CN107778158A - A kind of high-purity general gingerol, preparation method and the usage - Google Patents
A kind of high-purity general gingerol, preparation method and the usage Download PDFInfo
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- CN107778158A CN107778158A CN201610771664.7A CN201610771664A CN107778158A CN 107778158 A CN107778158 A CN 107778158A CN 201610771664 A CN201610771664 A CN 201610771664A CN 107778158 A CN107778158 A CN 107778158A
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- C07—ORGANIC CHEMISTRY
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- C07C49/00—Ketones; Ketenes; Dimeric ketenes; Ketonic chelates
- C07C49/20—Unsaturated compounds containing keto groups bound to acyclic carbon atoms
- C07C49/255—Unsaturated compounds containing keto groups bound to acyclic carbon atoms containing ether groups, groups, groups, or groups
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- 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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- C—CHEMISTRY; METALLURGY
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- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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Abstract
The invention discloses a kind of high-purity general gingerol, preparation method and the usage, belong to drug field, and in particular to the preparation method of general gingerol and its application to nausea and vomiting caused by chemotherapy.A kind of method for preparing general gingerol extract, including：A. low-temperature precipitation；B. it is concentrated under reduced pressure；C. macroporous resin column chromatography；D. it is concentrated under reduced pressure, obtains the general gingerol extract.It is an advantage of the invention that：The conventional methods such as extraction, silica gel column chromatography are avoided in separation process, reduce the use of a large amount of positive phase reagents.The general gingerol extract purity of preparation is high, prepares simple, non-stimulated, cheap, pharmacological evaluation confirms that drug effect is notable, available for the medicine for preparing preventing and treating vomiting.
Description
Technical field
The present invention relates to a kind of high-purity general gingerol, preparation method and the usage, belong to drug field, and in particular to total ginger
The preparation method of phenol and its application to nausea and vomiting caused by chemotherapy.
Background technology
Ginger and rhizoma zingiberis are respectively zingiberaceous plant ZingiberofficinaleRosc. new fresh quench stem or and dry root
Stem, it is the plant of the integration of drinking and medicinal herbs closely related with people's life and health.Main component in ginger is volatile oil composition, ginger
Capsaicin constituents and Diphenylheptane constituents, wherein most with gingerol content.Gingerol is made a living a variety of tools in (dry) ginger
There is the general name of the similar material of the structure of ginger pungent, 3- methoxyl group -4- hydroxy phenyls functional group is contained in its structure, main bag
Include gingerol class (Gingerols), zingiberene phenols (Shogals), zingiberone class (Zingerone), secondary ginger oil ketone (Paradols),
The peppery diones of ginger (Gingeriones), the peppery glycols of ginger (Gingerdiols).Modern pharmacology research finds that gingerol is ginger
Pharmacological action and present functions of prevention and health care main active.
Research shows that main chemical compositions are ginger phenolic compounds in gingerol, mainly comprising 4- gingerols, 6-gingerol, 8- ginger
Phenol, 10-gingerol etc. (structure chart is shown in accompanying drawing 1), these compounds are unstable, and under acid condition (PH ＜ 4.5), its hydroxyl can take off
Water forms salad oil, and in heating (general more than 80 DEG C) or alkalescence condition, its carbon-carbon bond can break to form zingiberone and corresponding
Aldehyde, therefore, the general gingerol to be separated that obtains must be carried out in the environment of low temperature, neutrality and chemical inertness.So far, prepare total
The method of gingerol mainly has solvent extraction separation-multiple solvent extraction, column chromatography, recrystallization etc..CN102258758A is public
A kind of preparation method of high-content liquid gingerols has been opened, it first removes small polar impurity in oleoresin ginger with petroleum ether extraction,
Crude product gingerol and water layer are obtained, then is extracted with hydrophobic solvent, by being recovered under reduced pressure to obtain high-content liquid gingerols.But this side
Method has had to gingerol mixture, and has used a large amount of positive phase reagents.(AB-8 macroreticular resins separate oleoresin ginger to reported in literature
In gingerol《Fine chemistry industry》2 months the 2nd phases of volume 26 in 2009), oleoresin ginger is separated with AB-8 macroporous absorbent resins, with ether
With n-hexane as eluant, eluent, detected with GC-MS, ginger aldehydes matter area percent is up to 55.68%.But what the method obtained
General gingerol content is only 55%, and eluent system is positive solvent system, is unfavorable for mass producing.Also there is reported in literature (knot
Brilliant gingerol being produced and identifying,《Food and industrial fermentation》The 10th phase of volume 31 in 2005), after oleoresin ginger is prepared, lead to
Cross dry chromatography, prepare TLC chromatographies and Sephadex LH-20 column chromatographies for 2 times, obtain crystalized gingerol.Though the method is prepared
The gingerol of higher degree, but operating procedure is relatively complicated, is not easy amplification and industrial production.
