CN102526315A - Preparation method of extracts of effective fractions of lychee seeds - Google Patents
Preparation method of extracts of effective fractions of lychee seeds Download PDFInfo
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Abstract
The invention belongs to the technical field of extraction and purification of traditional Chinese medicines, and particularly relates to a preparation method of extracts of effective fractions of lychee seeds. The method comprises the following steps of: (1) crushing the lychee seed medicinal material, adding ethanol and performing ultrasonic extraction; (2) recycling ethanol from the extract solution and diluting the extract with water, standing still and filtering; (3) adsorbing the filtrate by use of AB-8 macroporous resin, and eluting with water and ethanol later; (4) collecting the ethanol eluent, recycling ethanol and then concentrating to obtain thick paste; and (5) drying the extractum to obtain the extracts of the effective fractions of lychee seed. According to the invention, the extracts of the effective fractions, comprising the total flavones, total saponins and tannins of the lychee seeds are obtained at the same time by use of the sufficient extraction effect of ethanol on the effective components of the lychee seeds and the selection effect of the high-selectivity macroporous resin, and the total content of the total flavones, total saponins and tannins reaches over 70%; the process is simple and stable, and the quality is controllable; and the obtained extracts of the effective fractions of the lychee seeds conform to the requirements of the traditional Chinese medicine theory and the traditional Chinese medicine modernization.
Description
Technical field
The invention belongs to Chinese medicine extraction purification technique field, be specifically related to a kind of Chinese medicine Semen Litchi effective part group preparation method of extract.
Background technology
Semen Litchi (Lychee Seed, Litchi Seed) is the dry mature seed of sapindaceous plant Fructus Litchi (Litchi Chinensis Sonn); Another name Li Ren, litchi nuclear, Dali nuclear; Record in " 2010 editions one one of Chinese pharmacopoeia, warm in nature, sweet in the mouth, little hardship; Has promoting QI to circulate and dispersing the agglomeration of the pathogens, cold relieving pain relieving effect.Compendium of Material Medica record, Semen Litchi " quench the thirst, beneficial people's color, food end excessive thirst " (excessive thirst disease, modern medicine is called diabetes).Research shows that Semen Litchi has blood sugar lowering, blood lipid regulation, raising antioxidation, suppresses the effect of HBsAg.The research of Semen Litchi ingredient is comparatively abundant, and main component has saponin, flavone and anthocyan, phytosterol, tannin and Polyphenols, fatty acid, aminoacid, protein and polysaccharide etc.Experimentation and clinical treatment show Semen Litchi extract significantly blood sugar lowering and blood fat, effectively treat diabetes and metabolism syndrome.Make full use of local abundant Semen Litchi resource; The medicine that is developed to safe and effective, quality controllable treatment diabetes supplies clinical practice; To changing, have great social significance and market value because of life style changes the high trend of diabetes prevalence that causes.
Existing Semen Litchi extraction and purification process has decoction and alcohol sedimentation technique, ethanol extraction-purification by macroporous resin method etc., and spininess is used as impurity to all the other compositions to remove to certain single active ingredient or position, and the extract of its acquisition does not also meet the Chinese medicine theory." effective site " be meant from single medicinal material material or decoction pieces, extract prove effective one type of chemical constituent through animal and clinical trial.Compare with crude drug, its enrichment active substance, not only dose is little, and has improved curative effect.In one of characteristic of medical drugs be the compound recipe medication, the characteristics of Chinese medicine effect are many target spots, multi-section position, multi-level comprehensive function, and corresponding with it working substance basis also should be multicomponent rather than single component.Fructus Litchi and Semen Litchi and effective site thereof have pharmacology and pharmacodynamic actions such as blood sugar lowering, accent blood fat, antioxidation, inhibition virus, antitumor and anti-liver injury.Wherein, flavone compound can suppress virus and antitumor, and total saponins can suppress virus activity and blood sugar lowering, accent blood fat and strengthen insulin sensitivity, and flavonoid, total saponins class and compound of polysaccharide all have antioxidation, and polysaccharide can improve immunologic function.The effective site that derives from the different material medical material is formed compound recipe, and promptly " effective part group " is used for clinically, and not only embody the Chinese medicine characteristic, and improved technology content, also be to realize the modernization of Chinese medicine and international needs.
