；
(3) extracting solution concentrates: filter extracting solution, concentrates, and obtains extractum, reclaims ethanol；
(4) concentration is purified: with water saturated n-Butanol soluble extractum, cross leaching upper liquid, concentrate, make clear paste, obtain sour
Fructus Litchi Active principals, reclaims n-butyl alcohol；
(5) take a certain amount of clear paste according to a conventional method and measure the concentration of its active component.
Above-described acid Fructus Litchi is acid Semen Litchi, acid Folium Litchi, acid Fructus Litchi bar, acid Fructus Litchi bark and acid Fructus Litchi.
Above-described active component is mainly total saponins, possibly together with flavonoid.
Concentration of alcohol described in the above step (2) is 95%.
Soak time described in the above step (2) is 0.2-0.4 hour.
Its power of microwave extraction described in the above step (2) is 400-600W, and the time is the 80-100 second.
Concentration described in the above step (3) and (4) uses decompression distillation, and controlling temperature is 70 DEG C, and vacuum is-0.1
MPa。
Extractum described in the above step (3) and (4) and clear paste open bottle cap, control temperature 70 C in water-bath,
Evaporate into without alcohol taste.
The method of the present invention, compared with existing extractive technique, has a following obvious advantage:
(1) extraction purification of the present invention has simple, efficient, cheap and eco-friendly feature, is beneficial to produce.
(2) extraction ratio of the present invention is high, and extract component is clear and definite and purity is high, extracts result stable, it is possible to prepare higher treatment
Imitate and be easy to the preparation taken.
(3) solvent used by extraction is dehydrated alcohol, decreases this procedure of configuration concentration, also solves Extraction solvent and be difficult to wave
Dry problem, saves the time, simultaneously by recycling design for other side, economical, energy-conservation, is conducive to the carrying out produced.
(4) present invention is applicable to the extraction of ethanol position active component at each position of acid Fructus Litchi.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, but the present invention is not limited to following example.
Embodiment 1
Acid Semen Litchi, leaf, bar, bark and peel are separately dried, pulverize, cross 40 mesh sieves；Weigh 10g respectively and add difference
Extractor in, then be separately added into 200ml 95% ethanol, stir with Glass rod, soak the bubble time be the least
Time, carrying out microwave extraction, microwave power is 5OOW, and the time is 90 seconds；Filter extracting solution, decompression distillation respectively, control temperature
Degree is 70 DEG C, and vacuum is-0.1MPa, obtains extractum, reclaims ethanol；Respectively extractum is opened bottle cap, in water-bath
Controlling temperature 70 C, volatilization extractum is to without alcohol taste；Respectively with water saturated n-Butanol soluble extractum, cross leaching upper liquid, subtract
Pressure distillation, controlling temperature is 70 DEG C, and vacuum is-0.1MPa, makes clear paste, reclaims n-butyl alcohol；Respectively clear paste is opened
Bottle cap, controls temperature 70 C in water-bath, and volatilization clear paste, to without alcohol taste, respectively obtains acid Semen Litchi, leaf, bar, bark
Active component with peel.
Acid Fructus Litchi active component is dissolved with methanol respectively and is settled to 25mL, shake up standby.
Survey absorbance method with vanilla root rot development process, use ginsenoside R1Containing of total saponins in sample is measured for reference substance
Amount.Maximum absorption band is had at 536nm, so selecting 536nm for measuring wavelength according to ginsenoside's standard substance.Standard curve
Regression equation is Y=-0.05439+0.18484X, coefficient R2Being 0.9956, concentration is at 0.4-17.3mg L-1In the range of
There is good linear relationship.Thus obtain the absorbance of total saponins.
With aluminium salt colour developing spectrophotometry, using rutin is the content of flavone compound in reference substance measuring samples.According to
Rutin standard substance have maximum absorption band 505, so selecting 505 for measuring wavelength.Mark Regression Equations is
(Y=-0.00903+0.01231X), coefficient R is 0.9998, and concentration is 0.7-35.0mg L-1In the range of have good
Linear relationship.Thus obtain the absorbance of total flavones.
The sour Fructus Litchi total flavones of the present embodiment and total saponin extracts experimental result are shown in Table 1.