As can be seen here, due to the restriction of cost and yield, a kind of quick, easily operated, quality of finished product good is nowadays studied
And the method for preparing general gingerol that yield is larger, it is the big problem that the art faces.Vomiting is clinical common phenomenon, special
It is not that more serious nausea and vomiting often occur for Patients Receiving Chemotherapy.Although medicine currently used for treating nausea and vomiting compares
More, effect is unsatisfactory, although such as Ondansetron, Granisetron medicine has certain effect to emesis of chemotherapy, but due to it
It is expensive and have certain side effect, their use is also limit to a certain extent.
Traditional medicine thinks that vomiting is due to caused by stomach Qi rising, stomach Qi upward reversal, treatment vomiting should with regulating functional activities of qi,
Based on stopping nausea and vomiting by lowering the adverse flow of QI.Jiang Zuowei traditional Chinese medicines, usually there is the title of " panacea of vomitting ", its acrid flavour is warm-natured, returns spleen, stomach, lung channel, can open
Stomach preventing or arresting vomiting, inducing sweat and dispelling exogenous evils.It is more at present to form compound of Chinese herbal medicine vomit duo to chemotherapy using ginger and other medicinal materials by reported in literature, but
Because its chemical composition is complex, mechanism is failed to understand, clinically application has limitation.Gingerol is as chemical composition main in ginger
And effective component, it but there are no reported in literature and only utilize nausea and vomiting caused by general gingerol treatment chemotherapy.
The content of the invention
The invention solves first technical problem be to provide a kind of high-purity general gingerol.
The invention solves second technical problem be to provide a kind of quick, easily operated, quality of finished product good and yield
Larger general gingerol preparation method.
The invention solves the 3rd technical problem be to provide general gingerol extract be used for prevent and treat chemotherapy of tumors after vomit
Purposes.
To achieve the above object, the present invention uses following technical scheme：
A kind of method for preparing general gingerol extract, step are：
A. low-temperature precipitation：Content using general gingerol be 30~35wt% oleoresin gingers as raw material, add organic solvent A it is molten
Solution, obtains dark brown settled solution, adds a certain amount of organic solvent B, and condition of ultralow temperature is taken out after freezing 4~12h, obtains lower floor
Dark oily content；
B. it is concentrated under reduced pressure：Under the conditions of 0-70 DEG C, the grease obtained in a is concentrated under reduced pressure, solvent is removed, obtains general gingerol
Crude product；
C. macroporous resin column chromatography：The general gingerol crude product obtained in b is added into low-concentration ethanol dissolving, stirred, mistake
Filter obtains yellow alcoholic solution；Using sample size and resin volume ratio as 1:5~20 (g：Ml) loading macroporous resin column, alcohol-water are molten
Agent system elutions, collect the ethanol eluate of debita spissitudo；
D. it is concentrated under reduced pressure：Under the conditions of 0-70 DEG C, the ethanol eluate obtained in step c is concentrated under reduced pressure, obtained described
General gingerol extract.
Oleoresin ginger is prepared with supercritical carbon dioxide method for extracting in the step a, and described is overcritical
Carbon dioxide abstraction process includes two processes of the extraction carried out simultaneously and separation, in the extraction process extracting pressure be 30~
35MPa, extraction temperature are 40~50 DEG C；The separation process includes one-level separation and the second-order separation, point of the one-level separation
It is from condition：12~14MPa of pressure, 45~50 DEG C of temperature, the second-order separation condition are：5~6MPa of pressure, 35~45 DEG C of temperature；
The oleoresin ginger is the product obtained in primary separator.
