CN107915613A - A kind of preparation method of shampoo ginger gingerol - Google Patents
A kind of preparation method of shampoo ginger gingerol Download PDFInfo
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- CN107915613A CN107915613A CN201711357418.8A CN201711357418A CN107915613A CN 107915613 A CN107915613 A CN 107915613A CN 201711357418 A CN201711357418 A CN 201711357418A CN 107915613 A CN107915613 A CN 107915613A
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- gingerol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/35—Ketones, e.g. benzophenone
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/005—Antimicrobial preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/02—Preparations for cleaning the hair
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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- Chemical & Material Sciences (AREA)
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- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
A kind of preparation method the invention discloses shampoo with ginger gingerol, is related to chemical product preparing technical field.Head of the invention fast and efficiently extracts ginger gingerol using superfine communication technique and microwave ultrasonic wave auxiliary eutectic reagent abstraction technique from ginger；Then aqueous two phase extraction technique and supercritical CO are used successively2Abstraction technique is extracted and purified to gingerol in ginger；Finally by the solvent in extract be evaporated shampoo people's ginger gingerol.The preparation method of the present invention is easy to operate and environmentally protective, convenient and efficient and extraction efficiency is high, and obtained extract gingerol purity is high, and is free of organic solvent, skin compatibility is good, may be directly applied to assign shampoo antibacterial, antipruritic, Anti-hair loss and other effects in shampoo.
Description
Technical field
The present invention relates to the preparation method of chemical product preparing technical field, specially a kind of shampoo ginger gingerol.
Background technology
Shampoo also known as shampoo, are a kind of hair care articles with anti-dandruff, treatment oil and hair dyeing etc., are most common
Hair cosmetic, belongs to personal care market and develops earliest and one of most fast product.Early stage shampoo is hair and head
The detergent of skin, with formula, the development of technique, the product efficacy of shampoo will be more and more important, specific function and auxiliary work(
It will can constantly refine, moisten nutrition, improve an important factor for hair quality has become measurement shampoo.Except traditional anti-dandruff, anticreep
Hair etc., sun-proof, treatment oil, profit hair, it is disposable, without silicone oil, extraction, plant essence, Chinese herbal medicine the concept such as are nursed one's health and are also permeated one after another naturally
To hair washing field, become the new highlight of shampoo.
Ginger is the new fresh quench stem of ginger ginger.Research shows that ginger extract has anti-inflammatory, antimycotic effect, can
For treating infection caused by trichophyte, pityrosporum furfur, ringworm of the foot bacterium etc., it can also be used to seborrhagia disease and dandruff.Gingerol
It is one of principle active component of ginger, has and promote skin of head blood circulation, effectively anti-alopecia-stopping, suppresses the work of scalp pruritus
With.These researchs show that ginger extract is wanted in will having the function that in shampoo.But current most of ginger Capsaicin
The preparation method of extract uses substantial amounts of organic solvent, not only pollutes environment, while obtained extracting solution cannot be directly used to
In shampoo.Therefore, a kind of preparation method tool of a kind of environmentally protective and safe and efficient shampoo ginger extract is developed
There is important meaning.
The content of the invention
The present invention solves the problems, such as to there is provided a kind of preparation method of shampoo ginger gingerol, preparation of the invention
Method is easy to operate and environmentally protective, and convenient and efficient and extraction efficiency is high, and obtained extract gingerol purity is high, and does not contain
Solvent, skin compatibility is good, may be directly applied to assign shampoo antibacterial, antipruritic, Anti-hair loss and other effects in shampoo..
To solve the above problems, the present invention provides following technical solution：A kind of preparation side of shampoo ginger gingerol
Method, it is characterised in that comprise the following steps：
（（1）After taking a certain amount of hydrogen bond receptor to be mixed with hydrogen-bond donor according to certain molar ratio, in 80 DEG C -100 DEG C,
Agitating and heating for a period of time, forms the eutectic reagent of transparent and homogeneous under the conditions of 400-600rpm/min；
（2）After fresh ginger is cleaned, after the water on surface is dried, after section, dried extremely in 50-65 DEG C of vacuum drying chamber
After constant weight, 60 mesh sieves excessively are further ground into nanoscale micropowders after medicinal herb grinder crushes；
（3）After taking 8kg ginger nanoscale micropowders to be mixed with eutectic reagent-water mixed solvent, in 200-400W ultrasound work(
Rate, is obtained by filtration clear liquid under the conditions of the microwave power of 100-200W and 35-50 DEG C, residue is again after microwave-ultrasound 20-40min
Merge supernatant after being extracted 2-3 times with eutectic reagent-water mixed solvent, it is thick to obtain gingerol after being concentrated under reduced pressure into supernatant
Extract；
（4）Add salting liquid spiral type into after aqueous two-phase to gingerol crude extract, will upper phase take out after after vacuum distillation concentration,
Ethanol is added in upper phase eutectic agent precipitate is recycled into eutectic reagent, while by gingerol dissolving in ethanol, by ethanol
After mutually taking out the gingerol extract of preliminary purification is obtained after vacuum distillation drying；
（5）The gingerol extract of preliminary purification is transferred to supercritical CO2In extraction equipment, in 20-28MPa of pressure, extraction
Temperature is 40-60 DEG C, and alcohol-water is entrainer, the flow of fluid be 25~30L/h under the conditions of to ginsenoside extract into
After the purifying extraction of one step, after removing the solvent in extract, up to shampoo ginger gingerol.