" technical study of purification with macroreticular resin Semen Litchi total saponins " (Chinese experimental pharmacology of Chinese medical formulae magazine; The 16th the 8th phase of volume; The 22-24 page or leaf; In July, 2010) disclose a kind of method of extracting the Semen Litchi total saponins, extracted yet this method only is directed against this single active ingredient of total saponins, the extract effect of gained is limited." extraction process of total saponins is preferred in the Semen Litchi " (Chinese experimental pharmacology of Chinese medical formulae magazine; The 17th the 12nd phase of volume; The 48-49 page or leaf; In June, 2011) also disclose a kind of extraction of adopting ethanol lixiviate and ultrasonic-assisted extraction method to total saponins in the Semen Litchi, but do not related to the extraction of the part group that contains plurality of active ingredients.CN 102048885A discloses a kind of Semen Litchi saponin extraction process, and it can extract the effective ingredient of Semen Litchi, the Semen Litchi saponin content that extracts up to 85.0%, but same and not mentioned extraction to a plurality of effective part groups.
Summary of the invention
The objective of the invention is to provides the method that a kind of extraction ratio is high, technological process simply prepares Semen Litchi effective site group extract to the above technical problem that will solve.
In order to reach the above object, the invention provides a kind of method for preparing Semen Litchi effective site group extract, may further comprise the steps:
(1) get the Semen Litchi medical material, pulverizing the back is that 1g: 8～10ml adds ethanol according to solid-liquid ratio, soaks after 0.5～1 hour, carries out supersound extraction, and it is subsequent use to obtain extracting solution A;
(2) in medicinal residues, be that 1g: 8～10ml adds ethanol, soak after 0.5～1 hour, carry out supersound extraction, obtain extracting solution B, extracting solution A and extracting solution B merging according to solid-liquid ratio;
(3) extracting solution A that merges and extracting solution B are reclaimed ethanol to there not being the alcohol flavor, use distilled water diluting to being 0.4g/ml in crude drug amount concentration this medicinal liquid then, hold over night is filtered filtrate for later use;
(4) filtrating is through the AB-8 macroporous resin column, and elder generation carries out eluting with the pure water of 3 times of amount of resin then, discards water lotion, again with the active substance on the ethanol elution resin of 5 times of medical material amounts, and collects ethanol elution;
(5) ethanol elution of step (4) being collected reclaims ethanol to there not being the alcohol flavor, continues simmer down to extractum;
(6) with the said extractum evaporate to dryness of step (5), carry out low-temperature vacuum drying again, promptly get the extract of Semen Litchi effective part group.
As a kind of preferred implementation of the present invention, used concentration of alcohol is 70v/v% at least in said step (1), step (2), the step (4).
As a kind of preferred implementation of the present invention, used concentration of alcohol is 70v/v% in said step (1) and the step (2).
As a kind of preferred implementation of the present invention, the used concentration of alcohol of said step (4) is 75v/v%.
As a kind of preferred implementation of the present invention, adopt distilling under reduced pressure to reclaim ethanol in said step (3) and the step (5).
Further, the condition of said distilling under reduced pressure is vacuum-0.1MPa, 75 ℃ of temperature.
As a kind of preferred implementation of the present invention, in the said step (4), the flow velocity of filtrating through the AB-8 macroporous resin column, be per hour 2 times of bed volumes with the flow velocity of pure water eluting and with the flow velocity of ethanol elution.
As a kind of preferred implementation of the present invention, the relative density of the extractum in the said step (5) is 1.01～1.10.
As a kind of preferred implementation of the present invention, in the said step (6) with said extractum water bath method.
Further, the temperature of said water bath method is 100 ℃
As a kind of preferred implementation of the present invention, in the said step (6), vacuum drying condition is vacuum-0.1MPa, drying at room temperature 48 hours.
Through assay, adopt in the Semen Litchi effective site group extract that method of the present invention obtains, total flavones accounts for 20～30%, and total saponins accounts for 18～25%, and tannin accounts for 25～35%, and three's content sum is 63～90%.
Compared with prior art, method of the present invention has following obvious advantage: (1) processing step of the present invention is reasonable in design, and technological process is simple, is convenient to operation; (2) to adopt ethanol be extraction solvent in the present invention, and in conjunction with supersound extraction, extracting solution is used the AB-8 purification by macroporous resin; Can obtain containing the effective site group extract of total flavones, total saponins and tannin simultaneously; Definite ingredients, quality controllable, meet the requirement of the Chinese medicine theory and the modernization of Chinese medicine; (3) the effective part group extraction ratio is high, and it is complete to extract composition; (4) through reclaiming, ethanol and resin all can reuse, and economy, environmental protection can effectively be applied to commercial production.
The specific embodiment
Below in conjunction with specific embodiment the present invention is made further detailed description, but the present invention is not limited to following examples.