Organic solvent A in the step a is acetone, one kind in chloroform, ethyl acetate, ethanol, and addition is raw material
0.5~2 times (plastid ratio)；Organic solvent B is one kind in n-hexane, petroleum ether, chloroform, and addition is the 1 of organic solvent A
~5 times (volume ratios)；Condition of ultralow temperature in step a is -20 DEG C~-80 DEG C.Ethanol in low-concentration ethanol in the step c
Weight percent concentration is 5~25%, and dosage is 10~20 times (plastid ratios) of example weight；Macroreticular resin in the step c
One kind in model D101, AB-8, D4020, loading flow velocity are 0.5~1BV column volumes；Alcohol-water Elution range is
20%~90%, collect 40%~70% ethanol eluate.
Preferably, macroreticular resin model D101 in the step c.
The preferred following preparation method of the present invention：
A. low-temperature precipitation：Oleoresin ginger 250g, its general gingerol content are 30~35%, and supercritical carbon dioxide extracting obtains bar
Part is：Extracting pressure/temperature (30MPa/45 DEG C), one-level separating pressure/temperature (14MPa/50 DEG C), the second-order separation pressure/temperature
Spend (5MPa/35 DEG C)；Obtained in primary separator for the oleoresin ginger, in second-stage separator predominantly the volatile oil of ginger into
Point；
B. it is concentrated under reduced pressure：The oleoresin ginger obtained into a adds 250ml ethyl acetate and fully dissolved, and it is clear to obtain dark brown
Clear solution, then 750ml petroleum ether is added thereto, shake up, taken out after freezing 8h under the conditions of being placed in -80 DEG C, remove layer depth color
Grease；
C. macroporous resin column chromatography：Under the conditions of 50 DEG C, be concentrated under reduced pressure grease described in b, obtains general gingerol crude product；
D. it is concentrated under reduced pressure：Obtained general gingerol crude product in c is added into 2L25% ethanol solutions, stirred to abundant dissolving,
Filter to obtain yellow ethanol solution；By it with v=0.5BV/h speed loading D101 macroporous resin columns, column volume is about 2.0L, loading
After the completion of, respectively with 20%, 40%, 60%, 80% ethanol elution, collect 60% ethanol solution；Then at 0.08Mpa, 45 DEG C of bars
Be concentrated under reduced pressure to obtain general gingerol extract under part.
The present invention is existed using the oleoresin ginger that supercritical carbon dioxide extracting obtains as raw material using each composition in oleoresin ginger
Different solubility in organic solvent, low-temperature precipitation remove small polar impurity, then further separate through macroporous resin column chromatography pure
Change obtains high content general gingerol extract.
The general gingerol extract being prepared according to the method described above, general gingerol content are 80%-95%, and the extract has
High-purity and pharmacological activity.The gingerol extract that the present invention obtains is main chemical compositions and effective component in ginger, and ginger
Usually there is a title of " panacea of vomitting ", present invention display, high-purity general gingerol extract is there is the effect of fine in terms of preventing or arresting vomiting.
The detection method of general gingerol is high performance liquid chromatography, and testing conditions are：Chromatographic column：Octadecylsilane bonded silica
Glue is filler；Mobile phase：Methanol-water (60:40)；Flow velocity：1ml/min；Detection wavelength：280nm；Column temperature：30℃.
A kind of medicine for preventing and treating vomiting, contains described general gingerol extract.
The medicine also contains pharmaceutically acceptable auxiliary material.The selection of auxiliary material is common knowledge.
The medicine is peroral dosage form, including but not limited to tablet, capsule, pill, powder, electuary etc..
Application of the present invention protection general gingerol extract in the medicine for preparing preventing and treating vomiting.
