CN106729520A - A kind of preparation method of Ginger P.E - Google Patents
A kind of preparation method of Ginger P.E Download PDFInfo
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- CN106729520A CN106729520A CN201611153601.1A CN201611153601A CN106729520A CN 106729520 A CN106729520 A CN 106729520A CN 201611153601 A CN201611153601 A CN 201611153601A CN 106729520 A CN106729520 A CN 106729520A
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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
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/906—Zingiberaceae (Ginger family)
- A61K36/9068—Zingiber, e.g. garden ginger
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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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
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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
- A61K2236/30—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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Abstract
The invention discloses a kind of preparation method of Ginger P.E, mainly include the following steps that：1. ginger is cleaned, particle is cut into, 13 times of water of quality are added, stirring, heating controls 40 60 DEG C of temperature, add appropriate acid solution, regulation whole system pH value is between 36.Cellulase is added, cellulase and ginger ratio are 50u 600u：1g, digests 26 hours, filtering.2. relative density is concentrated the filtrate to for 1.10 1.20, ethanol solution is added in filtrate, whole solution ethanol concentration is reached 60% 80%, quiet to put 6 24 hours after stirring, filtering, concentration.This preparation method is simple, operation is simple, it is strong to amplify feasibility.
Description
Technical field
The present invention relates to a kind of method for preparing extractive of plant, and in particular to a kind of preparation method of Ginger P.E.
Background technology
Ginger is derived from the rhizome of Zingiber, and widely used in terms of biological medicine, Ginger P.E cannot be only used for orally
Therapy-related illness, it can also be used in external preparation, primarily serves effects of antiinflammation and bacteriostasis.The main active of ginger includes waving
Hair oil and gingerol two parts, and the main component of gingerol is 6- shogaols.《Chinese Pharmacopoeia》Also Ginger P.E is formulated
Respective standard.
Ginger can be higher with establishing in large scale, wide material sources, medical value in national most area.Generally make at home
Be used as medicine with its extract, the curative effect of the extract that the extremely complex different extracting mode of Ginger P.E component is obtained it is variant compared with
Greatly.And extracting factor is harsh or extraction step is cumbersome, differences between batches can be caused big, technique is unstable.In industrialization
During, this phenomenon is especially prominent.
A kind of freeze-drying is mentioned in CN102845754, ginger is crushed under the conditions of -20 DEG C, then extracted with microwave ethanol,
- 20 DEG C of pulverization conditions are very harsh in industrialization, it is difficult to industrialization.
The extraction to ginger domestic at present carries out more systematic research, main extracting method have steam method, milling process,
The methods such as solvent extraction method, super critical extraction, these methods are more or less all pure in certain defect, and steam method is carried
Take rate relatively low, power consumption is big, industrialization high cost；Milling process is most traditional extracting method, and recovery rate is extremely low；Solvent extraction will
Using to many organic solvents, high cost, industrialization danger coefficient is big；Super critical extraction is more new extraction side
Method, recovery rate is higher, but high cost, industrial device and working condition are harsh, and general producer is difficult with.
Ginger P.E is used to primarily serve antibacterial and seasoning effect in external preparation, obtained by different extraction processes
The fungistatic effect of Ginger P.E has larger difference.For current existing ginger extracting mode, the Ginger P.E of extraction
Fungistatic effect is not obvious, and utilization rate is relatively low.
The content of the invention
The present invention provides a kind of Ginger P.E preparation method for being easy to industrialization, and extract curative effect is substantially, between batch
Difference is small.
In order to solve the above problems, the solution of the present invention is as follows:
A kind of preparation method of Ginger P.E, comprises the following steps：
（1）Ginger is digested
Appropriate ginger is taken, broken ginger adds 1-3 times and measures（Quality weight）Water, stirring, heating, control temperature 40 DEG C -60 DEG C it
Between, acid solution is added, regulation pH value to 3.0-6.0 adds cellulose complex enzyme, and cellulase and ginger ratio are 50u-600u：
1g, digests 2-6 hours, filtering；
（2）Purification
Filtered fluid is concentrated into relative density for 1.10-1.20, high concentration ethanol solution is added in filtrate, make whole solution ethanol
Concentration reaches 60%-80%, quiet to put 6-24 hours after stirring, filtering, concentration.