Table 1: acid Fructus Litchi total flavones and total saponin extracts experimental result
| Acid Fructus Litchi raw material | Dosage (g) | Total flavones extraction ratio (%) | Total saponins extraction ratio (%) |
| 1 core | 10 | 8.768 | 2.870 |
| 2 leaves | 10 | 3.048 | 1.334 |
| 3 bars | 10 | 5.860 | 2.445 |
| 4 barks | 10 | 4.831 | 1.633 |
| 5 peels | 10 | 2.777 | 0.949 |
Embodiment 2
Acid Semen Litchi, leaf, bar, bark and peel are separately dried, pulverize, cross 40 mesh sieves；Weigh 10g respectively and add difference
Extractor in, then be separately added into 200ml 95% ethanol, stir with Glass rod, soak the bubble time be the least
Time, carrying out microwave extraction, microwave power is 5OOW, and the time is 80 seconds；Filtering extracting solution, decompression distillation, controlling temperature is
70 DEG C, vacuum is-0.1MPa, obtains extractum, reclaims ethanol；Extractum is opened bottle cap, water-bath controls temperature
70 DEG C, volatilization extractum is to without alcohol taste；Respectively with water saturated n-Butanol soluble extractum, cross leaching upper liquid, decompression distillation, control
Temperature processed is 70 DEG C, and vacuum is-0.1MPa, makes clear paste, reclaims n-butyl alcohol；Respectively clear paste is opened bottle cap, at water
Controlling temperature 70 C in bath, volatilization clear paste, to without alcohol taste, respectively obtains acid Semen Litchi, leaf, bar, bark and the work of peel
Property composition.
The sour Fructus Litchi total flavones of the present embodiment and total saponin extracts experimental technique operate according to embodiment 1, the results are shown in Table 2.
Table 2: acid Fructus Litchi total saponin extracts experimental result
| Acid Fructus Litchi raw material | Dosage (g) | Total flavones extraction ratio (%) | Total saponins extraction ratio (%) |
| 1 core | 10 | 0.83 | 0.145 |
| 2 leaves | 10 | 2.73 | 0.167 |
| 3 bars | 10 | 8.14 | 2.85 |
| 4 barks | 10 | 5.14 | 1.694 |
| 5 peels | 10 | 7.51 | 2.239 |
Embodiment 3
Acid Semen Litchi, leaf, bar, bark and peel are separately dried, pulverize, cross 40 mesh sieves；Weigh 10g respectively and add difference
Extractor in, then be separately added into 200ml 95% ethanol, stir with Glass rod, soak the bubble time be the least
Time, carrying out microwave extraction, microwave power is 4OOW, and the time is 100 seconds；Filter extracting solution, decompression distillation respectively, control
Temperature is 70 DEG C, and vacuum is-0.1MPa, obtains extractum, reclaims ethanol；Respectively extractum is opened bottle cap, at water-bath
Middle control temperature 70 C, volatilization extractum is to without alcohol taste；Respectively with water saturated n-Butanol soluble extractum, cross leaching upper liquid,
Decompression distillation, controlling temperature is 70 DEG C, and vacuum is-0.1MPa, makes clear paste, reclaims n-butyl alcohol；Clear paste is opened bottle
Lid, controls temperature 70 C in water-bath, volatilization clear paste to without alcohol taste, respectively obtain sour Semen Litchi, leaf, bar, bark and
The active component of peel.
The sour Fructus Litchi total flavones of the present embodiment and total saponin extracts experimental technique operate according to embodiment 1, the results are shown in Table 3.
Table 3: acid Fructus Litchi total saponin extracts experimental result
| Acid Fructus Litchi raw material | Dosage (g) | Total flavones extraction ratio (%) | Total saponins extraction ratio (%) |
| 1 core | 10 | 3.127 | 0.9209 |
| 2 leaves | 10 | 4.955 | 1.7255 |
| 3 bars | 10 | 4.504 | 1.4482 |
| 4 barks | 10 | 6.75 | 2.2572 |
| 5 peels | 10 | 1.15 | 0.4482 |
Use above-mentioned technique, be prepared for 3 batch acid Fructus Litchi active component extracts altogether.
Domestic scholars has been also carried out numerous studies, and such as soup builds duckweed 60% ethanol as solvent at microwave power 700w, uses
O.2 hour 150s productivity is 6.86, and we have found that acid Fructus Litchi bar and peel, at the ethanol of 80s95%, soak, then enters
Row microwave extraction, microwave power is 5OOW, the most energy-conservation but also save time, and the extraction ratio of saponin is 1.12%, finds acid Fructus Litchi bar simultaneously
With peel also contains substantial amounts of flavone and saponins compound.The ethanol leaching technology that Wang Yuzhi is also adopted by being similar to extracts, saponin
Extraction ratio be 1.818%.We respectively reach at the extraction ratio of the sour Semen Litchi total saponins using backflow, ultrasonic extraction this group
2.850% and 2.87%, hence it is evident that higher than common Fructus Litchi.
Lu Zhike, Li Wei et al. use productivity that the way of backflow extracts also 5.78%～6.80%, and 7.32%.We
This group is using backflow, the sour Semen Litchi total flavones extraction ratio best result of ultrasonic extraction not to reach 8.768% and 8.14%,
Apparently higher than common Fructus Litchi.
