CN104083505A - Method for extracting effective component from ethanol part of acid litchi - Google Patents
Method for extracting effective component from ethanol part of acid litchi Download PDFInfo
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- CN104083505A CN104083505A CN201410293286.7A CN201410293286A CN104083505A CN 104083505 A CN104083505 A CN 104083505A CN 201410293286 A CN201410293286 A CN 201410293286A CN 104083505 A CN104083505 A CN 104083505A
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Abstract
The invention discloses a method for extracting an effective component from an ethanol part of acid litchi. The method comprises the following steps: baking and crushing acid litchi, soaking in 95% ethanol for 0.2-0.4 hour, extracting for 80-100 seconds with microwave power of 400-600W, and concentrating to obtain an extract; recovering the ethanol, and dissolving the extract with n-butyl alcohol, filtering, concentrating at reduced pressure to prepare a clear extract, namely the total active component of acid litchi, and recovering the n-butyl alcohol, wherein the acid litchi is acid litchi kernels, acid litchi leaves, acid litchi stems, acid litchi barks and acid litchi fruit peels. The method has the characteristics of simple and effective extraction and purification and high extraction rate; the extract is definite in component and high in purity, and can be used for preparing preparations which have better curative effect and are convenient to take; a solvent for extraction is absolute ethyl alcohol, the step of configuring concentration is cancelled, the time is saved, and the recovered solvent can be used in other aspects. The method is economic, energy-saving and environment-friendly, is advantageous to production performance, and has good economical benefit, social benefit and ecological benefit.
Description
Technical field
The invention belongs to Chinese medicine extraction technical field, relate to the extracting method of a kind of sour Fructus Litchi ethanol position active component.
Background technology
Acid Fructus Litchi is sapindaceous plant acid Fructus Litchi (Litchi Chinensis Sonn) plant, main product is in the ground such as Guangdong, Guangxi, and sweet, the micro-hardship of its nature and flavor, warm in nature, returns liver, kidney channel, there is effect of promoting the circulation of blood eliminating stagnation, cold-dispelling pain-relieving, for " Chinese Pharmacopoeia " many editions records.From Fructus Litchi and Semen Litchi separable go out polysaccharide, total saponins and flavone compound isoreactivity composition, studies have shown that, Fructus Litchi and Semen Litchi and active component thereof are except having blocking synthesis of nitrosamine and removing nitrite ion, antioxidation and removing free radical and suppress HBsAg, outside the biological activity of HBeAg and HBV-DNA etc., also have antiinflammatory, pain relieving, bring down a fever and suppress mice transplanted tumor, to pharmacological actions such as anti-immune and acute liver damage, blood sugar lowering, tune blood fat, antioxidation and enhancing insulin resistant model rat insulin sensitivity.Particularly saponin component has the biological activitys such as antitumor, antibacterial, antiviral, treatment diabetes and cardiovascular disease in Semen Litchi.Experiment and clinical treatment show significantly blood sugar lowering, tune blood fat of Semen Litchi total saponins, effectively treat diabetes and metabolic syndrome.And the feature such as Chinese native medicine security is good, raw material is easy to get, price material benefit, toxic and side effects are little needs long-term prescription with respect to diabetes especially, the total saponins composition blood sugar lowering of developing in sour Fructus Litchi has certain meaning.And to Semen Litchi, known main pharmacodynamics material research still rests on runic thing at present, the confirmation of effective site and purification shortage system and standardization.And still lacking the research of Experiment and clinic presentations aspect sour Fructus Litchi blood sugar lowering, so promote sour Fructus Litchi from simple edible fruits, change into high value added product and Chinese medicine preparation and still need research.Make full use of sour Fructus Litchi, further exploitation treatment diabetes medicament has important social meaning and value, and then improves people's quality of life.So the blood sugar reducing component of developing in sour Fructus Litchi has very large prospect.
