CN109675002A - The extraction process of general gingerol - Google Patents

The extraction process of general gingerol Download PDF

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Publication number
CN109675002A
CN109675002A CN201910092793.7A CN201910092793A CN109675002A CN 109675002 A CN109675002 A CN 109675002A CN 201910092793 A CN201910092793 A CN 201910092793A CN 109675002 A CN109675002 A CN 109675002A
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ginger powder
added
acetone
general gingerol
eluent
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呼永河
肖雯婧
侯君
陈欣
温旭东
刘敏超
周先礼
单连海
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Western Theater General Hospital of PLA
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Western Theater General Hospital of PLA
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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
    • 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
    • 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
    • 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
    • A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
    • 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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Abstract

The invention discloses a kind of extraction processes of general gingerol, comprising the following steps: extracts and is concentrated Step 1: solvent is added into ginger powder, obtains medicinal extract；Step 2: medicinal extract is separated using column chromatography, eluent system is petroleum ether-acetone, eluent when eluent and petroleum ether-acetone volume ratio when collection petroleum ether-acetone volume ratio is 7~5:1 are 4~2:1, merges eluent and is simultaneously concentrated, obtain general gingerol；Ginger powder the preparation method comprises the following steps: rhizoma zingiberis is crushed, as ginger powder；The amount ratio of ginger powder and solvent is 1kg:3-5L；Solvent is that methylene chloride, ethyl acetate, acetone, ether or volume fraction are one of ethanol solution of 50-95%.In the extraction process of general gingerol of the present invention, column chromatography is carried out to medicinal extract by using petroleum ether-acetone of different volumes ratio, has obtained the general gingerol of high-purity.

Description

The extraction process of general gingerol
Technical field
The present invention relates to the preparation fields of Ginger P.E.It is more particularly related to a kind of extraction of general gingerol Technique.
Background technique
Ginger and rhizoma zingiberis are respectively the fresh rhizome or and dry rhizome of zingiberaceous plant.Ginger can season, and energy diseases prevention is strong Body.Root it is documented that, ginger can be used guard against a variety of diseases, such as alleviate arthralgia, reducing blood lipid, blood pressure lowering, prevention cardiac muscle A variety of symptoms such as infraction.In ginger or rhizoma zingiberis, general gingerol is one of main activity.
Currently, being often used solvent extraction method, multiple solvent extraction from the technique for extracting general gingerol in ginger or rhizoma zingiberis The methods of method, recrystallization, squeezing method are purified after extracting using macroreticular resin, the purity of obtained general gingerol compared with It is low, increase the production cost of general gingerol.
Summary of the invention
It is an object of the invention to solve at least the above problems, and provide the advantages of at least will be described later.
It is a still further object of the present invention to provide a kind of extraction processes of general gingerol, by using the stone of different volumes ratio Oily ether-acetone chromatographs medicinal extract column, has obtained the general gingerol of high-purity.
In order to realize these purposes and other advantages according to the present invention, a kind of extraction process of general gingerol is provided, is wrapped Include following steps:
It extracts and is concentrated Step 1: solvent is added into ginger powder, obtain medicinal extract；
Step 2: medicinal extract is separated using column chromatography, eluent system is petroleum ether-acetone, collects petroleum ether-acetone Eluent when eluent and petroleum ether-acetone volume ratio when volume ratio is 7~5:1 is 4~2:1, merging eluent are simultaneously dense Contracting, obtains general gingerol.
Preferably, in step 1 ginger powder the preparation method comprises the following steps: rhizoma zingiberis is crushed, as ginger powder.
Preferably, the amount ratio of ginger powder and solvent is 1kg:3-5L in step 1.
Preferably, it is 50- that solvent, which is methylene chloride, ethyl acetate, acetone, ether or volume fraction, in step 1 One of 95% ethanol solution.