Further, step（1）Described in hydrogen bond receptor be choline chloride, glycine betaine, one kind in l-cn；Hydrogen
Key donor is one or both of glucose, glycerine, urea, lactic acid, water；The hydrogen bond receptor and mole of hydrogen-bond donor
Than for 1：2；The heating time is 1-2h.
Further, step（2）Described in ginger slice thickness must not exceed 2mm；The nanoscale micropowders
Average grain diameter is not greater than 1um.
Further, step（3）Described in eutectic reagent-water mixed solvent in eutectic reagent account for cumulative volume ratio and be
40-75%；The ginger nanoscale micropowders are 1 with eutectic reagent-water mixed solvent mass volume ratio:15-20；Institute
It is 1.15-1.25g/mL to state concentrated solution density.
Further, step（4）Described in salting liquid be ammonium sulfate, sodium sulphate, sodium citrate and dipotassium hydrogen phosphate
In one kind；The concentration of the salting liquid is 0.25-0.5g/mL；The addition of the salting liquid is 35-50%.
Further, step（5）Described in entrainer in ethanol account for 50-65%.
Further, step（5）Described in shampoo with gingerol total content in ginger gingerol be not less than 80%.
As a result of above-mentioned preparation method, the present invention has the advantages that compared with prior art：
The present invention is given birth to using superfine communication technique, microwave ultrasonic wave auxiliary eutectic reagent abstraction technique using ultrasonic destruction
Plant cell wall in ginger fine powder accelerates the leaching rate of active ingredient, improves extraction efficiency, shortens operating time and reduction
The use of organic solvent, it is more environmentally protective；Ginger crude extract is carried out using eutectic reagent-salt aqueous two phase extraction technique
Purifying, different using partition coefficient remove highly polar compound in extract；Utilize supercritical CO2Abstraction technique is to people
Conopsea extraction is further purified to obtain high-purity gingerol extract；This method is environmentally protective, easy to operate, and what is obtained carries
Take thing gingerol concentration high.It can be directly used in through ginsenoside extract produced by the present invention in shampoo.
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment one
Take a certain amount of choline chloride with glycerine according to 1：After 2 molar ratio mixing, in 80 DEG C, stirred under the conditions of 500rpm/min
Heating 1h is mixed, forms the eutectic reagent of transparent and homogeneous；After fresh ginger is cleaned, after the water on surface is dried, thickness is cut into
After section of the degree less than 2mm, dried in 55 DEG C of vacuum drying chambers to constant weight, 60 mesh sieves are crossed after medicinal herb grinder crushes
Further it is ground into nanoscale micropowders；Take 8kg ginger nanoscale micropowders low with 65% choline chlorides of 150L-glycerine
After the mixing of congruent melting reagent-water mixed solvent, in 400W ultrasonic powers, microwave under the conditions of the microwave power of 150W and 35 DEG C-super
Clear liquid is obtained by filtration after sound 30min, residue merges supernatant after being extracted 2 times with eutectic reagent-water mixed solvent again, to supernatant
The gingerol crude extract that density is 1.15g/mL is obtained after being concentrated under reduced pressure in liquid；45% 0.25g/ is added to ginsenoside crude extract
ML metabisulfite solutions spiral type into after aqueous two-phase, will upper phase take out after depressurize inspissation contracting after, adding ethanol in upper phase will be low common
Molten agent precipitate recycling eutectic reagent, while by gingerol dissolving in ethanol, vacuum distillation drying after ethanol is mutually taken out
The gingerol extract of preliminary purification is obtained afterwards；The gingerol extract of preliminary purification is transferred to supercritical CO2Extraction equipment
In, in pressure 25MPa, Extracting temperature is 40 DEG C, and 55% alcohol-water is entrainer, and the flow of fluid is right under the conditions of 25L/h
After extraction is further purified in ginsenoside extract, after removing the solvent in extract, given birth to up to the shampoo that purity is 88%
Ginger gingerol.
