CN105560301B - A kind of ginkgo biloba p.e large-scale method for producing - Google Patents
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
The present invention relates to a kind of ginkgo biloba p.e large-scale method for producing, belong to natural plant extracts technical field of refinement.Mainly comprise the steps that ginkgo leaf crush after through mixed extractant solvent, extract liquor separation, upper layer of extraction liquid recycling design, it is residual that lower layer's extract liquor turns primary concentration precipitation, a concentrate is obtained, a concentrate is added n-butanol and is purified, and obtains water layer and n-butanol layer, water layer and n-butanol layer product are concentrated and dried respectively, obtain two kinds of products of water soluble ginkgo leaf extract A and alcohol-soluble ginkgo biloba p.e B.The simple process, yield is high, at low cost, and flavonoid of ginkgo biloba is high, ginkgoic acid removal is thorough.
Description
Technical field
The invention belongs to natural plant extracts technical field of refinement more particularly to a kind of ginkgo biloba p.e scale metaplasias
Production method.
Background technique
Containing the multiple components that natural activity flavones and amarolide etc. are beneficial with human health in ginkgo leaf, there is dissolution gallbladder
Sterol expands the effect of blood vessel, to improve brain disorder, artery sclerosis, hypertension, dizziness, tinnitus, headache, senile dementia,
Failure of memory etc. has positive effect.Through national health department detect prove: drink ginkgo leave tea can obviously reduce serum cholesterol,
Triglyceride and low-density blood lipoprotein, reduce the effect of internal depot lipid.For the adjusting of hyperlipidemia, hypertension and coronary disease
The complementary prevention and treatment of the diseases of cardiovascular and cerebrovascular systems patient such as disease and the weight-reducing of endomorphy type crowd etc. have good effect, are to prevent and treat
Treat the ideal drink of senile dementia.Be it is recognized in the world control, the optimal pharmaceutical compositions of anti-cardiovascular and cerebrovascular disease.
Ginkgo biloba p.e has no toxic side effect after de- ginkgoic acid can be widely used for medicine food cosmetic field, at present state
The ginkgo biloba p.e of interior production water solubility problems due to technology aspect are not solved very well always, product
It is mostly fat-soluble, and fat-soluble ginkgo biloba p.e economic value, application surface and in terms of not as good as water-soluble
Property ginkgo biloba p.e.
Currently, it is more about the research for extracting ginkgo biloba extract, by retrieval, find related patents and literature content such as
Under: in the patent of Publication No. CN102772452A, using ginkgo leaf or using common ginkgo biloba p.e as raw material, through organic solvent
Extraction with aqueous solution, extracting solution concentration and recovery solvent are diluted with water rear standing sedimentation, centrifugation or filtering removal precipitating, and clear liquid is used big
Hole resin adsorption, washing removal impurity are directly gone up the depickling of gel-type hydrogen bond absorbing resin and are rushed after aqueous solutions of organic solvent desorption
It washes, efflux and flushing liquor concentrate drying can must surpass extractive of low acidic gingko leaves.This method purification process need to be by resin twice
Processing, more than hour time-consuming for minimum needs 20, low efficiency；Another aspect resin can intercept part active principle, and production is received
Rate is low.
A kind of preparation method of ginkgo biloba p.e, publication number: CN104095889A provides a kind of ginkgo biloba p.e
Preparation method, this method be using ginkgo leaf as raw material, by alcohol or acetone, water is heavy, macroreticular resin column purification, boil water are heavy,
Macroporous resin column is secondarily purified, refrigeration precipitates, alcohol or acetone low-temperature water-soluble purification prepare ginkgo biloba p.e.Its product has
The characteristics of water-soluble, low phenolic acid, low anthocyanidin, low residue on ignition, wherein total flavonoids >=24% in ginkgo biloba p.e,
Terpene lactone >=9.5%, residue on ignition≤0.3%, procyanidine≤0.3%, total ginkgolic acid≤1ppm and cold water solubility
>=5%.This method realizes the quality for improving ginkgo biloba p.e using two step resin column methods and two-step precipitation, and process is numerous
It is trivial, and resin regeneration also can virtually waste of manpower, material resources.
Summary of the invention
To solve technical problem present in above-mentioned this field, the present invention provides a kind of ginkgo biloba p.e large-scale production
Method, the simple process and low cost improve ginkgo biloba extract matter, obtain the water-soluble and preferable ginkgo leaf of alcohol-soluble
Extract.