Preferably, the extracting method in step 1 is cold soaking extraction or refluxing extraction, wherein the time that cold soaking extracts For 24~96h, the time of refluxing extraction is 1~3h.
Preferably, the ginger powder in step 1 is pre-processed, pretreated detailed process are as follows:
S1, the methanol that 10 times of its gross mass amounts are added into ginger powder, and it is ultrasonically treated 1h, obtain turbid；
S2, the sand material for taking 20 times of ginger powder gross mass amounts, the sodium-chloride water solution that the mass fraction of 8 times of amounts is 10% mix, Stir-fry 20min under the conditions of being placed in 40~50 DEG C, obtains mixing, wherein the partial size of minimum sand material is greater than ginger powder particle in ginger powder Diameter；
S3, stir-fry mixing under the conditions of 60~65 DEG C, while turbid is added in equivalent in five times, after turbid is added, after Continuous stir-frying 1h, obtains stir-frying material；
S4, stir-frying material is separated by sieve, obtains sand layer and ginger powder layer, sand layer is rushed with methanol Wash, obtain washing lotion, by washing lotion it is laminated with ginger powder and and be concentrated, obtain pretreatment ginger powder, wherein the mesh of sieve is round knot Structure, the diameter of mesh is between the diameter of ginger powder particle in ginger powder and the particle size of minimum sand material.
Preferably, solvent is added in step 1 into ginger powder to extract and be concentrated, detailed process are as follows:
Then 5 times of ginger powder gross mass amounts are added in A1, the tetrahydrofuran for taking 10 times of ginger powder gross mass amounts into tetrahydrofuran Gas-phase silica is placed in 50 DEG C, stirs 10min under conditions of 400r/min, then under conditions of 60 DEG C, 400r/min dropwise The sulfuric acid solution of the 4M of 1 times of ginger powder gross mass amount is added, is added dropwise to sulfuric acid solution, continues to stir 20min again in seven times etc. The silane coupling agents of 6 times of ginger powder gross mass amounts are added in amount, are placed in 70 DEG C, stir 1h under conditions of 400r/min, filter, obtain Solid finally rinses solid with the ethanol solution of mass fraction 95%, and dries 6h under the conditions of solid is placed in 60 DEG C, is changed Property gas-phase silica, wherein silane coupling agent be (HO)3Si(CH2)3N(CH2PO3H2)2；
A2, acetic acid is added into solvent, the PH for adjusting solvent is 5~6, and modified gas-phase silica is then added, is placed in 50 DEG C, stir 20min under conditions of 400r/min, be cooled to room temperature, add ginger powder and extract, filter, obtain the first filter Liquid and filter residue, the methanol that 4 times of filter residue gross mass amounts are added into filter residue impregnate 15h, the second filtrate are obtained by filtration；
A3, the first filtrate, the second filtrate are merged and is concentrated, obtain medicinal extract.
The present invention is include at least the following beneficial effects:
The first, by the present invention in that being chromatographed with petroleum ether-acetone of different volumes ratio to medicinal extract column, general gingerol can be improved Purity, meanwhile, petroleum ether-acetone of different volumes ratio can also reduce residual of the general gingerol in silicagel column, improve general gingerol Recovery rate.
The second, ginger powder is pre-processed, and effectively increases the recovery rate of cell-wall breaking ratio and general gingerol；By the way that methanol is added Make ginger powder dispersion in methyl alcohol, convenient for mixing with the uniform of sand material, improves cell-wall breaking ratio；Sand material is added, during stir-frying Ginger powder and the friction of sand material may advantageously facilitate breaking-wall cell, and then improve recovery rate, and sodium chloride, which is added, facilitates breaking-wall cell；Sand Sublayer is rinsed with methanol, and avoidable general gingerol is bonded on sand, reduces the loss of general gingerol.