Advantages of the present invention：
A. it is therefore, super to face because the core of supercritical carbon dioxide extracting is the high-density CO 2 extraction under low temperature
The oleoresin ginger that boundary is obtained by extraction is not only seldom containing terpene volatile materials such as zingiberenes, almost without heavy-metal residual and organic solvent
Residual, and it is practically free of other water soluble ingredients.The present invention, can be final using the oleoresin ginger of this high-quality as raw material
The general gingerol almost without heavy-metal residual is obtained, its high purity 90%, various residual quantity of heavy metal are respectively less than 0.1ppm, described
Heavy metal includes arsenic, cadmium, lead, mercury；
B. low-temperature precipitation technology is used in separation process of the invention, removes most of small polar impurity in oleoresin ginger,
One is that of avoiding gingerol constituents by thermally labile, second, effectively reducing the applied sample amount of macroreticular resin；
C. the conventional methods such as extraction, silica gel column chromatography are avoided in separation process of the present invention, reduces a large amount of positive phase reagents
Use.In whole separation process, mainly using ethanol as separating medium, and it is often adopted in food and medicine industrial production
With, the security for preparing general gingerol is ensure that, and ethanol is easily recycled, it is reusable, reduce production cost；
D. the present invention alleviates vomiting medicine from the research of traditional Chinese medical science angle, has to delayed nausea and vomiting caused by chemotherapy good
Prevention effect.Pharmaceutical composition of the present invention, which prepares simple, non-stimulated, cheap, pharmacological evaluation, confirms that drug effect is notable.
Brief description of the drawings
Fig. 1 ginger phenolic compounds structure charts：During n=2,4- gingerols；During n=4,6-gingerol；During n=6,8-gingerol；N=8
When, 10-gingerol.
The high-purity general gingerol HPLC figures that Fig. 2 is prepared
Embodiment
Embodiment 1：Prepare high-purity general gingerol extract
A. oleoresin ginger 250g, its general gingerol content are 30.8%.Supercritical carbon dioxide extracting obtains condition：Extraction pressure
Power/temperature (30MPa/40 DEG C), one-level separating pressure/temperature (12MPa/45 DEG C), the second-order separation Pressure/Temperature (5MPa/35
℃).Obtained in primary separator for the oleoresin ginger, the predominantly volatile oil component of ginger in second-stage separator；
B. the oleoresin ginger that is obtained into a adds 125ml acetone and fully dissolved, and obtains dark brown settled solution, then to its
Middle addition 250ml n-hexane, shakes up, and is taken out after freezing 4h under the conditions of being placed in -20 DEG C, removes a layer dark oily content；
C. under the conditions of 45 DEG C, be concentrated under reduced pressure grease described in b, obtains general gingerol crude product 123.2g；
D. the obtained general gingerol crude product in c is added into 1.5L10% ethanol solutions, stirs to abundant dissolving, filter yellow
Color ethanol solution.By it with v=0.5BV/h speed loading D101 macroporous resin columns, column volume is about 1.5L, after completion of the sample,
Respectively with 10%, 30%, 50%, 70% ethanol elution, 50% ethanol solution is collected.Depressurized under the conditions of 0.08Mpa, 45 DEG C
It is concentrated to give general gingerol extract 54.7g.
General gingerol assay：High performance liquid chromatography
Chromatographic column：Octadecylsilane chemically bonded silica is filler；Mobile phase：Methanol-water (60:40)；Flow velocity：1ml/
min；Detection wavelength：280nm；Column temperature：30℃.
Detected through highly effective liquid phase chromatography detection method, its general gingerol content is up to 90.6%.
Embodiment 2：Prepare high-purity general gingerol extract
A. oleoresin ginger 500g, its general gingerol content are 32.3%.Supercritical carbon dioxide extracting obtains condition：Extraction pressure
Power/temperature (32MPa/45 DEG C), one-level separating pressure/temperature (14MPa/50 DEG C), the second-order separation Pressure/Temperature (5MPa/35
℃).Obtained in primary separator for the oleoresin ginger, the predominantly volatile oil component of ginger in second-stage separator；
B. the oleoresin ginger obtained into a adds 500ml ethyl acetate and fully dissolved, and obtains dark brown settled solution, then
1L n-hexane is added thereto, is shaken up, and is taken out after freezing 6h under the conditions of being placed in -40 DEG C, is removed a layer dark oily content；
C. under the conditions of 50 DEG C, be concentrated under reduced pressure grease described in b, obtains general gingerol crude product 214.6g；
D. the obtained general gingerol crude product in c is added into 4.1L20% ethanol solutions, stirs to abundant dissolving, filter yellow
Color ethanol solution.By it with v=1BV/h speed loading D101 macroporous resin columns, column volume is about 2.2L, after completion of the sample, point
Not with 25%, 35%, 55%, 75% ethanol elution, 75% ethanol solution is collected.Depressurized under the conditions of 0.08Mpa, 45 DEG C dense
Contract to obtain general gingerol extract 117.1g.