The preparation method of above-mentioned Ginger P.E, described water is purified water or drinking water.
The preparation method of above-mentioned Ginger P.E, described broken ginger is that ginger is broken into the bulk less than 1cm particle diameters
Thing.
The preparation method of above-mentioned Ginger P.E, described temperature control between 40 DEG C -60 DEG C, preferably 45 DEG C -55
Between DEG C.
The preparation method of above-mentioned Ginger P.E, described acid solution is hydrochloric acid solution, phosphate solution, Acetate Solution
In one or several, preferred hydrochloric acid solution.
The preparation method of above-mentioned Ginger P.E, described pH value is adjusted to 3-6, preferably 4-5.
The preparation method of above-mentioned Ginger P.E, described enzymolysis time is 2-6 hours, preferably 3-5 hours.
The preparation method of above-mentioned Ginger P.E, described high concentration ethanol solution is 95% ethanol solution or absolute ethyl alcohol
Solution, the rank of 95% ethanol solution is food grade or pharmaceutical grade, and the rank of absolute ethyl alcohol is food grade or pharmaceutical grade.
Described relative density is《Chinese Pharmacopoeia》Upper described relative density, detection method is used《Chinese Pharmacopoeia》Upper rule
Fixed relative density detection method.
The preparation method of above-mentioned Ginger P.E, described concentration is concentrated by the way of vacuum distillation.
The beneficial effects of the present invention are：One kind is provided and is easy to industrialization, bacteriostatic activity is strong and suitable for externally applied product
Ginger P.E, the present invention is tentatively digested using cellulose enzyme to ginger, by the cellulase hydrolysis Cheng little Fen in ginger
Son, is easy to active ingredient to separate.Cellulose enzyme solution preocess is complicated, harsh to enzymatic hydrolysis condition requirement, and enzymolysis of the invention
Process condition is built upon being got in multiple experimental basis, and enzymolysis process has fairly good durability and controllability.Ginger
Effective ingredient is water insoluble, is soluble in organic solvent.The present invention carries out extraction separation using ethanol, extract effective active into
Point, while effective components of ginger destructible under high temperature, strong acid-base, of the invention to be digested under the conditions of more gentle pH,
Enzyme step is killed present invention eliminates high temperature simultaneously, effective components of ginger is greatly protected, Product Activity is improve.
There is larger advantage relative to milling process, steam distillation and organic solvent direct extraction method, specific point
Analysis is as follows：
Milling process：The main method that ginger effective ingredient is extracted by physical impact, because the peppery phenol of ginger, volatile oil etc. are small molecule
It is present in ginger, and it is all water insoluble, and fashion of extrusion extracts the less efficient of effective ingredient.
Steam distillation：The main volatile oil component that ginger is obtained by distillation, the yield of gingerol is less.
The direct extracting process of organic solvent：It is organic due to there is the obstruction of cellulose family and other molecules to effective ingredient
The extraction efficiency of solvent is greatly reduced.
The present invention is first passed through with the mode of cellulase degradation, and ginger is first processed, and enzymolysis process temperature is low, enzyme
Solution preocess reaction is thorough.Can be good at protection gingerol and volatile oil component is smoothly extracted, the pharmacological activity of extract
Height, is conducive to the application in terms of biological medicine, and this method carries out extraction separation, step using conventional technological means
Simply, operating process controllability is strong, can industrialization it is high.
Specific embodiment
Clean fresh ginger is taken, is dried, detection moisture is 10%, cellulase（ZY130412）From Shanghai purple one
Chemical reagent work, activity is：10000u/g.
Comparative example 1
The ginger 1.1kg for drying is taken, broken ginger is put into steam distillation device, distilled, and liquid to be condensed goes out liquid increasingly
When slow, stop distillation.Distillate is obtained, 201.3g is concentrated to give.