Hereinafter, " 5 times of medical material amounts " refer to used ethanol volume with adding crude drug the ratio of weight be 5ml: 1g.Such as the Semen Litchi powder of getting 100g, then need use the ethanol of 500ml to carry out eluting.
Embodiment 1
Semen Litchi is ground into coarse powder.Get 100g Semen Litchi powder, add for the first time the 70v/v% ethanol of 1000ml, soaked after 0.5 hour supersound extraction 1 hour, inclining, it is subsequent use to container extracting solution A.In medicinal residues, continue to add the 70v/v% ethanol of 800ml, soak after 1 hour, supersound extraction 1 hour, inclining extracting solution B, merges extracting itself and the first time extracting solution A that obtains.Extracting solution A that merges and extracting solution B are reclaimed ethanol to there not being the alcohol flavor.The mode that reclaims is preferably distilling under reduced pressure and reclaims (vacuum-0.1MPa, 75 ℃ of temperature).Medicinal liquid behind the recovery ethanol is settled to 250ml with distilled water diluting, and hold over night is filtered filtrate for later use.Filtrating is at first with the AB-8 macroporous resin column (processing method see below) of flow velocity through having handled of 2 times of bed volumes per hour; Carry out eluting with the pure water of 3 times of amount of resin with the flow velocity of 2 times of bed volumes per hour then; Discard water lotion; And then carry out the active substance on the eluting resin with the flow velocity of 2 times of bed volumes per hour, and collect this ethanol elution with the 75v/v% ethanol of 5 times of medical material amounts (being 500ml).Ethanol elution is carried out decompression recycling ethanol to there not being alcohol flavor (vacuum-0.1MPa, 75 ℃ of temperature), continue to be concentrated into relative density and be 1.05 extractum (this relative density refers to the density with respect to water).With extractum water bath method (100 ℃), put into vacuum drying oven low-temperature vacuum drying (vacuum-0.1MPa, drying at room temperature 48 hours), promptly obtain the extract of Semen Litchi effective part group.
Wherein, the processing method of AB-8 macroporous resin is following: get pharmaceutical clean grade AB-8 macroporous resin, wet method is packed in the resin column; Remove the resin of bubbling through the water column; After putting solid carbon dioxide from the lower end, with 95v/v% ethanol drip washing post layer, until leacheate and water mix with 1: 1 volume ratio do not show muddiness till; Use a large amount of pure water rinsing post layers then, do not have the alcohol flavor until effluent and get final product.
The extract of above gained Semen Litchi effective part group is measured through ultraviolet visible spectrophotometry can know the wherein content of relevant composition: general flavone content (referring to account for the mass ratio of total solid substance) is about 21%; Total saponin content (referring to account for the mass ratio of total solid substance) is about 20%, and content of tannin (referring to account for the mass ratio of total solid substance) is about 30%.
Embodiment 2
Semen Litchi is ground into coarse powder.Get 100g Semen Litchi powder, add the 70v/v% ethanol of 800ml for the first time, soak after 1 hour, supersound extraction 1 hour, inclining, it is subsequent use to container extracting solution A.In medicinal residues, continue to add the 70v/v% ethanol of 1000ml, soak after 0.5 hour, supersound extraction 1 hour, inclining extracting solution B, merges extracting itself and the first time extracting solution A that obtains.Extracting solution A that merges and extracting solution B are reclaimed ethanol to there not being the alcohol flavor.The mode that reclaims is preferably distilling under reduced pressure and reclaims (vacuum-0.1MPa, 75 ℃ of temperature).Medicinal liquid behind the recovery ethanol is settled to 250ml with distilled water diluting, and hold over night is filtered filtrate for later use.Filtrating is at first with the AB-8 macroporous resin column of flow velocity through having handled of 2 times of bed volumes per hour; Carry out eluting with the pure water of 3 times of amount of resin with the flow velocity of 2 times of bed volumes per hour then; Discard water lotion; And then carry out the active substance on the eluting resin with the flow velocity of 2 times of bed volumes per hour, and collect this ethanol elution with the 75v/v% ethanol of 5 times of medical material amounts (being 500ml).Ethanol elution is carried out decompression recycling ethanol to there not being alcohol flavor (vacuum-0.1MPa, 75 ℃ of temperature), continue to be concentrated into relative density and be 1.01～1.10 extractum (this relative density refers to the density with respect to water).With extractum water bath method (100 ℃), put into vacuum drying oven low-temperature vacuum drying (vacuum-0.1MPa, drying at room temperature 48 hours), promptly obtain the extract of Semen Litchi effective part group.