Chen Quan refined Zheng public affairs inscription et al. uses the way of backflow to extract Folium Litchi and peel, all finds that Flavonoid substances has antioxidation and lives
Property, but in leaf, general flavone content is relatively low.This group find acid Folium Litchi, bar, bark and peel use its flavone of suitable method and
The content of saponin and the content difference of core are little, the even above core having, and these find to show in acid this ancient seeds of Fructus Litchi,
The content of its flavone and saponin is the abundantest, its leaf, bar, bark and peel all can as natural flavone or the source of saponin,
And select these position content of suitable method fine.
The volume and weight also having important difference acid Semen Litchi exactly is all sweet Fructus Litchi (the such as cv. Feizixiao on common market
Etc. kind) 2-3 times.This experiment is found that this acid Fructus Litchi also has and some common character of the Fructus Litchi on common market,
Simultaneously it has also been found that when using same backflow, ultrasonic extracting process to extract, the total flavones in acid Fructus Litchi and the content of total saponins
Obviously higher than common Fructus Litchi.
Result shows: through assay, adopts in the sour Fructus Litchi extract being obtained by the present invention and all contains greater activity material
Total flavones and total saponins, the total saponins general flavone content difference in the sour Fructus Litchi different parts that employing different process obtains is little, acid
Total saponin content in Fructus Litchi bark is minimum.Total saponin content in acid Fructus Litchi and core is most, total in acid Fructus Litchi bark
Flavones content is higher.Under this Optimizing Technical, the extraction ratio of total flavones total saponins is higher, extracts result stable, meets the modern times and carries
Take in industry save time, efficient, energy-conservation requirement.
Simultaneously because the yield of Fructus Litchi reaches 1,500,000 tons every year, the waste material core of generation, peel etc. the most probably have 150,000 tons, utilize
The method of the present invention turns waste into wealth, and by the pressure of greatly alleviation, provides cheap for diabetes, cancer treatment drugs simultaneously
Raw material, it may be said that be the method for at one stroke doulbe-sides' victory.
Claims (4)
1. the extracting method of a sour Fructus Litchi ethanol position active component, it is characterised in that: comprise the steps of
(1) dry pulverizing: dried according to a conventional method by acid Fructus Litchi medical material, pulverize 40 mesh, obtain acid litchi powder standby；
(2) microwave extraction: acid litchi powder is added in extractor, adds soak with ethanol, carry out microwave extraction；
(3) extracting solution concentrates: filter extracting solution, concentrates, and obtains extractum, reclaims ethanol；
(4) concentration is purified: with water saturated n-Butanol soluble extractum, cross leaching upper liquid, concentrate, make clear paste, obtain sour Fructus Litchi Active principals, reclaim n-butyl alcohol；
(5) take a certain amount of clear paste after constant volume according to a conventional method and measure the concentration of its active component；
Described sour Fructus Litchi is acid Semen Litchi, acid Folium Litchi, acid Fructus Litchi bar, acid Fructus Litchi bark and acid Fructus Litchi；
Concentration of alcohol described in described step (2) is 95 %；
Soak time described in described step (2) is 0.2-0.4 hour；
Its power of microwave extraction described in described step (2) is 400-600 W, and the time is the 80-100 second；
Extractum described in described step (3) and (4) and clear paste open bottle cap, control temperature 70 DEG C, evaporate into without alcohol taste in water-bath.
The extracting method of a kind of acid Fructus Litchi ethanol position the most according to claim 1 active component, it is characterised in that: described active component is mainly flavonoid, possibly together with total saponins.
The extracting method of a kind of acid Fructus Litchi ethanol position the most according to claim 1 active component, it is characterised in that: the concentration described in described step (3) and (4) uses decompression distillation, and controlling temperature is 70 DEG C, and vacuum is-0.1 MPa.
4. the extracting method of a sour Fructus Litchi ethanol position active component, it is characterised in that: comprise the steps of and acid Semen Litchi, leaf, bar, bark and peel are separately dried, pulverize, cross 40 mesh sieves；Weighing 10g respectively to add in different extractors, then be separately added into the ethanol of 95 % of 200 mL, stir with Glass rod, the immersion bubble time is 0.3 hour, carries out microwave extraction, and microwave power is 500 W, and the time is 90 seconds；Filtering extracting solution, decompression distillation respectively, controlling temperature is 70 DEG C, and vacuum is-0.1 MPa, obtains extractum, reclaims ethanol；Respectively extractum being opened bottle cap, control temperature 70 DEG C in water-bath, volatilization extractum is to without alcohol taste；Respectively with water saturated n-Butanol soluble extractum, crossing leaching upper liquid, decompression distillation, controlling temperature is 70 DEG C, and vacuum is-0.1 MPa, makes clear paste, reclaims n-butyl alcohol；Respectively clear paste is opened bottle cap, controlling temperature 70 DEG C in water-bath, volatilization clear paste, to without alcohol taste, respectively obtains acid Semen Litchi, leaf, bar, bark and the active component of peel, acid Fructus Litchi active component is dissolved with methanol respectively and is settled to 25 mL, then measure the concentration of active component.
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