The present invention adopts the following technical solutions: a kind of ginkgo biloba p.e large-scale method for producing, comprising the following steps:
(1) pretreatment of raw material: ginkgo leaf is crushed to obtain ginkgo leaf powder, mesh number is 20~60 mesh；
(2) mixed extractant solvent: mixed extractant solvent smashed ginkgo leaf obtains extract liquor after filtering；
(3) extract liquor separates: extract liquor settle and separate in separation equipment；Upper layer of extraction liquid recycling design, lower layer's extraction
Liquid turns primary concentration；
(4) once concentration and precipitation are residual: lower layer's extract liquor being concentrated, then removes molten residual, obtains a concentrate；
(5) it isolates and purifies: n-butanol being added in a concentrate and is isolated and purified, water layer and n-butanol layer are obtained；
(6) secondary concentration and precipitation are residual: water layer and n-butanol layer be concentrated to precipitation is residual to obtain water layer and n-butanol layer respectively
Concentrate；
(7) dry: water layer and n-butanol layer concentrate being separately dried, water soluble ginkgo leaf extract A is obtained and alcohol is molten
Property ginkgo biloba p.e two kinds of products of B.
Mixed solvent in step (2) of the present invention is n-hexane: ethanol water volume ratio is 1:1~12, institute
Stating concentration of alcohol in ethanol water is 20~80%.
Step (2) mixed extractant solvent number of the present invention is 2~4 times, and 30~60 DEG C of extraction temperature, extraction time is
0.5~2h；Raw material and mixed solvent mass volume ratio are 1:2~4, and the mass unit is kg, and the volume unit is L.
The settle and separate time is 0.5-2h in step (3) of the present invention.
Lower layer's extract liquor residual is removed to 500ppm or less for molten in step (4) of the present invention.
The additive amount of addition n-butanol is 5-9 times of a concentrate volume in step (5) of the present invention, can be divided into 1-
3 additions.
It is molten in step (6) of the present invention residual to be removed to 300ppm or less.
It is dry for spray drying, vacuum drying or freeze-drying in step (7) of the present invention.
The beneficial effects of adopting the technical scheme are that 1, using n-hexane, alcohol mixed solvent extract silver
Apricot leaf improves effective component yield, while can impurity of the step separation based on ginkgoic acid；2, it is isolated and purified using n-butanol
Target product effectively active constituent-enriched content and can be divided into water-soluble preferable ginkgo biloba p.e by ginkgo biloba p.e
A and the preferable ginkgo biloba p.e B two parts product of alcohol-soluble, wherein ginkgo biloba p.e A room temperature water solubility >=6%,
Middle ginkgo biloba p.e B room temperature ethyl alcohol solubility >=9%；3, the simple process and low cost, effect is preferable, improves ginkgo leaf
Extract quality not only increases ginkgo biloba p.e product content yield and product quality, and reduces production cost, silver
Flavone total content yield is 90% or more, and ginkgolides total content yield is 85% or more.
Specific embodiment
The present invention will be further described in detail below with reference to specific embodiments.
Embodiment 1
(1), 100 kilograms of ginkgo leaves are taken, are crushed using pulverizer, 20 mesh ginkgo leaf powders are obtained；
(2), mixed extractant solvent: use n-hexane: 50% ethyl alcohol is that the mixed solvent of 1:1 makees Extraction solvent, raw material and mixed
Bonding solvent mass volume ratio is 1:2；The ginkgo leaf powder crushed is added, extraction conditions: extraction 3 times, first pass temperature 45 C, when
Between 120min；Extract liquor is obtained by filtration in second time temperature 45 C, time 60min；
(3), n-hexane layer and alcohol layer separation: squeezing into separator for extract liquor, stands 1h, isolated lower layer's extraction
Liquid alcohol layer is concentrated, and upper layer of extraction liquid recycling design recycles；
(4), it once concentration and the molten residual removing of ethyl alcohol: by alcohol layer in enrichment facility after recycling design, is transferred to molten residual
In removing means finally residual 500ppm is removed to hereinafter, concentrate purifies for molten；
(5), n-butanol purifies: a concentrate being transferred in a separator and 5 times of concentrate volumes are once added
N-butanol, filtered after stirring 2h, filtrate stands 30min, isolated water layer and n-butanol layer product；
(6), secondary concentration and the molten residual removing of n-butanol: water layer and n-butanol layer product are returned in enrichment facility respectively
After receiving solvent, it is transferred in molten residual removing means and finally residual is removed to 300ppm or less for molten；
(7), dry: molten residual water layer will have been taken off and n-butanol layer ginkgo biloba p.e thick paste is put into pallet in hot state
In, pallet is put into vacuum oven and carries out product drying, drying time 8h, temperature is 68 DEG C, water-solubility ginkgo after drying
Leaf extract A product 0.75kg, flavonoid of ginkgo biloba 27.85%, ginkgolic acid content 0.52ppm, ginkgolides content
6.12%；Obtain alcohol-soluble ginkgo biloba p.e B product weight 1.32kg, flavonoid of ginkgo biloba 29.61%, ginkgolic acid content
0.63ppm, ginkgolides content 6.54%.
