CN106074631B - A kind of low ginkgoic acid low ash divides the industrialized preparing process of ginkgo biloba p.e - Google Patents
A kind of low ginkgoic acid low ash divides the industrialized preparing process of ginkgo biloba p.e Download PDFInfo
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- YXHVCZZLWZYHSA-FPLPWBNLSA-N Ginkgoic acid Chemical compound CCCCCC\C=C/CCCCCCCC1=CC=CC(O)=C1C(O)=O YXHVCZZLWZYHSA-FPLPWBNLSA-N 0.000 title claims abstract description 94
- 235000008100 Ginkgo biloba Nutrition 0.000 title claims abstract description 61
- 244000194101 Ginkgo biloba Species 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000000605 extraction Methods 0.000 claims abstract description 30
- 241000218628 Ginkgo Species 0.000 claims abstract description 28
- 235000011201 Ginkgo Nutrition 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 239000012530 fluid Substances 0.000 claims abstract description 23
- 239000011347 resin Substances 0.000 claims abstract description 21
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 239000000284 extract Substances 0.000 claims abstract description 18
- 239000012528 membrane Substances 0.000 claims abstract description 17
- 238000001728 nano-filtration Methods 0.000 claims abstract description 17
- 238000000746 purification Methods 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 55
- 235000019441 ethanol Nutrition 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- 235000009827 Prunus armeniaca Nutrition 0.000 claims description 6
- 244000018633 Prunus armeniaca Species 0.000 claims description 6
- 239000012046 mixed solvent Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 4
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 239000003599 detergent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000000047 product Substances 0.000 description 14
- 229930003935 flavonoid Natural products 0.000 description 11
- 150000002215 flavonoids Chemical class 0.000 description 11
- 235000017173 flavonoids Nutrition 0.000 description 11
- 239000009429 Ginkgo biloba extract Substances 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 238000010828 elution Methods 0.000 description 4
- 229940068052 ginkgo biloba extract Drugs 0.000 description 4
- 235000020686 ginkgo biloba extract Nutrition 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- YXHVCZZLWZYHSA-UHFFFAOYSA-N (Z)-6-[8-pentadecenyl]salicylic acid Natural products CCCCCCC=CCCCCCCCC1=CC=CC(O)=C1C(O)=O YXHVCZZLWZYHSA-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- HVAUUPRFYPCOCA-AREMUKBSSA-N 2-O-acetyl-1-O-hexadecyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCCOC[C@@H](OC(C)=O)COP([O-])(=O)OCC[N+](C)(C)C HVAUUPRFYPCOCA-AREMUKBSSA-N 0.000 description 1
- 206010008132 Cerebral thrombosis Diseases 0.000 description 1
- 201000001429 Intracranial Thrombosis Diseases 0.000 description 1
- 108010003541 Platelet Activating Factor Proteins 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000008485 antagonism Effects 0.000 description 1
- 230000002785 anti-thrombosis Effects 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019439 ethyl acetate Nutrition 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 229930184727 ginkgolide Natural products 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000007688 immunotoxicity Effects 0.000 description 1
- 231100000386 immunotoxicity Toxicity 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/16—Ginkgophyta, e.g. Ginkgoaceae (Ginkgo family)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- 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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses the industrialized preparing process that a kind of low ginkgoic acid low ash divides ginkgo biloba p.e, comprising the following steps: takes ginkgo leaf to smash, Extraction solvent is added, stirring is extracted, and filtering obtains ginkgo extract；Ginkgo extract is used into nanofiltration membrane, ginkgoic acid and inorganic salts in extracting solution is removed, obtains trapped fluid；By trapped fluid through macroporous resin purification, refined solution is obtained；Refined solution is concentrated, is spray-dried, obtains ginkgo biloba p.e product.Ginkgo acid content in the ginkgo biloba p.e that this method is prepared is less than 1ppm, and ash content is simple, efficient less than 0.3%, is capable of the removing level of quantified controlling ginkgoic acid, it can be achieved that large-scale continuous mass production.
Description
Technical field
The invention belongs to natural extract technical field of purification, and in particular to a kind of low ginkgoic acid low ash divides ginkgo leaf to extract
The industrialized preparing process of object.