Detected through highly effective liquid phase chromatography detection method, method is with embodiment 1, and its general gingerol content is up to 88.0%.
Embodiment 3：Prepare high-purity general gingerol extract
A. oleoresin ginger 500g, its general gingerol content are 34.7%.Supercritical carbon dioxide extracting obtains condition：Extraction pressure
Power/temperature (30MPa/45 DEG C), one-level separating pressure/temperature (12MPa/45 DEG C), the second-order separation Pressure/Temperature (5MPa/35
℃).Obtained in primary separator for the oleoresin ginger, the predominantly volatile oil component of ginger in second-stage separator；
B. the oleoresin ginger that is obtained into a adds 250ml chloroforms and fully dissolved, and obtains dark brown settled solution, then to its
Middle addition 1L petroleum ether, shakes up, and is taken out after freezing 8h under the conditions of being placed in -80 DEG C, removes a layer dark oily content；
C. under the conditions of 50 DEG C, be concentrated under reduced pressure grease described in b, obtains general gingerol crude product 220.8g；
D. the obtained general gingerol crude product in c is added into 3.3L25% ethanol solutions, stirs to abundant dissolving, filter yellow
Color ethanol solution.By it with v=0.5BV/h speed loading D101 macroporous resin columns, column volume is about 2.2L, after completion of the sample,
Respectively with 25%, 45%, 65%, 85% ethanol elution, 65% ethanol solution is collected.Depressurized under the conditions of 0.09Mpa, 50 DEG C
It is concentrated to give general gingerol extract 106.4g.
Detected through highly effective liquid phase chromatography detection method, method is with embodiment 1, and its general gingerol content is up to 91.3%.
Embodiment 4：Prepare high-purity general gingerol extract
A. oleoresin ginger 250g, its general gingerol content are 33.4%.Supercritical carbon dioxide extracting obtains condition：Extraction pressure
Power/temperature (30MPa/45 DEG C), one-level separating pressure/temperature (14MPa/50 DEG C), the second-order separation Pressure/Temperature (5MPa/35
℃).Obtained in primary separator for the oleoresin ginger, the predominantly volatile oil component of ginger in second-stage separator；
B. the oleoresin ginger obtained into a adds 250ml ethyl acetate and fully dissolved, and obtains dark brown settled solution, then
750ml petroleum ether is added thereto, is shaken up, and is taken out after freezing 8h under the conditions of being placed in -80 DEG C, is removed a layer dark oily content；
C. under the conditions of 50 DEG C, be concentrated under reduced pressure grease described in b, obtains general gingerol crude product 100.2g；
D. the obtained general gingerol crude product in c is added into 2L25% ethanol solutions, stirs to abundant dissolving, filter to obtain yellow
Ethanol solution.By it with v=0.5BV/h speed loading D101 macroporous resin columns, column volume is about 2.0L, after completion of the sample, point
Not with 20%, 40%, 60%, 80% ethanol elution, 60% ethanol solution is collected.Depressurized under the conditions of 0.08Mpa, 45 DEG C dense
Contract to obtain general gingerol extract 56.8g.
Detected through highly effective liquid phase chromatography detection method, method is with embodiment 1, and its general gingerol content is up to 91.7%.
Embodiment 5：It is prepared by soft capsule
1st, the preparation of gelatin solution：Gelatin 100g, glycerine 40g, distilled water 130g
Take gelatin to add suitable quantity of water to make its expansion, separately put glycerine and remaining distilled water in glue pot, be heated to 70 DEG C -80
DEG C, it is well mixed, standing makes foam float, and removes the foam of floating, and filtering uses.
2nd, the preparation of fluid：General gingerol extract 300ml is taken, mixes, fills with the edible vegetable oil of heated sterilizing, clarification
Divide and stir evenly, produce.