GINKGO BILOBA EXTRACT total content yield is 92.28%, and ginkgolides total content yield is 88.13%.
Embodiment 2
(1), 100 kilograms of ginkgo leaves are taken, are crushed using pulverizer, 60 mesh ginkgo leaf powders are obtained；
(2), mixed extractant solvent: use n-hexane: 70% proportion of ethanol is that the mixed solvent of 1:1 makees Extraction solvent, raw material
It is 1:3 with mixed solvent mass volume ratio；The ginkgo leaf powder crushed is added, extraction conditions: extraction 4 times, first pass temperature 45
DEG C, time 120min；Second time temperature 45 C, time 60min；Third is all over temperature 45 C, time 60min；4th time temperature 45
DEG C, extract liquor is obtained by filtration in time 30min；
(3), n-hexane layer and alcohol layer separation: squeezing into separator for extract liquor, stands 1h, isolated lower layer's extraction
Liquid alcohol layer is concentrated, and upper layer of extraction liquid recycling design recycles；
(4), it once concentration and the molten residual removing of ethyl alcohol: by alcohol layer in enrichment facility after recycling design, is transferred to molten residual
In removing means finally residual 500ppm is removed to hereinafter, concentrate purifies for molten；
(5), n-butanol purifies: a concentrate being transferred in a separator and 9 times of concentration objects are added in three times
Long-pending n-butanol filters after stirring 1.5h, and filtrate stands 60min, isolated water layer and n-butanol layer product；
(6), secondary concentration and the molten residual removing of n-butanol: water layer and n-butanol layer product are returned in enrichment facility respectively
After receiving solvent, it is transferred in molten residual removing means and finally residual is removed to 300ppm or less for molten；
(7), dry: molten residual ginkgo biloba p.e thick paste will have been taken off and be freeze-dried, water soluble ginkgo leaf extracts after drying
Object A product weight is 0.55kg, flavonoid of ginkgo biloba 28.30%, ginkgolic acid content 0.66ppm, ginkgolides content
6.36%；Obtain alcohol-soluble ginkgo biloba p.e B product weight 1.53kg, flavonoid of ginkgo biloba 26.04%, ginkgolic acid content
0.48ppm, ginkgolides content 6.45%.
GINKGO BILOBA EXTRACT total content yield is 93.81%, and ginkgolides total content yield is 89.05%.
Embodiment 3
(1), 100 kilograms of ginkgo leaves are taken, are crushed using pulverizer, 40 mesh ginkgo leaf powders are obtained；
(2), mixed extractant solvent: use n-hexane: 20% proportion of ethanol is that the mixed solvent of 1:12 makees Extraction solvent, former
Material is 1:4 with mixed solvent mass volume ratio；The ginkgo leaf powder crushed is added, extraction conditions: extraction 3 times, first pass temperature
30 DEG C, time 120min；Second time temperature 60 C, time 60min；Extraction is obtained by filtration all over temperature 60 C, time 30min in third
Take liquid；
(3), n-hexane layer and alcohol layer separation: squeezing into separator for extract liquor, stands 0.5h, isolated lower layer's extraction
Liquid alcohol layer is taken to be concentrated, upper layer of extraction liquid recycling design recycles；
(4), it once concentration and the molten residual removing of ethyl alcohol: by alcohol layer in enrichment facility after recycling design, is transferred to molten residual
In removing means finally residual 300ppm is removed to hereinafter, concentrate purifies for molten；
(5), n-butanol purifies: a concentrate being transferred in a separator and 6 times of concentration objects are added in two portions
Long-pending n-butanol filters after stirring 1.5h, and filtrate stands 60min, isolated water layer and n-butanol layer product；
(6), secondary concentration and the molten residual removing of n-butanol: water layer and n-butanol layer product are returned in enrichment facility respectively
After receiving solvent, it is transferred in molten residual removing means and finally residual is removed to 300ppm or less for molten；
(7), dry: molten residual ginkgo biloba p.e thick paste will have been taken off and be spray-dried, water soluble ginkgo leaf extracts after drying
Object A product weight is 0.46kg, flavonoid of ginkgo biloba 30.65%, ginkgolic acid content 0.38ppm, ginkgolides content
6.09%；Obtain alcohol-soluble ginkgo biloba p.e B product weight 1.76kg, flavonoid of ginkgo biloba 29.35%, ginkgolic acid content
0.26ppm, ginkgolides content 6.72%.