Background technique
Ginkgo biloba p.e (Ginkgo Biloba Extract) is a kind of active principle extracted from ginkgo leaf, tool
There is the effects of improving cardiovascular circulation, antagonism platelet activating factor and antithrombotic, can be used for preventing and treating senile silly
Stay with the diseases such as cerebral thrombosis, primary medicinal component be GINKGO BILOBA EXTRACT and ginkgolides.However also have containing some in ginkgo leaf
Malicious ingredient-ginkgoic acid (ginkgoic acids), research find that ginkgoic acid has sensitization, cytotoxicity and immunotoxicity etc.
Effect, is the major toxicity substance in ginkgo biloba p.e GBE, edible safety has caused the great attention of people, state
The GBE quality standard regulation ginkgo acid content generally acknowledged on border is necessarily less than 5mg/kg.
Current market sales of ginkgo biloba p.e largely uses alcohol extracting method or water extraction to extract to obtain, and is extracting
A large amount of ginkgoic acid is extracted in journey, causes Ginkgolic Acid in Extract of Ginkgo biloba Leaves content available on the market irregular,
It is apparently higher than quality criteria requirements.Therefore must have it is efficient, simple, and can industrialized production method reduce ginkgo acid content.
There are the method for some removal Ginkgolic Acid in Extract of Ginkgo biloba Leaves, but most cumbersome at present, is not easy to realize big rule
Mould industrialized production.Such as a kind of preparation side of ginkgo biloba p.e is disclosed in the patent of Publication No. CN105267257A
Ginkgo leaf is first crushed ethyl alcohol heating and refluxing extraction by method, and pH is adjusted to alkalinity, and refrigeration is placed 12-72 hours, and it is pure to cross macroporous resin column
Change, filter, sterilizing obtains ginkgo biloba p.e.Impurity peaks are eluted using 25% ethyl alcohol and 10% sodium acetate solution, using 30~
50% ethanol elution target component peak.Although the invention can remove the ginkgoic acid in ginkgo biloba extract, process is complicated, time-consuming
It is long, and the specific steps without clearly proposing removal ginkgoic acid；In the patent of Publication No. CN104739898A, use is polynary
Alcohol surfactant removes the ginkgoic acid in ginkgo biloba p.e, and the ginkgoic acid in this method treated ginkgo biloba p.e is small
In 5ppm, but this method is the processing to ginkgo biloba p.e product, and ginkgoic acid can not be removed from extraction process, increases work
Sequence.It is for another example disclosed in the patent of Publication No. CN103110671B a kind of using silver-colored in nano material removing ginkgo biloba p.e
The method of apricot acid and heavy metal.This method is by extracting, column chromatography, ferriferrous oxide material adsorb ginkgoic acid, Magneto separate, separation
Liquid, concentrate drying obtain ginkgo biloba p.e.Although this method can reduce the content of ginkgoic acid, increased using nano material cost
Add, is not suitable for being mass produced.
In short, at present both at home and abroad removal EGb in ginkgoic acid method mainly have solvent extraction removal, resin removal method,
New material Adsorption.Although low ginkgoic acid EGb can be made in the above several method, organic solvent extraction is wanted
It is repeatedly washed using organic solvent, wastes a large amount of reagents, and residual quantity is big, inflammable and explosive, security risk is big；Resin removing needs special
Macroreticular resin, expensive, pretreatment complexity, service life is limited, and the production cycle is long, higher cost；Using novel
Material, increased costs are not suitable for industrialized production.Therefore, it is necessary to develop a kind of not only scientific and efficient but also be able to achieve the big life of serialization
The technology of the removal ginkgoic acid of production.
Summary of the invention
The shortcomings that in order to overcome the prior art, the present invention provide the industry that a kind of low ginkgoic acid low ash divides ginkgo biloba p.e
Change production method, can effectively remove ginkgoic acid in extraction process, it is time saving, efficient, it is easier to realize continuous mass production.
The technical scheme adopted by the invention to solve the technical problem is that: a kind of low ginkgoic acid low ash divides ginkgo biloba p.e
Industrialized preparing process, comprising the following steps:
(1) it takes ginkgo leaf to smash, Extraction solvent is added, stirring is extracted, and filtering obtains ginkgo extract；
(2) ginkgo extract is used into nanofiltration membrane, removes ginkgoic acid and inorganic salts in extracting solution, is retained
Liquid；
(3) trapped fluid is obtained into refined solution through macroporous resin purification；
(4) refined solution is concentrated, is spray-dried, obtains ginkgo biloba p.e product.