Comparative example 2
The ginger 1.1kg for drying is taken, broken ginger according to the operation of milling process, is extruded ginger liquid, is concentrated into about 203.5g.
Comparative example 3
The ginger 1.1kg for drying is taken, broken ginger is extracted 2 times with 95% ethanol, measures 95% ethanol for 4 times every time.Filtering, merges twice
Extract solution, is concentrated into 202.7g.
Embodiment 1
The ginger that 1.1kg is dried is weighed, broken ginger is put into enzymolysis container, adds 3 times of drinking water of amount, stirring, heating, control
Temperature is 60 DEG C, and PH most 6.0 is adjusted with watery hydrochloric acid, adds the cellulose complex enzyme of 60g, is digested 6 hours, and filtering, decompression is steamed
It is 1.19 to be distilled in hair device to solution relative density, adds appropriate absolute ethyl alcohol, solution ethanol concentration is reached 80%, is stirred,
Quiet to put 24 hours, filtering concentrates the filtrate to 206.2g.
Embodiment 2
The ginger that 1.1kg is dried is weighed, is shredded, be put into enzymolysis container, add 1 times of drinking water of amount, stirring, heating, control
Temperature is 40 DEG C, and PH most 4.0 is adjusted with watery hydrochloric acid, adds the cellulose complex enzyme of 5g, is digested 2 hours, and filtering is evaporated under reduced pressure
It is 1.11 to be distilled in device to solution relative density, adds 95% appropriate ethanol, solution ethanol concentration is reached 60%, and stirring is quiet
Put 6 hours, filter, concentrate the filtrate to 202.5g.
Embodiment 3
The ginger that 1.1kg is dried is weighed, is shredded, be put into enzymolysis container, add 2 times of drinking water of amount, stirring, heating, control
Temperature is 50 DEG C, and PH most 4.5 is adjusted with watery hydrochloric acid, adds the cellulose complex enzyme of 30g, is digested 4 hours, and filtering, decompression is steamed
It is 1.15 to be distilled in hair device to solution relative density, adds 95% appropriate ethanol, solution ethanol concentration is reached 70%, is stirred,
Quiet to put 12 hours, filtering concentrates the filtrate to 200.8g.
Embodiment 4
The ginger that 1.1kg is dried is weighed, is shredded, be put into enzymolysis container, add 3 times of drinking water of amount, stirring, heating, control
Temperature is 50 DEG C, and PH most 4.5 is adjusted with watery hydrochloric acid, adds the cellulose complex enzyme of 10g, is digested 6 hours, and filtering, decompression is steamed
It is 1.14 to be distilled in hair device to solution relative density, adds 95% appropriate ethanol, solution ethanol concentration is reached 70%, is stirred,
Quiet to put 18 hours, filtering concentrates the filtrate to 201.4g.
Embodiment 5
The ginger that 1.1kg is dried is weighed, is shredded, be put into enzymolysis container, add 1 times of drinking water of amount, stirring, heating, control
Temperature is 50 DEG C, and PH most 4.5 is adjusted with watery hydrochloric acid, adds the cellulose complex enzyme of 40g, is digested 2 hours, and filtering, decompression is steamed
It is 1.15 to be distilled in hair device to solution relative density, adds 95% appropriate ethanol, solution ethanol concentration is reached 70%, is stirred,
Quiet to put 12 hours, filtering concentrates the filtrate to 203.8g.
Embodiment 6
The ginger that 1.1kg is dried is weighed, is shredded, be put into enzymolysis container, add 2 times of drinking water of amount, stirring, heating, control
Temperature is 50 DEG C, and PH most 4.5 is adjusted with watery hydrochloric acid, adds the cellulose complex enzyme of 50g, is digested 4 hours, and hydrolysis temperature is 50
DEG C, filtering, it is 1.16 to be distilled in decompression evaporator to solution relative density, adds 95% appropriate ethanol, makes solution ethanol concentration
70% is reached, stirring is quiet to put 12 hours, filtering concentrates the filtrate to 202.5g.