GINKGO BILOBA EXTRACT total content yield is 91.09%, and ginkgolides total content yield is 90.75%.
Embodiment 4
(1), 100 kilograms of ginkgo leaves are taken, are crushed using pulverizer, 40 mesh ginkgo leaf powders are obtained；
(2), mixed extractant solvent: use n-hexane: 80% proportion of ethanol is that the mixed solvent of 1:3 makees Extraction solvent, raw material
It is 1:3 with mixed solvent mass volume ratio；The ginkgo leaf powder crushed is added, extraction conditions: extraction 3 times, first pass temperature 40
DEG C, time 120min；Second time temperature 50 C, time 60min；Extraction is obtained by filtration all over temperature 60 C, time 60min in third
Liquid；
(3), n-hexane layer and alcohol layer separation: squeezing into separator for extract liquor, stands 2h, isolated lower layer's extraction
Liquid alcohol layer is concentrated, and upper layer of extraction liquid recycling design recycles；
(4), it once concentration and the molten residual removing of ethyl alcohol: by alcohol layer in enrichment facility after recycling design, is transferred to molten residual
In removing means finally residual 400ppm is removed to hereinafter, concentrate purifies for molten；
(5), n-butanol purifies: a concentrate being transferred in a separator and 8 times of concentrate volumes are once added
N-butanol, filtered after stirring 1h, filtrate stands 40min, isolated water layer and n-butanol layer product；
(6), secondary concentration and the molten residual removing of n-butanol: water layer and n-butanol layer product are returned in enrichment facility respectively
After receiving solvent, it is transferred in molten residual removing means and finally residual is removed to 300ppm or less for molten；
(7), dry: molten residual ginkgo biloba p.e thick paste will have been taken off and be put into pallet in hot state, pallet is put into
Vacuum oven carries out product drying, drying time 10h, and temperature is 70 DEG C, water soluble ginkgo leaf extract A product after drying
Weight is respectively 0.98kg, flavonoid of ginkgo biloba 27.55%, ginkgolic acid content 0.72ppm, ginkgolides content 6.91%；
Obtain alcohol-soluble ginkgo biloba p.e B product weight 1.65kg, flavonoid of ginkgo biloba 28.34%, ginkgolic acid content
0.81ppm, ginkgolides content 6.99%.
GINKGO BILOBA EXTRACT total content yield is 92.15%, and ginkgolides total content yield is 90.48%.
Embodiment 5
(1), 100 kilograms of ginkgo leaves are taken, are crushed using pulverizer, 20 mesh ginkgo leaf powders are obtained；
(2), mixed extractant solvent: use n-hexane: 60% proportion of ethanol is that the mixed solvent of 1:6 makees Extraction solvent, raw material
It is 1:4 with mixed solvent mass volume ratio；The ginkgo leaf powder crushed is added, extraction conditions: extraction 2 times, first pass temperature 60
DEG C, time 120min；Second time 55 DEG C of temperature, extract liquor is obtained by filtration in time 120min；
(3), n-hexane layer and alcohol layer separation: squeezing into separator for extract liquor, stands 1h, isolated lower layer's extraction
Liquid alcohol layer is concentrated, and upper layer of extraction liquid recycling design recycles；
(4), it once concentration and the molten residual removing of ethyl alcohol: by alcohol layer in enrichment facility after recycling design, is transferred to molten residual
In removing means finally residual 500ppm is removed to hereinafter, concentrate purifies for molten；
(5), n-butanol purifies: a concentrate being transferred in a separator and 7 times of concentrate volumes are once added
N-butanol, filtered after stirring 1h, filtrate stands 30min, isolated water layer and n-butanol layer product；
(6), secondary concentration and the molten residual removing of n-butanol: water layer and n-butanol layer product are returned in enrichment facility respectively
After receiving solvent, it is transferred in molten residual removing means and finally residual is removed to 300ppm or less for molten；
(7), dry: molten residual ginkgo biloba p.e thick paste will have been taken off and be put into pallet in hot state, pallet is put into
Vacuum oven carries out product drying, and drying time 8h, water soluble ginkgo leaf extract A product weight is after drying
1.21kg, flavonoid of ginkgo biloba 26.42%, ginkgolic acid content 0.83ppm, ginkgolides content 6.23%；Obtain alcohol-soluble
Ginkgo biloba p.e product weight 1.68Kg, flavonoid of ginkgo biloba 27.05%, ginkgolic acid content 0.68ppm, ginkgolides
Content 6.49%.