Modified gas-phase silica is added into solvent for third, make ginger powder cold soaking extract or refluxing extraction in ginger powder with Gas-phase silica rubs, and improves cell-wall breaking ratio, and then improve the recovery rate of general gingerol；Sulfuric acid is added and is convenient for gas phase hard charcoal Black surface forms silicone hydroxyl, promotes to form stable silicon oxygen silicon key between gas-phase silica and silane coupling agent, several times equivalent Silane coupling agent, which is added, can reduce the probability that silane coupling agent itself is condensed, and improve the utilization rate of silane coupling agent；It uses (HO)3Si(CH2)3N(CH2PO3H2)2Gas-phase silica is modified, gas-phase silica on the one hand can be improved in solvent Dispersibility, increase contact of the ginger powder with gas-phase silica, improve cell-wall breaking ratio, on the other hand using silane coupling agent to gas Phase white carbon black is modified, and can reduce absorption of the gas-phase silica to general gingerol, convenient for the separation of general gingerol and gas-phase silica, Improve recovery rate；It is rinsed using ethanol solution convenient for the silane of the silane coupling agent not reacted, self-condensation is even The separation for joining agent and gas-phase silica, avoids introducing new impurity in general gingerol.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification Text can be implemented accordingly.
<embodiment 1>
The extraction process of general gingerol, comprising the following steps:
Step 1: the ethanol solution that 3L volume fraction is 50% is added into 3kg ginger powder carries out cold soaking extraction, and it is concentrated, Obtain medicinal extract, wherein the time that cold soaking extracts is for 24 hours；
Step 2: medicinal extract is separated using column chromatography, eluent system is petroleum ether-acetone, successively uses petroleum ether- Acetone volume ratio is that the system of 1:0,10:1,7:1,4:1,0:1 are eluted, and is collected when petroleum ether-acetone volume ratio is 7:1 Eluent when eluent and petroleum ether-acetone volume ratio are 4:1 merges eluent and is concentrated, obtains general gingerol.
In step 1 ginger powder the preparation method comprises the following steps: rhizoma zingiberis is crushed, as ginger powder.
<embodiment 2>
The extraction process of general gingerol, comprising the following steps:
Step 1: the ethanol solution that 4L volume fraction is 70% is added into 3kg ginger powder carries out cold soaking extraction, and it is concentrated, Obtain medicinal extract, wherein the time that cold soaking extracts is 60h；
Step 2: medicinal extract is separated using column chromatography, eluent system is petroleum ether-acetone, successively uses petroleum ether- Acetone volume ratio is that the system of 1:0,10:1,6:1,3:1,0:1 are eluted, and is collected when petroleum ether-acetone volume ratio is 6:1 Eluent when eluent and petroleum ether-acetone volume ratio are 3:1 merges eluent and is concentrated, obtains general gingerol.
In step 1 ginger powder the preparation method comprises the following steps: rhizoma zingiberis is crushed, as ginger powder.
<embodiment 3>
The extraction process of general gingerol, comprising the following steps:
Step 1: the ethanol solution that 5L volume fraction is 95% is added into 3kg ginger powder carries out cold soaking extraction, and it is concentrated, Obtain medicinal extract, wherein the time that cold soaking extracts is 96h；
Step 2: medicinal extract is separated using column chromatography, eluent system is petroleum ether-acetone, successively uses petroleum ether- Acetone volume ratio is that the system of 1:0,10:1,5:1,2:1,0:1 are eluted, and is collected when petroleum ether-acetone volume ratio is 5:1 Eluent when eluent and petroleum ether-acetone volume ratio are 2:1 merges eluent and is concentrated, obtains general gingerol.
In step 1 ginger powder the preparation method comprises the following steps: rhizoma zingiberis is crushed, as ginger powder.