Trapped fluid in step (2) of the present invention need to be washed by nanofiltration membrane, and detergent is Extraction solvent, water, washing
Dosage is the 1/10-1/3 of trapped fluid quality, and washing times are 2-4 times.
Trapped fluid in step (2) of the present invention need to be washed by nanofiltration membrane, and each wash time is 10-20min/
It is secondary.
Extracting temperature is 40-50 DEG C in the step (1) of the present invention, and extraction time is 3 times, and extraction time is 1-2h/ times；
Extraction solvent is the mixed solvent of solvent A and ethyl alcohol, and the volume ratio of the solvent A and ethyl alcohol is 1:2-4；The solvent A is fourth
Any one of ketone, acetone or ethyl acetate, Extraction solvent volume are 3-5 times of material quality, and the volume unit is L, institute
Stating mass unit is kg.
The molecular weight of nanofiltration membrane retention substance is 400-600 dalton in step (2) of the present invention.
Ginkgoic acid < 1ppm, ash content < 0.3% in ginkgo biloba p.e product obtained in step (4) of the present invention.
Macroreticular resin is polar macroporous adsorption resin in step (3) of the present invention；Cutting in step (3) of the present invention
It stays and is concentrated into no ethyl alcohol on liquid before macroreticular resin.
Macroporous resin purification step in step (3) of the present invention are as follows: washing amount is 1-3 times of column volume, and parsing dosage is
2-5 times of column volume, the ethyl alcohol that the parsing solvent is 40-70%.
Spray drying condition in step (4) of the present invention are as follows: spraying intake air temperature is at 140-180 DEG C, air outlet temperature
80-90 DEG C of degree.
In the step (1) of the present invention in raw material ginkgo leaf: total flavonoids content: 0.700-1.200%, ginkgoic acid contain
Amount: 60-110ppm.
Ginkgoic acid and ginkgo biloba extract effective substance method reference standard " ginkgo biloba p.e LY/T in the present invention
1699-2007》。
The beneficial effects of adopting the technical scheme are that (1) is extracted using mixed solvent, extraction is more thorough,
Yield is higher, low compared with the extraction feed liquid ginkgo acid content that single alcohol solvent extraction obtains；(2) using in nanofiltration membrane removing extracting solution
Ginkgoic acid, it is not only time saving but also simple, while can also remove the salinity of product, reduce product ash content, improve product purity, Er Qieshe
Standby simple for structure compact, occupied area is small, and low energy consumption, easy to operate, it can be achieved that automated job, stability is good, easy to maintain.
(3) by the present invention in that with cleaning solvent and water, trapped fluid is further washed by nanofiltration membrane, by silver remaining in trapped fluid
Apricot acid, ash content further remove, and the removal efficiency of ginkgoic acid are improved to a greater extent, in the ginkgo biloba p.e being prepared
Ginkgo acid content is less than 1ppm, and ash content is simple, efficiently less than 0.3%, the removing for capableing of quantified controlling ginkgoic acid it is horizontal, it can be achieved that
Large-scale continuous mass production.
Specific embodiment
The present invention is described in further details by the following examples.
Embodiment 1
A kind of low ginkgoic acid low ash divides the industrialized preparing process of ginkgo biloba p.e, comprising the following steps:
(1) ginkgo leaf is taken to smash 50kg(total flavonoids content 0.7213%, ginkgoic acid 65ppm), it is molten that 3 times of extractions are added
Agent, 40 DEG C of stirrings are extracted 3 times, and extraction time is 1h/ times, and filtering, merging filtrate obtains ginkgo extract；Extraction solvent be butanone with
The volume ratio of the mixed solvent of ethyl alcohol, butanone and ethyl alcohol is 1:2, and total flavonoids yield is 99.03% in extracting solution.
(2) ginkgo extract is used into 400 dalton nanofiltration membranes, removes ginkgoic acid and inorganic salts in extracting solution,
It is concentrated into feed liquid 1/3, obtains trapped fluid；The Extraction solvent and water for using trapped fluid quality 1/10 respectively, in nanofiltration membrane system
Trapped fluid is washed, and washing times are 2 times, and each wash time is 10min/ times.