The suppression of the Ginger P.E obtained by above-mentioned comparative examples and embodiment is detected using cylinder-plate method and filter paper enzyme
Bacterium effect, specific method is as follows：
Solvent：20% ethanol（Due to the peppery phenol of ginger effective ingredient ginger and volatilization, oil does not dissolve in water, therefore molten with a certain proportion of ethanol
Liquid）.
Culture medium（From the extensive and profound in meaning star Bioisystech Co., Ltd in Beijing）：Beef peptone culture medium（Bacterium is used）；Horse
Bell potato glucose sugar agar medium（Fungi is used）.
Main agents：Absolute ethyl alcohol（Hunan Er-kang Pharmaceutical Co., Ltd.）.
Strain（Chinese microorganism strain collection）：Escherichia coli, golden yellow glucose coccus, saccharomyces cerevisiae, Penicillium citrinum,
aspergillus, Sharpe typhoid bacillus.
Actication of culture：All strain transposings for test are entered on corresponding test tube slant culture medium, it is every kind of to connect three, carefully
Bacterium puts culture 18-24h in 37 DEG C of constant incubators；Brewer's yeast, Penicillium citrinum, aspergillus place 28 DEG C of insulating boxs in, culture 48
DEG C hour.
Cylinder-plate method operating process
2 parts of the various embodiments described above extract being taken respectively, being diluted with 20% ethanol, ultrasound 10 minutes, fully dissolving are diluted to respectively
200mg/ml, takes supernatant as test liquid.
Respectively by the examination loaded on 20*200mm kinds respectively of beef peptone culture medium and potato dextrose agar
Guan Zhong, every 15ml, is cooled to 48-50 DEG C after sterilizing, be separately added into above-mentioned experiment bacteria suspension 0.1ml.Plate is down flat after mixing, often
Strain test organisms is repeated 3 times.With 4 stainless steel Oxford rings of equidistant uniform placement, internal diameter in each flat board（6.0+0.1）Mm,
It is high（10.0+0.1）Mm, external diameter（8.0+0.1）mm.Drop fills test liquid sample respectively in sequence.It is blank with 20% ethanol solution
Control solvent, is covered with ceramic dome, and after spreading 2h in 0-4 DEG C of refrigerator, bacterium cultivates 24 hours, yeast under the conditions of 37 DEG C
Bacterium and mould are cultivated 48 hours under the conditions of 28 DEG C, detect each inhibition zone.
Filter paper enzyme operating process
The culture medium that will have been configured sterilizes by high-pressure sterilizing pot, is cooled to 50 DEG C -60 DEG C, and sterile working is poured into hot air sterilization
Culture dish in, each culture dish pours into about 10ml-15ml.Thickness about 1.5ml in culture dish.Dipped in respectively with aseptic cotton carrier
Various bacteria suspensions are taken, is equably applied to various containing suitable culture dish surface, put in 37 DEG C of incubators and taken out after 15min, mesh
The agar surface that makes dry, it is stand-by, take out through after hot air sterilization filtrate of uniform size justify the scraps of paper, above-mentioned mixing is put respectively and is carried
Take in liquid, soak 10 minutes, with aseptic nipper tweezer filter paper dick, be put into containing on surface plate by sterile working.Every kind of bacterium is cooked 3
Ware, each surface plate sticks a filter paper dick at a certain distance（Result seeks its average value）.Then each surface plate is put
Enter culture in incubator（37 DEG C of bacterium, cultivates 24 hours.28 DEG C of mould, cultivates 48 hours）, take out detect each surface plate in
Inhibition zone size.
Testing result such as following table：
The cylinder-plate method of table 1. detects the antibacterial result statistical form of Ginger P.E
The filter paper enzyme of table 2. detects the antibacterial result statistical form of Ginger P.E
Remarks：Numeral in above table is the bacterium loop diameter size of bacterium, and unit is millimeter, the numeral in filter paper detection method
Diameter including filter paper.
From above-mentioned test data analyzer, Ginger P.E of the invention is in terms of antibacterial activity compared with other traditional methods
It is good, and the present invention is easy to operate, it is easy to industrialization production, with very strong economic results in society.