<embodiment 4>
The extraction process of general gingerol, comprising the following steps:
Step 1: 3L methylene chloride is added into 3kg ginger powder carries out refluxing extraction, and it is concentrated, obtains medicinal extract, wherein return The time that stream extracts is 1h；
Step 2: medicinal extract is separated using column chromatography, eluent system is petroleum ether-acetone, successively uses petroleum ether- Acetone volume ratio is that the system of 1:0,10:1,5:1,2:1,0:1 are eluted, and is collected when petroleum ether-acetone volume ratio is 5:1 Eluent when eluent and petroleum ether-acetone volume ratio are 2:1 merges eluent and is concentrated, obtains general gingerol.
In step 1 ginger powder the preparation method comprises the following steps: rhizoma zingiberis is crushed, as ginger powder.
<embodiment 5>
The extraction process of general gingerol, comprising the following steps:
Step 1: 4L acetone is added into 3kg ginger powder carries out refluxing extraction, and it is concentrated, obtains medicinal extract, wherein reflux mentions The time taken is 2h；
Step 2: medicinal extract is separated using column chromatography, eluent system is petroleum ether-acetone, successively uses petroleum ether- Acetone volume ratio is that the system of 1:0,10:1,5:1,2:1,0:1 are eluted, and is collected when petroleum ether-acetone volume ratio is 5:1 Eluent when eluent and petroleum ether-acetone volume ratio are 2:1 merges eluent and is concentrated, obtains general gingerol.
In step 1 ginger powder the preparation method comprises the following steps: rhizoma zingiberis is crushed, as ginger powder.
<embodiment 6>
The extraction process of general gingerol, comprising the following steps:
Step 1: 5L ether is added into 3kg ginger powder carries out refluxing extraction, and it is concentrated, obtains medicinal extract, wherein reflux mentions The time taken is 3h；
Step 2: medicinal extract is separated using column chromatography, eluent system is petroleum ether-acetone, successively uses petroleum ether- Acetone volume ratio is that the system of 1:0,10:1,5:1,2:1,0:1 are eluted, and is collected when petroleum ether-acetone volume ratio is 5:1 Eluent when eluent and petroleum ether-acetone volume ratio are 2:1 merges eluent and is concentrated, obtains general gingerol.
In step 1 ginger powder the preparation method comprises the following steps: rhizoma zingiberis is crushed, as ginger powder.
<embodiment 7>
The extraction process of general gingerol, comprising the following steps:
Step 1: 5L ethyl acetate is added into 3kg ginger powder carries out refluxing extraction, and it is concentrated, obtains medicinal extract, wherein return The time that stream extracts is 3h；
Step 2: medicinal extract is separated using column chromatography, eluent system is petroleum ether-acetone, successively uses petroleum ether- Acetone volume ratio is that the system of 1:0,10:1,5:1,2:1,0:1 are eluted, and is collected when petroleum ether-acetone volume ratio is 5:1 Eluent when eluent and petroleum ether-acetone volume ratio are 2:1 merges eluent and is concentrated, obtains general gingerol.
In step 1 ginger powder the preparation method comprises the following steps: rhizoma zingiberis is crushed, as ginger powder.