3rd, pill：Gelatin solution and fluid are respectively put into gelatin solution storage tank and liquor tank, using automatic rotary transformation of ownership capsule
Machine produces, and accurately controls amount of liquid medicine by controlling pump, the ball of capsule and pill 5000 is made.
Embodiment 6：General gingerol extract vomits the influence of experiment to cisplatin induced pigeon
1st, experiment material
1.1 experimental animal
Healthy pigeon, male and female half and half.
1.2 given the test agent
General gingerol, Zhongxin Innova Laboratories Drug Manufacturing Room provide, and are prepared by the method for embodiment 4.
1.3 reagent
Cisplatin for injection (freeze-dried powder), Qilu Pharmaceutical Co., Ltd..
2nd, test method
Healthy pigeon 30 is taken, male and female half and half, is divided into 3 groups by body weight equilibrium：Model control group, general gingerol low dose group
(60mg/kg), general gingerol high dose group (120mg/kg).Each group pigeon gastric infusion (10mL/kg), model control group is given
Volume pure water, for three days on end.1 hour after last dose, cis-platinum (4.0mg/kg, 2.0ml/kg) is injected intravenously, single cage is raised,
Observe pigeon vomiting incubation period, the vomiting number in 8h and vomiting sum frequency.After injecting cis-platinum, pigeon vomits, and stretches neck, opens
Mouthful, shrug, phenomena such as belly shrinks, restored calm to pigeon and be calculated as 1 vomiting, vomitted after incubation period pointed injection to vomitting for the first time
The time told, vomiting sum frequency refer to pigeon in the observation period and stretch neck, dehisce, shrug, the total degree that belly shrinks.With model control group
Statistical comparison is carried out, result of the test is counted using SPSS11.0.
3rd, experimental result
The general gingerol of table 1 vomits the influence of experiment to cisplatin induced pigeon
Compared with control group, * P<0.05,**P<0.01.
Result of the test shows, the dosage group successive administration 3 days of general gingerol two, is vomitted after substantially shortening pigeon injection cis-platinum
Incubation period, reduce 8 hours in vomiting number and vomiting sum frequency, more have significant difference (P with model control group<0.05,
P<0.01).Prompt general gingerol that there is the pharmacological action of certain suppression vomit duo to chemotherapy.
Claims (10)
- A kind of 1. method for preparing general gingerol extract, it is characterised in that step is：A. low-temperature precipitation：Content using general gingerol be 30~35wt% oleoresin gingers as raw material, add organic solvent A dissolving, obtain To dark brown settled solution, a certain amount of organic solvent B is added, condition of ultralow temperature is taken out after freezing 4~12h, obtains lower floor's dark color Grease；B. it is concentrated under reduced pressure：Under the conditions of 0-70 DEG C, the grease obtained in a is concentrated under reduced pressure, solvent is removed, it is thick to obtain general gingerol Product；C. macroporous resin column chromatography：The general gingerol crude product obtained in b is added into low-concentration ethanol dissolving, stirs, filters To yellow alcoholic solution；Using sample size and resin volume ratio as 1:5~20 (g：Ml) loading macroporous resin column, ethanol-water system System elution, collect the ethanol eluate of debita spissitudo；D. it is concentrated under reduced pressure：Under the conditions of 0-70 DEG C, the ethanol eluate obtained in step c is concentrated under reduced pressure, obtains total ginger Phenol extraction thing.
- A kind of 2. method for preparing general gingerol extract according to claim 1, it is characterised in that：Ginger in the step a Oleoresin is prepared with supercritical carbon dioxide method for extracting, and described supercritical carbon dioxide extracting process includes same Two processes of Shi Jinhang extraction and separation, extracting pressure be 30~35MPa in the extraction process, and extraction temperature is 40~50 ℃；The separation process includes one-level separation and the second-order separation, and the separation condition of the one-level separation is：12~14MPa of pressure, 45~50 DEG C of temperature, the second-order separation condition are：5~6MPa of pressure, 35~45 DEG C of temperature；The oleoresin ginger is primary separator In obtained product.
- A kind of 3. method for preparing general gingerol extract according to claim 1 or 2, it is characterised in that：In the step a Organic solvent A be acetone, chloroform, ethyl acetate, one kind in ethanol, addition is 0.5~2 times (plastid ratio) of raw material； Organic solvent B is one kind in n-hexane, petroleum ether, chloroform, and addition is 1~5 times (volume ratio) of organic solvent A；Step a In condition of ultralow temperature be -20 DEG C~-80 DEG C.