Wherein, the processing method of AB-8 macroporous resin is following: get pharmaceutical clean grade AB-8 macroporous resin, wet method is packed in the resin column; Remove the resin of bubbling through the water column; After putting solid carbon dioxide from the lower end, with 95v/v% ethanol drip washing post layer, until leacheate and water mix with 1: 1 volume ratio do not show muddiness till; Use a large amount of pure water rinsing post layers then, do not have the alcohol flavor until effluent and get final product.
The extract of above gained Semen Litchi effective part group is measured through ultraviolet visible spectrophotometry can know the wherein content of relevant composition: general flavone content (referring to account for the mass ratio of total solid substance) is about 20%; Total saponin content (referring to account for the mass ratio of total solid substance) is about 25%, and content of tannin (referring to account for the mass ratio of total solid substance) is about 32%.
Embodiment 3 pilot scale scale-ups
Take by weighing 10Kg Semen Litchi coarse powder, add for the first time the 70v/v% ethanol of 100L, soaked after 0.5 hour supersound extraction 1 hour, inclining, it is subsequent use extracting solution to container.Medicinal residues continue to add the 70v/v% ethanol of 80L, soak after 0.5 hour, and supersound extraction 1 hour, inclining extracting solution and the merging of primary extracting solution; To there not being alcohol flavor (vacuum-0.1MPa, 75 ℃ of temperature), extracting solution is settled to 25L with distilled water diluting with the total extracting solution decompression recycling ethanol after merging, and hold over night is filtered filtrate for later use.Filtrating is at first with the AB-8 macroporous resin column of flow velocity through having handled of 2 times of bed volumes per hour; Carry out eluting with the pure water of 3 times of amount of resin with the flow velocity of 2 times of bed volumes per hour then; Discard water lotion; And then carry out the active substance on the eluting resin with the flow velocity of 2 times of bed volumes per hour, and collect this part ethanol elution with the 75v/v% ethanol of 5 times of medical material amounts (being 50L).The ethanol elution decompression recycling ethanol to there not being alcohol flavor (vacuum-0.1MPa, 75 ℃ of temperature), is continued to be concentrated into relative density and is 1.01～1.10 extractum (this relative density refers to the density with respect to water).With above extractum water bath method (100 ℃), put into vacuum drying oven low-temperature vacuum drying (vacuum-0.1MPa, drying at room temperature 48 hours), promptly obtain the extract of Semen Litchi effective part group.
Wherein, the processing method of macroporous resin is following: get the pharmaceutical clean grade AB-8 macroporous resin of 20Kg, wet method is packed in the resin column; Remove the resin of bubbling through the water column; After putting solid carbon dioxide from the lower end, with 95v/v% ethanol drip washing post layer, until leacheate and water mix at 1: 1 do not show muddiness till; Use a large amount of pure water rinsing post layers then, do not have the alcohol flavor until effluent and get final product.
The Semen Litchi effective site group extract that obtains is measured wherein content of effective through ultraviolet visible spectrophotometry, and the dried cream quality of weighing extract is calculated paste-forming rate (the dried cream quality/medical material of paste-forming rate=extract feed intake quality * 100%)
Adopt above-mentioned technology, prepared 3 batches of Semen Litchi extracts altogether, result such as table 1.
Table 1 pilot plant test result
The result shows: paste-forming rate is 3% in the extract, has reached purification effect; Extract can be surveyed in the composition, and general flavone content reaches 20.1～20.5%, and total saponin content reaches 19.3～20%; Content of tannin reaches 31.8～32.2%; Three's sum reaches more than 71%, reaches steady quality, controlled requirement, meets the requirement of the modernization of Chinese medicine; Process stabilizing can be realized suitability for industrialized production.
Claims (10)
1. Semen Litchi effective part group preparation method of extract is characterized in that may further comprise the steps:
1) get the Semen Litchi medical material, pulverizing the back is that 1g: 8～10ml adds ethanol according to solid-liquid ratio, soaks after 0.5～1 hour, carries out supersound extraction, and it is subsequent use to obtain extracting solution A;
2) in medicinal residues, be that 1g: 8～10ml adds ethanol, soak after 0.5～1 hour, carry out supersound extraction, obtain extracting solution B, extracting solution A and extracting solution B merging according to solid-liquid ratio;
3) extracting solution A that merges and extracting solution B are reclaimed ethanol to there not being the alcohol flavor, use distilled water diluting to being 0.4g/ml in crude drug amount concentration this medicinal liquid then, hold over night is filtered filtrate for later use;
4) filtrating is through the AB-8 macroporous resin column, and elder generation carries out eluting with the pure water of 3 times of amount of resin then, discards water lotion, again with the active substance on the ethanol elution resin of 5 times of medical material amounts, and collects ethanol elution;
5) ethanol elution of step 4) being collected reclaims ethanol to there not being the alcohol flavor, continues simmer down to extractum;
6) with the said extractum evaporate to dryness of step 5), carry out low-temperature vacuum drying again, promptly get the extract of Semen Litchi effective part group.