GINKGO BILOBA EXTRACT total content yield is 90.90%, and ginkgolides total content yield is 85.65%.
Claims (7)
1. a kind of ginkgo biloba p.e large-scale method for producing, which comprises the following steps:
(1) pretreatment of raw material: ginkgo leaf is crushed to obtain ginkgo leaf powder, mesh number is 20~60 mesh；
(2) mixed extractant solvent: mixed extractant solvent smashed ginkgo leaf obtains extract liquor after filtering；
(3) extract liquor separates: extract liquor settle and separate in separation equipment；Upper layer of extraction liquid recycling design, lower layer's extract liquor turn
Primary concentration；
(4) once concentration and precipitation are residual: lower layer's extract liquor being concentrated, then removes molten residual, obtains a concentrate；
(5) it isolates and purifies: n-butanol being added in a concentrate and is isolated and purified, water layer and n-butanol layer are obtained；
(6) secondary concentration and precipitation are residual: residual water layer and the n-butanol layer of obtaining of precipitation is concentrated in water layer and n-butanol layer respectively and is concentrated
Object；
(7) dry: water layer and n-butanol layer concentrate being separately dried, water soluble ginkgo leaf extract A and alcohol-soluble silver are obtained
Two kinds of products of apricot leaf extract B；
Mixed solvent in the step (2) is n-hexane: ethanol water volume ratio is 1:1~12, and the ethyl alcohol is water-soluble
Concentration of alcohol is 20~80% in liquid.
2. a kind of ginkgo biloba p.e large-scale method for producing according to claim 1, which is characterized in that the step
(2) mixed extractant solvent number is 2~4 times, and 30~60 DEG C of extraction temperature, extraction time is 0.5~2h；Raw material and mixed solvent
Mass volume ratio is 1:2~4, and the mass unit is kg, and the volume unit is L.
3. a kind of ginkgo biloba p.e large-scale method for producing according to claim 1, which is characterized in that the step
(3) the settle and separate time is 0.5-2h in.
4. a kind of ginkgo biloba p.e large-scale method for producing according to claim 1 to 3, which is characterized in that
Lower layer's extract liquor residual is removed to 500ppm or less for molten in the step (4).
5. a kind of ginkgo biloba p.e large-scale method for producing according to claim 1 to 3, which is characterized in that
The additive amount of addition n-butanol is 5-9 times of a concentrate volume in the step (5), is divided into 1-3 addition.
6. a kind of ginkgo biloba p.e large-scale method for producing according to claim 1 to 3, which is characterized in that
It is molten in the step (6) residual to be removed to 300ppm or less.
7. a kind of ginkgo biloba p.e large-scale method for producing according to claim 1 to 3, which is characterized in that
It is dry for spray drying, vacuum drying or freeze-drying in the step (7).
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1911257A (en) * | 2005-08-10 | 2007-02-14 | 北京联合伟华药业有限公司 | Extractive of ginkgo tree leaves, prepn. method and application thereof |
| CN102106877A (en) * | 2010-12-22 | 2011-06-29 | 晨光生物科技集团股份有限公司 | Production process of gingko leaf extract |
| CN103393671A (en) * | 2013-08-21 | 2013-11-20 | 上海信谊百路达药业有限公司 | Extracting and refining method of ginkgolide |
-
2015
- 2015-12-29 CN CN201511006328.5A patent/CN105560301B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1911257A (en) * | 2005-08-10 | 2007-02-14 | 北京联合伟华药业有限公司 | Extractive of ginkgo tree leaves, prepn. method and application thereof |
| CN102106877A (en) * | 2010-12-22 | 2011-06-29 | 晨光生物科技集团股份有限公司 | Production process of gingko leaf extract |
| CN103393671A (en) * | 2013-08-21 | 2013-11-20 | 上海信谊百路达药业有限公司 | Extracting and refining method of ginkgolide |
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