Embodiment two
Take a certain amount of glycine betaine with ethylene glycol according to 1：After 2 molar ratio mixing, in 80 DEG C, stirred under the conditions of 400rpm/min
Heating 1h is mixed, forms the eutectic reagent of transparent and homogeneous；After fresh ginger is cleaned, after the water on surface is dried, thickness is cut into
After section of the degree less than 2mm, dried in 55 DEG C of vacuum drying chambers to constant weight, 60 mesh sieves are crossed after medicinal herb grinder crushes
Further it is ground into nanoscale micropowders；Take 8kg ginger nanoscale micropowders low with 60% glycine betaines of 160L-ethylene glycol
After the mixing of congruent melting reagent-water mixed solvent, in 500W ultrasonic powers, microwave under the conditions of the microwave power of 100W and 40 DEG C-super
Clear liquid is obtained by filtration after sound 25min, residue merges supernatant after being extracted 3 times with eutectic reagent-water mixed solvent again, to supernatant
The gingerol crude extract that density is 1.18g/mL is obtained after being concentrated under reduced pressure in liquid；40% 0.35g/ is added to ginsenoside crude extract
ML sodium citrate solutions spiral type into after aqueous two-phase, will upper phase take out after depressurize inspissation contracting after, adding ethanol in upper phase will be low
Congruent melting agent precipitate recycles eutectic reagent, while by gingerol dissolving in ethanol, after ethanol is mutually taken out is evaporated under reduced pressure dry
The gingerol extract of preliminary purification is obtained after dry；The gingerol extract of preliminary purification is transferred to supercritical CO2Extraction dress
In putting, in pressure 26MPa, Extracting temperature is 40 DEG C, and 60% alcohol-water is entrainer, and the flow of fluid is under the conditions of 24L/h
After extraction is further purified to ginsenoside extract, after removing the solvent in extract, used up to the shampoo that purity is 86%
Ginger gingerol.
Embodiment three
Take a certain amount of l-cn with ethylene glycol according to 1：After 2 molar ratio mixing, in 90 DEG C, under the conditions of 500rpm/min
Agitating and heating 1.5h, forms the eutectic reagent of transparent and homogeneous；After fresh ginger is cleaned, after the water on surface is dried, cut
After section into thickness less than 2mm, dried in 55 DEG C of vacuum drying chambers to constant weight, 60 are crossed after medicinal herb grinder crushes
Mesh sieve is further ground into nanoscale micropowders；Take 8kg ginger nanoscale micropowders and 70% l-cns of 150L-second
It is micro- under the conditions of the microwave power of 150W and 40 DEG C in 400W ultrasonic powers after the mixing of glycol eutectic reagent-water mixed solvent
Clear liquid is obtained by filtration after ripple-ultrasound 25min, residue merges supernatant after being extracted 3 times with eutectic reagent-water mixed solvent again,
The gingerol crude extract that density is 1.15g/mL is obtained after being concentrated under reduced pressure into supernatant；45% is added to ginsenoside crude extract
0.35g/mL dipotassium hydrogen phosphate solutions spiral type into after aqueous two-phase, will upper phase take out after depressurize inspissation contracting after, added in upper phase
Eutectic agent precipitate is recycled eutectic reagent by ethanol, while by gingerol dissolving in ethanol, is subtracted after ethanol is mutually taken out
The gingerol extract of preliminary purification is obtained after pressure distillation is dry；The gingerol extract of preliminary purification is transferred to overcritical
CO2In extraction equipment, in pressure 25MPa, Extracting temperature is 35 DEG C, and 70% alcohol-water is entrainer, and the flow of fluid is 25L/
It is 87% up to purity after removing the solvent in extract after extraction is further purified to ginsenoside extract under h condition
Shampoo ginger gingerol.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of changes, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (7)
1. a kind of shampoo preparation method of ginger gingerol, it is characterised in that comprise the following steps：
（1）After taking a certain amount of hydrogen bond receptor to be mixed with hydrogen-bond donor according to certain molar ratio, in 80 DEG C -100 DEG C, 400-
Agitating and heating for a period of time, forms the eutectic reagent of transparent and homogeneous under the conditions of 600rpm/min；
（2）After fresh ginger is cleaned, after the water on surface is dried, after section, dried extremely in 50-65 DEG C of vacuum drying chamber
After constant weight, 60 mesh sieves excessively are further ground into nanoscale micropowders after medicinal herb grinder crushes；
（3）After taking 8kg ginger nanoscale micropowders to be mixed with eutectic reagent-water mixed solvent, in 200-400W ultrasound work(
Rate, is obtained by filtration clear liquid under the conditions of the microwave power of 100-200W and 35-50 DEG C, residue is again after microwave-ultrasound 20-40min
Merge supernatant after being extracted 2-3 times with eutectic reagent-water mixed solvent, it is thick to obtain gingerol after being concentrated under reduced pressure into supernatant
Extract；
（4）Add salting liquid spiral type into after aqueous two-phase to gingerol crude extract, will upper phase take out after after vacuum distillation concentration,
Ethanol is added in upper phase eutectic agent precipitate is recycled into eutectic reagent, while by gingerol dissolving in ethanol, by ethanol
After mutually taking out the gingerol extract of preliminary purification is obtained after vacuum distillation drying；
（5）The gingerol extract of preliminary purification is transferred to supercritical CO2In extraction equipment, in 20-28MPa of pressure, extraction
Temperature is 40-60 DEG C, and alcohol-water is entrainer, the flow of fluid be 25~30L/h under the conditions of to ginsenoside extract into
After the purifying extraction of one step, after removing the solvent in extract, up to shampoo ginger gingerol.