The Chinese patent CN200410013168.2 of the applicant National Medical College Of Right Rivers, Chinese medicine preparation and the production method thereof for the treatment of diabetes.It is to be made up of the raw material of following parts by weight: Fructus Citri grandis 5-15, and Fructus Litchi 5-10, Fructus psidii guajavae immaturus-10, Semen Mori 3-8, Fructus Lycii 3-10, described Fructus Litchi is sour Fructus Litchi.Its production stage is:, by sour Fructus Litchi, Fructus Citri grandis sarcocarp, squeeze the juice with juice extractor (1), and fruit juice filters, and heating is concentrated, obtains A liquid; Semen Mori, Fructus Citri grandis, Fructus psidii guajavae immaturus, add water 5 times, heated and boiled water extraction twice, and each 2-3 hour, the heating of water extraction liquid is concentrated, filters, and obtains water extraction liquid B; (2) A liquid is mixed with B liquid, mixed liquor adds 70-95% ethanol precipitation, its volume ratio, and mixed liquor: 70-95% ethanol=1: 3, after mixing, put 4 DEG C of-8 DEG C of standing 16-24 hour, cross elimination precipitation, obtain C liquid; (3) reclaim ethanol.C liquid is placed in the liquor-saturated retracting device of second and reclaims ethanol, and the medicine liquid heating of recovery concentrates to obtain D liquid, gets D liquid, add appropriate syrup and adjuvant, obtain oral liquid, or it is concentrated that D liquid is continued to heating, obtain fluid extract E, spraying is dry, and the powder that gets dry extract, gets dried cream powder F, mix with appropriate amount of auxiliary materials, granule processed, or add appropriate amount of auxiliary materials, the dosage form product of making capsule, tablet, spansule and pharmaceutically can using.The technical problem of this production method is that the active component of sour Fructus Litchi could not effectively extract.
Existing Chinese medicine extraction has the methods such as alcohol reflux, microwave extraction, purification by macroporous resin, and spininess, for certain single active ingredient or position, is removed its unwanted composition.It is with strong points, and effective ingredient is concrete, expends less, does not need to be removed impurity through other technique.Compared with crude drug, its enrichment effective ingredient, not only taking dose is few, effectively acts on specific target position, taking convenience, curative effect are good.And one of characteristic of middle medical drugs is compound recipe medication, be characterized in many target spots, multiple location, multi-level comprehensive function, slowly and not concrete, pharmacological action is unintelligible, corresponding to the corresponding effective component extracting of the concrete state of an illness for curative effect.In acid Semen Litchi, flavone compound has blood sugar lowering, adjusts blood fat, antioxygen, anti-hepatitis virus, the effect such as protects the liver.Total saponins can suppress virus activity blood sugar lowering, tune blood fat and increase insulin sensitivity, and polysaccharide is being brought into play biological action at aspects such as antitumor, antiinflammatory, antiviral, blood sugar lowering, defying age, anticoagulation and immunological enhancement.Carry out Study on extraction by the effective ingredient to clear and definite in Chinese medicine, not only reach distinctive effect in Chinese medicine, and by production, solved the problem of Chinese medicine containing quantity not sufficient, make it more modernization and industrialization.
Summary of the invention
The object of the invention is to the technical problem that will solve for above, provide that a kind of extraction ratio is high, purity is high, the extracting method of the simple sour Fructus Litchi ethanol of technological process position active component.
The present invention is achieved in that
An extracting method for sour Fructus Litchi ethanol position active component, is characterized in that comprising following steps:
(1) dry and pulverize: sour Fructus Litchi medical material is dried according to a conventional method, pulverize 40 orders, obtain sour litchi powder for subsequent use;
(2) microwave extraction: sour litchi powder is added in extractor, then add soak with ethanol, carry out microwave extraction;
(3) extracting solution is concentrated: filter extracting solution, and concentrated, obtain extractum, reclaim ethanol;
(4) purify and concentrate: with water saturated n-butyl alcohol dissolving extractum, cross leaching upper strata liquid, concentrated, make clear paste, obtain sour Fructus Litchi Active principals, reclaim n-butyl alcohol;
(5) get according to a conventional method a certain amount of clear paste and measure the concentration of its active component.
Above-described sour Fructus Litchi is sour Semen Litchi, sour Folium Litchi, sour Fructus Litchi bar, sour Fructus Litchi bark and sour Fructus Litchi.