<embodiment 8>
The extraction process of general gingerol, comprising the following steps:
Step 1: the methanol of 10 times of its gross mass amounts is added into 3kg ginger powder, and it is ultrasonically treated 1h, obtains turbid, In, wherein ginger powder the preparation method comprises the following steps: rhizoma zingiberis is crushed to partial size lower than 1mm, as ginger powder；Take 20 times of ginger powder gross mass amounts Sand material, 8 times amount mass fractions be 10% sodium-chloride water solution mix, stir-fry 20min under the conditions of being placed in 40~50 DEG C, Obtain mixing, wherein the partial size of sand material is 0.5~2cm；Stir-fry mixing under the conditions of 60~65 DEG C, while equivalent adds in five times Enter turbid and keep stir-frying 1h after turbid is added, obtains stir-frying material；Stir-frying material is separated by sieve, obtains sand Layer and ginger powder layer, sand layer is rinsed with methanol, obtains washing lotion, by washing lotion it is laminated with ginger powder and and be concentrated, obtain pre- place Manage ginger powder, wherein the mesh of sieve is circular configuration, and the diameter of mesh is 0.2cm；
The tetrahydrofuran of 10 times of ginger powder gross mass amounts of pretreatment is taken, the pretreatment total matter of ginger powder is then added into tetrahydrofuran The gas-phase silicas for measuring 5 times of amounts are placed in 50 DEG C, stir 10min under conditions of 400r/min, then in 60 DEG C, 400r/min Under the conditions of be added dropwise pretreatment 1 times of ginger powder gross mass amount 4M sulfuric acid solution, be added dropwise to sulfuric acid solution, continue to stir The silane coupling agents of 6 times of ginger powder gross mass amounts are added in equivalent to 20min in seven times again, are placed in 70 DEG C, under conditions of 400r/min 1h is stirred, filtering obtains solid, finally rinses solid with the ethanol solution of mass fraction 95%, and solid is placed in 60 DEG C of items Dry 6h under part, obtains modified gas-phase silica, wherein silane coupling agent is (HO)3Si(CH2)3N(CH2PO3H2)2；To 5L second Acetic acid is added in acetoacetic ester, the PH for adjusting ethyl acetate is 5~6, and modified gas-phase silica is then added, be placed in 50 DEG C, 20min is stirred under conditions of 400r/min, is cooled to room temperature, and is added ginger powder and is carried out refluxing extraction 3h, filtering obtains the first filter Liquid and filter residue, the methanol that 4 times of filter residue gross mass amounts are added into filter residue impregnate 15h, the second filtrate are obtained by filtration；By the first filter Liquid, the second filtrate merge and are concentrated, and obtain medicinal extract.
Step 2: medicinal extract is separated using column chromatography, eluent system is petroleum ether-acetone, successively uses petroleum ether- Acetone volume ratio is that the system of 1:0,10:1,5:1,2:1,0:1 are eluted, and is collected when petroleum ether-acetone volume ratio is 5:1 Eluent when eluent and petroleum ether-acetone volume ratio are 2:1 merges eluent and is concentrated, obtains general gingerol.
<comparative example 1>
General gingerol extraction process is the same as embodiment 7, wherein the difference is that medicinal extract is purified using macroreticular resin, elutes Agent is the ethanol solution that volume fraction is 60%.
<comparative example 2>
General gingerol extraction process is the same as embodiment 8, wherein the difference is that ginger powder is not pre-processed.
<comparative example 3>
General gingerol extraction process is the same as embodiment 8, wherein the difference is that pretreatment ginger powder is directly returned using ethyl acetate Stream extracts 3h, is not added with modified gas-phase silica.
<comparative example 4>
General gingerol extraction process is the same as embodiment 8, wherein the difference is that gas-phase silica does not use (HO)3Si(CH2)3N (CH2PO3H2)2It is modified.
<experimental result>
1, the purity of general gingerol
By general gingerol obtained by embodiment 4, embodiment 5, embodiment 7, comparative example 1 respectively through highly effective liquid phase chromatography detection method Detection, wherein chromatographic column: octadecylsilane chemically bonded silica is filler, mobile phase: methanol, the water of volume ratio 3:2, detection Wavelength: 280nm, testing result is as shown in table 1,
The purity of table 1, general gingerol
Group Purity
Embodiment 4 91.8%
Embodiment 5 93.3%
Embodiment 7 94.2%
Comparative example 1 90.6%
The result shows that petroleum ether-acetone by using different volumes ratio chromatographs medicinal extract column, the pure of general gingerol can be improved Degree.