A kind of 2. preparation method of shampoo ginger gingerol according to claim 1, it is characterised in that step（1）In
The hydrogen bond receptor is choline chloride, one kind in glycine betaine, l-cn；Hydrogen-bond donor for glucose, glycerine, urea,
One or both of lactic acid, water；The hydrogen bond receptor and the molar ratio of hydrogen-bond donor are 1:2；The heating time is
1-2h。
A kind of 3. preparation method of shampoo ginger gingerol according to claim 1, it is characterised in that step（2）In
The ginger slice thickness must not exceed 2mm；The nanoscale micropowders average grain diameter is not greater than 1um.
A kind of 4. preparation method of shampoo ginger gingerol according to claim 1, it is characterised in that step（3）In
It is 40-75% that eutectic reagent, which accounts for cumulative volume ratio, in the eutectic reagent-water mixed solvent；The ginger nanoscale surpasses
Fine powder is 1 with eutectic reagent-water mixed solvent mass volume ratio:15-20；The concentrated solution density is 1.15-1.25g/
mL。
A kind of 5. preparation method of shampoo ginger gingerol according to claim 1, it is characterised in that step（4）In
The salting liquid is one kind in ammonium sulfate, sodium sulphate, sodium citrate and dipotassium hydrogen phosphate；The concentration of the salting liquid is
0.25-0.5g/mL；The addition of the salting liquid is 35-50%.
A kind of 6. preparation method of shampoo ginger gingerol according to claim 1, it is characterised in that step（5）In
Ethanol accounts for 50-65% in the entrainer.
A kind of 7. preparation method of shampoo ginger gingerol according to claim 1, it is characterised in that step（5）In
The shampoo is not less than 80% with gingerol total content in ginger gingerol.
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| CN201711357418.8A CN107915613A (en) | 2017-12-16 | 2017-12-16 | A kind of preparation method of shampoo ginger gingerol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111995509A (en) * | 2020-07-31 | 2020-11-27 | 株洲千金药业股份有限公司 | Preparation method of gingerol |
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|---|---|---|---|---|
| CN102101876A (en) * | 2010-11-23 | 2011-06-22 | 苏州派腾生物医药科技有限公司 | Preparation method of arctiin |
| CN106963700A (en) * | 2017-05-23 | 2017-07-21 | 林燕 | A kind of extracting method of winter jasmine active ingredient |
| CN106977580A (en) * | 2017-05-23 | 2017-07-25 | 林燕 | A kind of extracting method of natural high-purity tea saponin |
| CN107184461A (en) * | 2017-05-23 | 2017-09-22 | 林燕 | A kind of extracting method of pawpaw polyphenol |
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2017
- 2017-12-16 CN CN201711357418.8A patent/CN107915613A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102101876A (en) * | 2010-11-23 | 2011-06-22 | 苏州派腾生物医药科技有限公司 | Preparation method of arctiin |
| CN106963700A (en) * | 2017-05-23 | 2017-07-21 | 林燕 | A kind of extracting method of winter jasmine active ingredient |
| CN106977580A (en) * | 2017-05-23 | 2017-07-25 | 林燕 | A kind of extracting method of natural high-purity tea saponin |
| CN107184461A (en) * | 2017-05-23 | 2017-09-22 | 林燕 | A kind of extracting method of pawpaw polyphenol |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111995509A (en) * | 2020-07-31 | 2020-11-27 | 株洲千金药业股份有限公司 | Preparation method of gingerol |
| CN111995509B (en) * | 2020-07-31 | 2023-04-14 | 株洲千金药业股份有限公司 | Preparation method of gingerol |
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Application publication date: 20180417 |