- A kind of 4. method for preparing general gingerol extract according to claim 1 or 2, it is characterised in that：In the step c The weight percent concentration of ethanol is 5~25% in low-concentration ethanol, and dosage is 10~20 times (plastid ratios) of example weight；Institute One kind in macroreticular resin model D101, AB-8, D4020 in step c is stated, loading flow velocity is 0.5~1BV column volumes；Second Alcohol-water elution scope is 20%~90%, collects 40%~70% ethanol eluate.
- 5. a kind of method for preparing general gingerol extract according to claim 1 or 2, it is characterised in that including following step Suddenly：A. low-temperature precipitation：Oleoresin ginger 250g, its general gingerol content are 30~35%, and supercritical carbon dioxide extracting obtains condition For：Extracting pressure/temperature (30MPa/45 DEG C), one-level separating pressure/temperature (14MPa/50 DEG C), the second-order separation Pressure/Temperature (5MPa/35℃)；Obtained in primary separator for the oleoresin ginger, in second-stage separator predominantly the volatile oil of ginger into Point；B. it is concentrated under reduced pressure：The oleoresin ginger obtained into a adds 250ml ethyl acetate and fully dissolved, and it is molten to obtain dark brown clarification Liquid, then 750ml petroleum ether is added thereto, shake up, taken out after freezing 8h under the conditions of being placed in -80 DEG C, remove a layer dark oil Thing；C. macroporous resin column chromatography：Under the conditions of 50 DEG C, be concentrated under reduced pressure grease described in b, obtains general gingerol crude product；D. it is concentrated under reduced pressure：Obtained general gingerol crude product in c is added into 2L25% ethanol solutions, stirred to abundant dissolving, filtering Obtain yellow ethanol solution；By it with v=0.5BV/h speed loading D101 macroporous resin columns, column volume is about 2.0L, completion of the sample Afterwards, 60% ethanol solution is collected with 20%, 40%, 60%, 80% ethanol elution respectively；Under the conditions of 0.08Mpa, 45 DEG C Be concentrated under reduced pressure to obtain general gingerol extract.
- 6. the general gingerol extract being prepared according to method any one of claim 1 to 5.
- A kind of 7. medicine for preventing and treating vomiting, it is characterised in that：Contain the general gingerol extract described in claim 6.
- 8. the medicine of preventing and treating vomiting according to claim 7, it is characterised in that：Also contain pharmaceutically acceptable auxiliary material.
- 9. the medicine of the preventing and treating vomiting according to claim 7 or 8, it is characterised in that：For peroral dosage form, selected from tablet, glue One kind in wafer, pill, powder and electuary.
- 10. application of the general gingerol extract in the medicine for preparing preventing and treating vomiting described in claim 6.
Priority Applications (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112138131A (en) * | 2020-10-11 | 2020-12-29 | 成都克洛玛生物科技有限公司 | Preparation method and application of total gingerol external preparation |
| CN117942384A (en) * | 2024-03-26 | 2024-04-30 | 北京元延医药科技股份有限公司 | Preparation method of ginger oil with high biological activity and supercritical carbon dioxide extraction |
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| US20090011059A1 (en) * | 2005-12-22 | 2009-01-08 | Naoki Ishiguro | Ginger Extract For Inhibiting Human Drug Transporters |
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| US20090011059A1 (en) * | 2005-12-22 | 2009-01-08 | Naoki Ishiguro | Ginger Extract For Inhibiting Human Drug Transporters |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112138131A (en) * | 2020-10-11 | 2020-12-29 | 成都克洛玛生物科技有限公司 | Preparation method and application of total gingerol external preparation |
| CN117942384A (en) * | 2024-03-26 | 2024-04-30 | 北京元延医药科技股份有限公司 | Preparation method of ginger oil with high biological activity and supercritical carbon dioxide extraction |
| CN117942384B (en) * | 2024-03-26 | 2024-06-04 | 北京元延医药科技股份有限公司 | Preparation method of ginger oil with high biological activity and supercritical carbon dioxide extraction |
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