(3) trapped fluid is concentrated into no ethyl alcohol, through D301 macroporous resin purification, obtains refined solution；
Macroporous resin purification step are as follows: pass through 1 times of column volume washed with impurities, 3 times of 55% ethanol elutions of column volume obtain pure
Change liquid.
(4) refined solution is concentrated, is spray-dried, spraying intake air temperature 90 DEG C of air outlet temperature, obtains silver at 140 DEG C
Apricot leaf extract product.
It is 0.8ppm, ash content 0.25%, total flavonoids content 26%, content yield through ginkgoic acid in testing product
90.22%。
Embodiment 2
A kind of low ginkgoic acid low ash divides the industrialized preparing process of ginkgo biloba p.e, comprising the following steps:
(1) ginkgo leaf is taken to smash 80kg(total flavonoids content 0.8345%, ginkgoic acid 83ppm), it is molten that 3 times of extractions are added
Agent, 45 DEG C of stirrings are extracted 3 times, and extraction time is 1.5h/ times, and filtering, merging filtrate obtains ginkgo extract；Extraction solvent is acetone
With the mixed solvent of ethyl alcohol, the volume ratio of acetone and ethyl alcohol is 1:3, and total flavonoids yield is 98.46% in extracting solution.
(2) ginkgo extract is used into 500 dalton nanofiltration membranes, removes ginkgoic acid and inorganic salts in extracting solution,
It is concentrated into feed liquid 1/3, obtains trapped fluid；The Extraction solvent and water for using trapped fluid quality 1/5 respectively, to cutting in nanofiltration membrane system
Liquid is stayed to be washed, washing times are 3 times, and each wash time is 10min/ times.
(3) trapped fluid is concentrated into no ethyl alcohol, through AB-8 macroporous resin purification, obtains refined solution；
Macroporous resin purification step are as follows: pass through 2 times of column volume washed with impurities, 5 times of 40% ethanol elutions of column volume obtain pure
Change liquid.
(4) refined solution is concentrated, is spray-dried, spraying intake air temperature 88 DEG C of air outlet temperature, obtains silver at 165 DEG C
Apricot leaf extract product.
It is 0.5ppm, ash content 0.19%, total flavonoids content 28%, content yield through ginkgoic acid in testing product
91.23%。
Embodiment 3
Refined solution is obtained, concentration is except after ethyl alcohol, spray drying, intake air temperature is at 180 DEG C, 90 DEG C of air outlet temperature, i.e.,
Obtain ginkgo biloba p.e product.It is not detected through ginkgoic acid in testing product, ash content 0.11%, total flavonoids content 29% contains
Measure rate 90.56%.
A kind of low ginkgoic acid low ash divides the industrialized preparing process of ginkgo biloba p.e, comprising the following steps:
(1) ginkgo leaf is taken to smash 70kg(total flavonoids content 0.7545%, ginkgoic acid 105ppm), it is molten that 5 times of extractions are added
Agent, 50 DEG C of stirrings are extracted 3 times, and extraction time is 2h/ times, and filtering, merging filtrate obtains ginkgo extract；Extraction solvent is acetic acid second
The volume ratio of the mixed solvent of ester and ethyl alcohol, ethyl acetate and ethyl alcohol is 1:4, and total flavonoids yield is in extracting solution
98.36%。
(2) ginkgo extract is used into 600 dalton nanofiltration membranes, removes ginkgoic acid and inorganic salts in extracting solution,
It is concentrated into feed liquid 1/3, obtains trapped fluid；The Extraction solvent and water for using trapped fluid quality 1/3 respectively, to cutting in nanofiltration membrane system
Liquid is stayed to be washed, washing times are 4 times, and each wash time is 20min/ times.
(3) trapped fluid is concentrated into no ethyl alcohol, through ADS-17 macroporous resin purification, obtains refined solution；
Macroporous resin purification step are as follows: pass through 3 times of column volume washed with impurities, 2 times of 70% ethanol elutions of column volume obtain pure
Change liquid.
(4) refined solution is concentrated, is spray-dried, spraying intake air temperature 90 DEG C of air outlet temperature, obtains silver at 180 DEG C
Apricot leaf extract product.