Above-described active component is mainly total saponins, also contains 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 80-100 second.
Concentrated employing distilling under reduced pressure described in the above step (3) and (4), controlling temperature is 70 DEG C, vacuum is-0.1MPa.
Extractum and clear paste described in the above step (3) and (4) are opened bottle cap, control temperature 70 C in water-bath, evaporate into without alcohol taste.
Method of the present invention, compared with existing extractive technique, has following obvious advantage:
(1) extraction purification of the present invention have simply, efficient, cheap and eco-friendly feature, be beneficial to production.
(2) extraction ratio of the present invention is high, and extract component is clear and definite and purity is high, extracts result stable, can prepare higher curative effect and the preparation of being convenient to take.
(3) extracting solvent used is dehydrated alcohol, has reduced this procedure of configuration concentration, has also solved and has extracted the problem that solvent is difficult for volatilizing, save time, and simultaneously by reclaiming solvent for other side, economy, energy-conservation, be conducive to the carrying out producing.
(4) the present invention is applicable to the extraction of the ethanol position active component at each position of sour 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 examples.
Embodiment 1
Sour Semen Litchi, leaf, bar, bark and peel be dry, pulverize respectively, cross 40 mesh sieves; O.3 hour take respectively 10g and add in different extractors, then add respectively 95% the ethanol of 200ml, stir with Glass rod, soak the bubble time for, carry out microwave extraction, microwave power is 5OOW, and the time is 90 seconds; Filter respectively extracting solution, distilling under reduced pressure, controlling temperature is 70 DEG C, vacuum is-0.1MPa to obtain extractum, recovery ethanol; Respectively extractum is opened to bottle cap, control temperature 70 C in water-bath, volatilization extractum is extremely without alcohol taste; Dissolve extractum with water saturated n-butyl alcohol respectively, cross leaching upper strata liquid, distilling under reduced pressure, controlling temperature is 70 DEG C, vacuum is-0.1MPa to make clear paste, recovery n-butyl alcohol; Respectively clear paste is opened to bottle cap, control temperature 70 C in water-bath, volatilization clear paste, to without alcohol taste, obtains respectively the active component of sour Semen Litchi, leaf, bar, bark and peel.
Sour Fructus Litchi active component is settled to 25mL with dissolve with methanol respectively, shakes up for subsequent use.
Survey absorbance method with vanillin-perchloric acid development process, adopt ginsenoside R
1for the content of total saponins in reference substance working sample.There is maximum absorption band according to ginsenoside's standard substance at 536nm, so select 536nm for measuring wavelength.Standard curve regression equation is Y=-0.05439+0.18484X, coefficient R
2be 0.9956, concentration is at 0.4-17.3mgL
-1in scope, there is good linear relationship.Thereby obtain the absorbance of total saponins.
With aluminum salt colour developing spectrophotometry, adopting rutin is the content of flavone compound in reference substance measuring samples.There is maximum absorption band according to rutin standard substance 505, so select 505 for measuring wavelength.Mark Regression Equations is (Y=-0.00903+0.01231X), and coefficient R is 0.9998, and concentration is 0.7-35.0mgL
-1in scope, there is good linear relationship.Thereby obtain the absorbance of total flavones.
The sour Fructus Litchi total flavones of the present embodiment and total saponin extracts experimental result are in table 1.
Table 1: sour 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
Sour Semen Litchi, leaf, bar, bark and peel be dry, pulverize respectively, cross 40 mesh sieves; O.2 hour take respectively 10g and add in different extractors, then add respectively 95% the ethanol of 200ml, stir with Glass rod, soak the bubble time for, carry out microwave extraction, microwave power is 5OOW, and the time is 80 seconds; Filter extracting solution, distilling under reduced pressure, controlling temperature is 70 DEG C, vacuum is-0.1MPa to obtain extractum, recovery ethanol; Extractum is opened to bottle cap, control temperature 70 C in water-bath, volatilization extractum is extremely without alcohol taste; Dissolve extractum with water saturated n-butyl alcohol respectively, cross leaching upper strata liquid, distilling under reduced pressure, controlling temperature is 70 DEG C, vacuum is-0.1MPa to make clear paste, recovery n-butyl alcohol; Respectively clear paste is opened to bottle cap, control temperature 70 C in water-bath, volatilization clear paste, to without alcohol taste, obtains respectively the active component of sour Semen Litchi, leaf, bar, bark and peel.