Claims (9)
1. a kind of preparation method of Ginger P.E, comprises the following steps：
（1）Ginger is digested：Appropriate ginger is taken, broken ginger adds 1-3 times and measures（Quality weight）Water, stirring, heating, control temperature
Between 40 DEG C -60 DEG C, acid solution is added, regulation pH value to 3.0-6.0 adds cellulose complex enzyme, cellulase and ginger ratio
Example is 50u-600u：1g, digests 2-6 hours, filtering；（2）Purification：Relative density is concentrated the filtrate to between 1.10-1.20,
Ethanol solution is added in filtrate, whole solution ethanol concentration is reached 60%-80%, quiet to put 6-24 hours after stirring, filtering is dense
Contracting.
2. the preparation method of Ginger P.E according to claim 1, it is characterised in that：Water used be purified water or
Drinking water.
3. the preparation method of Ginger P.E according to claim 1, it is characterised in that：Ginger is broken into less than 1cm particle diameters
Block.
4. the preparation method of Ginger P.E according to claim 1, it is characterised in that：Temperature is 45 DEG C -55 DEG C.
5. the preparation method of Ginger P.E according to claim 1, it is characterised in that：The acid solution of enzymolysis process is hydrochloric acid
One or several in solution, phosphate solution, Acetate Solution, preferably hydrochloric acid solution.
6. the preparation method of Ginger P.E according to claim 1, it is characterised in that：PH value is adjusted to 4-5.
7. the preparation method of Ginger P.E according to claim 1, it is characterised in that：Enzymolysis time is 3-5 hours.
8. the thing preparation method of Ginger P.E according to claim 1, it is characterised in that：Ethanol solution is 95% ethanol
Solution or ethanol solution, the rank of 95% ethanol solution is food grade or pharmaceutical grade, and the rank of absolute ethyl alcohol is food grade
Or pharmaceutical grade.
9. the preparation method of Ginger P.E according to claim 1, it is characterised in that：Described condensing mode is used and subtracted
The mode of distillation is pressed to be concentrated.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107595743A (en) * | 2017-10-10 | 2018-01-19 | 胡江宇 | A kind of ginger preparation method of composition for antibacterial |
| CN107594286A (en) * | 2017-10-10 | 2018-01-19 | 胡江宇 | A kind of preservative containing ginger composition |
| CN107647032A (en) * | 2017-11-14 | 2018-02-02 | 安徽华健生物科技有限公司 | A kind of processing method of jujube shredded ginger tea |
| CN108484378A (en) * | 2018-03-26 | 2018-09-04 | 常德金德新材料科技股份有限公司 | The extracting method of gingerol in a kind of ginger |
| CN113730315A (en) * | 2020-05-28 | 2021-12-03 | 株式会社一集募娥 | Ginger water composition containing ginger extract and preparation method thereof |
-
2016
- 2016-12-14 CN CN201611153601.1A patent/CN106729520A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| K.L. NAGENDRA CHARI等: "Enzyme-assisted extraction of bioactive compounds from ginger(Zingiber officinale Roscoe)", 《FOOD CHEMISTRY》 * |
| 徐丽萍等: "纤维素酶-超声辅助提取姜辣素的工艺优化", 《中国调味品》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107595743A (en) * | 2017-10-10 | 2018-01-19 | 胡江宇 | A kind of ginger preparation method of composition for antibacterial |
| CN107594286A (en) * | 2017-10-10 | 2018-01-19 | 胡江宇 | A kind of preservative containing ginger composition |
| CN107647032A (en) * | 2017-11-14 | 2018-02-02 | 安徽华健生物科技有限公司 | A kind of processing method of jujube shredded ginger tea |
| CN108484378A (en) * | 2018-03-26 | 2018-09-04 | 常德金德新材料科技股份有限公司 | The extracting method of gingerol in a kind of ginger |
| CN113730315A (en) * | 2020-05-28 | 2021-12-03 | 株式会社一集募娥 | Ginger water composition containing ginger extract and preparation method thereof |
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