It is not detected through ginkgoic acid in testing product, ash content 0.11%, total flavonoids content 29%, content yield
90.56%。
The above embodiments are only used to illustrate and not limit the technical solutions of the present invention, although referring to above-described embodiment to this hair
It is bright to be described in detail, those skilled in the art should understand that: still the present invention can be modified or be waited
With replacement, without departing from the spirit or scope of the invention, or any substitutions, should all cover in power of the invention
In sharp claimed range.
Claims (4)
1. the industrialized preparing process that a kind of low ginkgoic acid low ash divides ginkgo biloba p.e, it is characterised in that: the following steps are included:
(1) it takes ginkgo leaf to smash, Extraction solvent is added, stirring is extracted, and filtering obtains ginkgo extract；The Extracting temperature is 40-
50 DEG C, extraction time is 3 times, and extraction time is 1-2h/ times；Extraction solvent be solvent A and ethyl alcohol mixed solvent, solvent A with
The volume ratio of ethyl alcohol is 1:2-4；The solvent A is any one of butanone, acetone or ethyl acetate, and Extraction solvent volume is original
3-5 times for expecting quality, the volume unit are L, and the mass unit is kg；
(2) ginkgo extract is used into nanofiltration membrane, removes ginkgoic acid and inorganic salts in extracting solution, obtains trapped fluid；Institute
The molecular weight for stating nanofiltration membrane retention substance is 400-600 dalton；
(3) trapped fluid is obtained into refined solution through macroporous resin purification；
(4) refined solution is concentrated, is spray-dried, obtains ginkgo biloba p.e product, the silver in the ginkgo biloba p.e product
Apricot acid < 1ppm, ash content < 0.3%；
Trapped fluid in the step (2) need to be washed by nanofiltration membrane, and detergent is Extraction solvent and water, and washing dosage is retention
The 1/10-1/3 of liquid quality, washing times are 2-4 times.
2. a kind of low ginkgoic acid low ash according to claim 1 divides the industrialized preparing process of ginkgo biloba p.e, special
Sign is: the trapped fluid in the step (2) need to be washed by nanofiltration membrane, and each wash time is 10-20min/ times.
3. a kind of low ginkgoic acid low ash according to claim 1 or 2 divides the industrialized preparing process of ginkgo biloba p.e,
Be characterized in that: macroreticular resin is polar macroporous adsorption resin in the step (3)；Macropore on trapped fluid in the step (3)
No ethyl alcohol is concentrated into before resin.
4. a kind of low ginkgoic acid low ash according to claim 1 or 2 divides the industrialized preparing process of ginkgo biloba p.e,
It is characterized in that: macroporous resin purification step in the step (3) are as follows: washing amount is 1-3 times of column volume, and parsing dosage is column volume
2-5 times, it is described parsing solvent be 40-70% ethyl alcohol.
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| CN1515582A (en) * | 2003-01-08 | 2004-07-28 | 浙江康恩贝制药股份有限公司 | Preparation method of low-acid Ginkgo biloba extract |
| WO2005105122A1 (en) * | 2004-04-29 | 2005-11-10 | Goetect Gmbh | Ginkgo biloba extract and method for producing the same |
| CN101036631A (en) * | 2007-04-09 | 2007-09-19 | 上海同济生物制品有限公司 | Ginkgo leaves purified lyophiled powder preparing technique |
| CN103961381A (en) * | 2013-01-24 | 2014-08-06 | 中国林业科学研究院林产化学工业研究所 | Method for negative-pressure boiling extraction and preparation of low-acid ginkgo extract |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1515582A (en) * | 2003-01-08 | 2004-07-28 | 浙江康恩贝制药股份有限公司 | Preparation method of low-acid Ginkgo biloba extract |
| WO2005105122A1 (en) * | 2004-04-29 | 2005-11-10 | Goetect Gmbh | Ginkgo biloba extract and method for producing the same |
| CN101036631A (en) * | 2007-04-09 | 2007-09-19 | 上海同济生物制品有限公司 | Ginkgo leaves purified lyophiled powder preparing technique |
| CN103961381A (en) * | 2013-01-24 | 2014-08-06 | 中国林业科学研究院林产化学工业研究所 | Method for negative-pressure boiling extraction and preparation of low-acid ginkgo extract |
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