Sour Fructus Litchi total flavones and the total saponin extracts experimental technique of the present embodiment operate according to embodiment 1, the results are shown in Table 2.
Table 2: sour 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
Sour Semen Litchi, leaf, bar, bark and peel be dry, pulverize respectively, cross 40 mesh sieves; O.4 hour take respectively 10g and add in different extractors, then add respectively 95% the ethanol of 200ml, stir with Glass rod, soak the bubble time for, carry out microwave extraction, microwave power is 4OOW, and the time is 100 seconds; Filter respectively extracting solution, distilling under reduced pressure, controlling temperature is 70 DEG C, vacuum is-0.1MPa to obtain extractum, recovery ethanol; Respectively extractum is opened to bottle cap, control temperature 70 C in water-bath, volatilization extractum is extremely without alcohol taste; Dissolve extractum with water saturated n-butyl alcohol respectively, cross leaching upper strata liquid, distilling under reduced pressure, controlling temperature is 70 DEG C, vacuum is-0.1MPa to make clear paste, recovery n-butyl alcohol; Clear paste is opened to bottle cap, control temperature 70 C in water-bath, volatilization clear paste, to without alcohol taste, obtains respectively the active component of sour Semen Litchi, leaf, bar, bark and peel.
Sour Fructus Litchi total flavones and the total saponin extracts experimental technique of the present embodiment operate according to embodiment 1, the results are shown in Table 3.
Table 3: sour 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 |
Adopt above-mentioned technique, prepared altogether 3 batches of sour Fructus Litchi active component extracts.
Domestic scholars has also been carried out large quantity research, for example soup build duckweed with 60% ethanol as solvent at microwave power 700w, adopting 150s productive rate is 6.86, and we find sour Fructus Litchi bar and the peel ethanol at 80s95%, soak O.2 hour, then carry out microwave extraction, microwave power is 5OOW, not only energy-conservation but also save time, the extraction ratio of saponin is 1.12%, finds also to contain a large amount of flavone and saponins compound in sour Fructus Litchi bar and peel simultaneously.Wang Yuzhi also adopts similar ethanol leaching technology to extract, and the extraction ratio of saponin is 1.818%.We have reached respectively 2.850% and 2.87% at the extraction ratio of the sour Semen Litchi total saponins that adopts backflow, ultrasonic extraction at this group, apparently higher than common Fructus Litchi.
The people such as Lu Zhike, Li Wei adopts productive rate that the way of backflow extracts also 5.78%～6.80%, and 7.32%.We have not reached 8.768% and 8.14% at the sour Semen Litchi total flavones extraction ratio best result that adopts backflow, ultrasonic extraction at this group, apparently higher than common Fructus Litchi.
The public inscription of refined Zheng of Chen Quan waits people to adopt the way of backflow to extract Folium Litchi and peel, all find that Flavonoid substances has antioxidant activity, but in leaf, general flavone content is lower.This group find sour Folium Litchi, bar, bark and peel adopt the content of its flavone of suitable method and saponin and the content difference of core little, have even higher than core, these discoveries show in this ancient seeds of sour Fructus Litchi, the content of its flavone and saponin is very abundant, its leaf, bar, bark and peel all can be used as the source of natural flavone or saponin, and select these position content of suitable method fine.
Also have volume and weight that important difference is exactly sour Semen Litchi be all sweet Fructus Litchi on common market kinds such as () such as cv. Feizixiaos 2-3 doubly.This experiment found this sour Fructus Litchi also have with common market on some common character of Fructus Litchi, also find that the total flavones in sour Fructus Litchi and the content of total saponins are all apparently higher than common Fructus Litchi in the time adopting same backflow, ultrasonic extracting process to extract simultaneously.