2. method for preparing according to claim 1 is characterized in that: said step 1), step 2) in used concentration of alcohol be 70v/v%.
3. method for preparing according to claim 1 is characterized in that: the used concentration of alcohol of said step 4) is 75v/v%.
4. method for preparing according to claim 1 is characterized in that: adopt distilling under reduced pressure to reclaim ethanol in said step 3) and the step 5).
5. method for preparing according to claim 4 is characterized in that: the condition of said distilling under reduced pressure is vacuum-0.1MPa, 75 ℃ of temperature.
6. method for preparing according to claim 1 is characterized in that: in the said step 4), the flow velocity of filtrating through the AB-8 macroporous resin column, be per hour 2 times of bed volumes with the flow velocity of pure water eluting and with the flow velocity of ethanol elution.
7. method for preparing according to claim 1 is characterized in that: the relative density of the extractum in the said step 5) is 1.01～1.10.
8. method for preparing according to claim 1 is characterized in that: in the said step 6) with said extractum water bath method.
9. method for preparing according to claim 8 is characterized in that: the temperature of said water bath method is 100 ℃.
10. method for preparing according to claim 1 is characterized in that: in the said step 6), vacuum drying condition is vacuum-0.1MPa, drying at room temperature 48 hours.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102836265A (en) * | 2012-09-24 | 2012-12-26 | 广州市中医医院 | Litchi seed dropping pill and preparation method thereof |
| CN103638177A (en) * | 2013-06-30 | 2014-03-19 | 金玛瑙香水（明光）有限公司 | Extraction process of lychee seed saponin |
| CN104547205A (en) * | 2014-12-11 | 2015-04-29 | 惠州学院 | Method for extracting lychee seedvflavonoids via ultrasonic wave |
| CN105902663A (en) * | 2016-04-25 | 2016-08-31 | 中山职业技术学院 | Preparation method of litchi seed flavonoids |
| CN105962283A (en) * | 2016-05-03 | 2016-09-28 | 王胜 | Plant salt containing lychee seed extract and preparation method of plant salt |
| CN110638896A (en) * | 2019-09-09 | 2020-01-03 | 天津科技大学 | Application of lychee seed extract with effects of reducing blood pressure and improving complications of lychee seed extract and preparation method of preparation |
| CN115634180A (en) * | 2022-11-02 | 2023-01-24 | 广东岭南职业技术学院 | Litchi seed composition and preparation method and application thereof |
| CN116832097A (en) * | 2023-07-03 | 2023-10-03 | 广州湾区生物医药研究院 | Litchi seed fermentation product, preparation method thereof and application of litchi seed fermentation product in preparation of products with anti-inflammatory effect |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102836265A (en) * | 2012-09-24 | 2012-12-26 | 广州市中医医院 | Litchi seed dropping pill and preparation method thereof |
| CN103638177A (en) * | 2013-06-30 | 2014-03-19 | 金玛瑙香水（明光）有限公司 | Extraction process of lychee seed saponin |
| CN104547205A (en) * | 2014-12-11 | 2015-04-29 | 惠州学院 | Method for extracting lychee seedvflavonoids via ultrasonic wave |
| CN105902663A (en) * | 2016-04-25 | 2016-08-31 | 中山职业技术学院 | Preparation method of litchi seed flavonoids |
| CN105902663B (en) * | 2016-04-25 | 2020-04-14 | 中山职业技术学院 | Preparation method of lychee seed flavone |
| CN105962283A (en) * | 2016-05-03 | 2016-09-28 | 王胜 | Plant salt containing lychee seed extract and preparation method of plant salt |
| CN110638896A (en) * | 2019-09-09 | 2020-01-03 | 天津科技大学 | Application of lychee seed extract with effects of reducing blood pressure and improving complications of lychee seed extract and preparation method of preparation |
| CN115634180A (en) * | 2022-11-02 | 2023-01-24 | 广东岭南职业技术学院 | Litchi seed composition and preparation method and application thereof |
| CN116832097A (en) * | 2023-07-03 | 2023-10-03 | 广州湾区生物医药研究院 | Litchi seed fermentation product, preparation method thereof and application of litchi seed fermentation product in preparation of products with anti-inflammatory effect |
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