2, cell-wall breaking ratio
The breaking-wall cell situation of 200 mesh ginger powders is observed under the microscope, meanwhile, observation embodiment 8,2~4 institute of comparative example are right The broken wall situation of medicinal extract is answered, the results are shown in Table 2；
Table 2, cell-wall breaking ratio
Group Cell-wall breaking ratio
Embodiment 8 95%
Ginger powder 79%
Comparative example 2 88%
Comparative example 3 91%
Comparative example 4 90%
The result shows that may advantageously facilitate breaking-wall cell to the friction of ginger powder by sand material, the recovery rate of general gingerol is improved；Add Enter modified gas-phase silica and pass through gas-phase silica during the extraction process and breaking-wall cell may advantageously facilitate to the friction of ginger powder.
3, gas-phase silica settles situation
Gas-phase silica is in the dispersion of ethyl acetate in observation extraction process, and the results are shown in Table 3；
Table 3, delamination
Group Delamination
Embodiment 8 Gas-phase silica is evenly dispersed
Comparative example 4 Gas-phase silica sinks
The result shows that using (HO)3Si(CH2)3N(CH2PO3H2)2Gas-phase silica is modified, gas phase can be improved Dispersibility of the white carbon black in solvent increases contact of the ginger powder with gas-phase silica, improves sporoderm-broken rate.
4, the recovery rate of general gingerol
In ginger powder, the theoretical content of general gingerol is 9.6%, calculates the recovery rate of general gingerol in 3kg ginger powder, recovery rate=total Amount/ginger powder amount × 100% of gingerol, the results are shown in Table 4；
Table 4, recovery rate
Group Recovery rate %
Embodiment 7 8.0
Embodiment 8 9.0
Comparative example 1 7.7
Comparative example 2 8.3
Comparative example 3 8.7
The result shows that petroleum ether-acetone of different volumes ratio can also reduce residual of the general gingerol in silicagel column, improve total The recovery rate of gingerol；Modified gas-phase silica is added when by being pre-processed and extracted to ginger powder can effectively improve total ginger The recovery rate of phenol.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited In specific details and embodiment shown and described herein.

Claims (7)

1. the extraction process of general gingerol, which comprises the following steps:
It extracts and is concentrated Step 1: solvent is added into ginger powder, obtain medicinal extract；
Step 2: medicinal extract is separated using column chromatography, eluent system is petroleum ether-acetone, collects petroleum ether-acetone volume Eluent when eluent and petroleum ether-acetone volume ratio when than for 7~5:1 are 4~2:1 merges eluent and is simultaneously concentrated, Obtain general gingerol.
2. the extraction process of general gingerol as described in claim 1, which is characterized in that in step 1 ginger powder the preparation method comprises the following steps: Rhizoma zingiberis is crushed, as ginger powder.
3. the extraction process of general gingerol as described in claim 1, which is characterized in that the amount ratio of ginger powder and solvent in step 1 For 1kg:3-5L.
4. the extraction process of general gingerol as described in claim 1, which is characterized in that solvent is methylene chloride, second in step 1 Acetoacetic ester, acetone, ether or volume fraction are one of the ethanol solution of 50-95%.
5. the extraction process of general gingerol as described in claim 1, which is characterized in that the extracting method in step 1 mentions for cold soaking It takes or refluxing extraction, wherein the time that cold soaking extracts is 24~96h, and the time of refluxing extraction is 1~3h.
6. the extraction process of general gingerol as described in claim 1, which is characterized in that the ginger powder in step 1 has carried out pre- place Reason, pretreated detailed process are as follows:
S1, the methanol that 10 times of its gross mass amounts are added into ginger powder, and it is ultrasonically treated 1h, obtain turbid；
S2, the sand material for taking 20 times of ginger powder gross mass amounts, the sodium-chloride water solution that the mass fraction of 8 times of amounts is 10% mix, juxtaposition Stir-fry 20min under the conditions of 40~50 DEG C, obtains mixing, wherein the partial size of minimum sand material be greater than ginger powder in ginger powder particle it is straight Diameter；
S3, stir-fry mixing under the conditions of 60~65 DEG C, while equivalent addition turbid continues to turn over after turbid is added in five times 1h is fried, stir-frying material is obtained；
S4, stir-frying material is separated by sieve, obtains sand layer and ginger powder layer, sand layer is rinsed with methanol, is obtained To washing lotion, by washing lotion it is laminated with ginger powder and and be concentrated, obtain pretreatment ginger powder, wherein the mesh of sieve is circular configuration, mesh Diameter between the diameter of ginger powder particle in ginger powder and the particle size of minimum sand material.