Result shows: through assay, in the sour Fructus Litchi extract that adopts method of the present invention to obtain, all contain greater activity material total flavones and total saponins, total saponins general flavone content difference in the sour Fructus Litchi different parts that employing different process obtains is little, and the total saponin content in sour Fructus Litchi bark is minimum.Total saponin content in acid Fructus Litchi and core is maximum, and the general flavone content in sour Fructus Litchi bark is higher.Under this Optimizing Technical, the extraction ratio of total flavones total saponins is higher, extracts result stable, meet modern extract in industry save time, efficient, energy-conservation requirement.
Simultaneously because the output of Fructus Litchi reaches 1,500,000 tons every year, the waste material core, the peel etc. that produce also probably have 150,000 tons, utilize method of the present invention to turn waste into wealth, by the pressure of alleviation greatly, for diabetes, cancer treatment drugs provide cheap raw material, can be described as the method for doulbe-sides' victory at one stroke simultaneously.
Claims (8)
1. an extracting method for sour Fructus Litchi ethanol position active component, is characterized in that comprising following steps:
(1) dry and pulverize: sour Fructus Litchi medical material is dried according to a conventional method, pulverize 40 orders, obtain sour litchi powder for subsequent use;
(2) microwave extraction: sour litchi powder is added in extractor, then add soak with ethanol, carry out microwave extraction;
(3) extracting solution is concentrated: filter extracting solution, and concentrated, obtain extractum, reclaim ethanol;
(4) purify and concentrate: with water saturated n-butyl alcohol dissolving extractum, cross leaching upper strata liquid, concentrated, make clear paste, obtain sour Fructus Litchi Active principals, reclaim n-butyl alcohol;
(5) get a certain amount of clear paste after standardize solution according to a conventional method and measure the concentration of its active component.
2. the extracting method of a kind of sour Fructus Litchi ethanol according to claim 1 position active component, is characterized in that: described sour Fructus Litchi is sour Semen Litchi, sour Folium Litchi, sour Fructus Litchi bar, sour Fructus Litchi bark and sour Fructus Litchi.
3. the extracting method of a kind of sour Fructus Litchi ethanol according to claim 1 position active component, is characterized in that: described active component is mainly flavonoid, also contains total saponins.
4. the extracting method of a kind of sour Fructus Litchi ethanol according to claim 1 position active component, is characterized in that: the concentration of alcohol described in described step (2) is 95 %.
5. the extracting method of a kind of sour Fructus Litchi ethanol according to claim 1 position active component, is characterized in that: the soak time described in described step (2) is 0.2-0.4 hour.
6. the extracting method of a kind of sour Fructus Litchi ethanol according to claim 1 position active component, is characterized in that: its power of microwave extraction described in described step (2) is 400-600 W, and the time is 80-100 second.
7. the extracting method of a kind of sour Fructus Litchi ethanol according to claim 1 position active component, is characterized in that: the concentrated employing distilling under reduced pressure described in described step (3) and (4), and controlling temperature is 70 DEG C, vacuum is-0.1 MPa.
8. the extracting method of a kind of sour Fructus Litchi ethanol according to claim 1 position active component, is characterized in that: extractum and clear paste described in described step (3) and (4) are opened bottle cap, controls 70 DEG C of temperature in water-bath, evaporates into without alcohol taste.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104740619A (en) * | 2015-03-17 | 2015-07-01 | 华中农业大学 | Inflammation-induced protein component, and preparation method and product thereof |
| CN105943681A (en) * | 2016-04-28 | 2016-09-21 | 广州市中医医院 | Semen litchi steroid saponin extract having function of improving insulin resistance |
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2014
- 2014-06-26 CN CN201410293286.7A patent/CN104083505B/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104740619A (en) * | 2015-03-17 | 2015-07-01 | 华中农业大学 | Inflammation-induced protein component, and preparation method and product thereof |
| CN105943681A (en) * | 2016-04-28 | 2016-09-21 | 广州市中医医院 | Semen litchi steroid saponin extract having function of improving insulin resistance |
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