7. the extraction process of general gingerol as described in claim 1, which is characterized in that in step 1 into ginger powder be added solvent into Row is extracted and is concentrated, detailed process are as follows:
A1, the tetrahydrofuran for taking 10 times of ginger powder gross mass amounts, are then added the gas phase of 5 times of ginger powder gross mass amounts into tetrahydrofuran White carbon black is placed in 50 DEG C, stirs 10min under conditions of 400r/min, is then added dropwise under conditions of 60 DEG C, 400r/min The sulfuric acid solution of the 4M of 1 times of ginger powder gross mass amount, is added dropwise to sulfuric acid solution, and continuing stirring 20min, equivalent adds in seven times again The silane coupling agents for entering 6 times of ginger powder gross mass amounts are placed in 70 DEG C, stir 1h under conditions of 400r/min, filter, consolidate Body finally rinses solid with the ethanol solution of mass fraction 95%, and dries 6h under the conditions of solid is placed in 60 DEG C, is modified Gas-phase silica, wherein silane coupling agent is (HO)3Si(CH2)3N(CH2PO3H2)2；
A2, acetic acid is added into solvent, the PH for adjusting solvent is 5~6, and modified gas-phase silica is then added, be placed in 50 DEG C, 20min is stirred under conditions of 400r/min, is cooled to room temperature, ginger powder is added and extracts, and is filtered, is obtained the first filtrate and filter Slag, the methanol that 4 times of filter residue gross mass amounts are added into filter residue impregnate 15h, the second filtrate are obtained by filtration；
A3, the first filtrate, the second filtrate are merged and is concentrated, obtain medicinal extract.
CN201910092793.7A 2019-01-30 2019-01-30 The extraction process of general gingerol Pending CN109675002A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101085727A (en) * 2007-07-05 2007-12-12 中国人民解放军第四一一医院 Method for preparing 6-gingerol and 8-gingerol from ginger
CN101255206A (en) * 2008-04-09 2008-09-03 暨南大学 Molecular engram polymer for purifying 6-gingerol as well as preparation and uses thereof
CN102220036A (en) * 2011-06-02 2011-10-19 北京化工大学 Method for preparing white carbon black modified by silane coupling agent
CN104001128A (en) * 2014-05-20 2014-08-27 西南交通大学 Total gingerol ointment for treating chilblain and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101085727A (en) * 2007-07-05 2007-12-12 中国人民解放军第四一一医院 Method for preparing 6-gingerol and 8-gingerol from ginger
CN101255206A (en) * 2008-04-09 2008-09-03 暨南大学 Molecular engram polymer for purifying 6-gingerol as well as preparation and uses thereof
CN102220036A (en) * 2011-06-02 2011-10-19 北京化工大学 Method for preparing white carbon black modified by silane coupling agent
CN104001128A (en) * 2014-05-20 2014-08-27 西南交通大学 Total gingerol ointment for treating chilblain and preparation method thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
LEE B S，等: "Preparation and investigations of antioxidative effect of gingerol from ginger(Zingiber officinale Roscoe)extract", 《JOURNAL OF PHARMACEUTICAL SCIENCES》 *
康睿宇，等: "纳米SiO2的制备、改性和应用", 《化工时刊》 *
曲清莉，等: "利用GC-MS和电子鼻研究超微粉碎对姜风味物质的影响", 《中国调味品》 *
黄雪松: "姜粉测定方法研究", 《中国调味品》 *

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Application publication date: 20190426