CN109106930A - anti-aging black ginger extract and preparation method thereof - Google Patents
anti-aging black ginger extract and preparation method thereof Download PDFInfo
- Publication number
- CN109106930A CN109106930A CN201810869975.6A CN201810869975A CN109106930A CN 109106930 A CN109106930 A CN 109106930A CN 201810869975 A CN201810869975 A CN 201810869975A CN 109106930 A CN109106930 A CN 109106930A
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- Prior art keywords
- black ginger
- extract
- aging
- ethyl acetate
- powder
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Classifications
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- A—HUMAN NECESSITIES
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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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)
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- 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
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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Abstract
The invention discloses a kind of anti-aging black ginger extracts and preparation method thereof.The preparation method of the anti-aging black ginger extract after black ginger active component liquid nitrogen frozen, is broken into powder, is obtained black ginger powder using black ginger active component as raw material；Then it is extracted using black ginger powder, obtains anti-aging black ginger extract.The anti-aging black ginger extract that the present invention obtains is deep ace-high long-lived food materials, can be by inhibiting nonenzymatic glycosylation of protein reaction to prevent the generation of glycation product, to reduce the incidence of age-related chronic disease and Protein degradation；In addition, also there is significant improvement result to learning memory disorder, enhance brain free radical Scavenging activity, the denaturation for improving hippocampal neuron falls off.
Description
Technical field
The present invention relates to biological product technical fields, more particularly to a kind of anti-aging black ginger extract and its preparation side
Method.
Background technique
Black ginger, scientific name Kaempferia parviflora Wall.Ex Braker, belongs to zingiberaceous plant, Japan also by
Referred to as RADIX CURCUMAE.Black ginger is spontaneous centered on Southeast Asia or cultivates, because can easily obtain.It is regarded in the black ginger of Thailand
It is locality since ancient times with regard to the conventional foodstuff of daily consumption for one kind of traditional herbal medicines.Civil in locality, black ginger is just used to grow
Support strong, enhancing energy, reduction blood glucose, regain one's strength, improve circulation, improve indigestion etc..
Zingiberaceous plant is broadly divided into zingiber, turmeric and three kinds of black zingiber.The main special composition of ginger is ginger oil,
Its effect is to improve blood flow, has perspiration, is commonly used in the products such as stacte, essential oil.Curcuma it is main special
Ingredient is turmeric, and effect is to improve liver function, prevents senile dementia.The main special composition of black ginger is more methoxies
Base class flavones, effect are anti-oxidant, expansion blood vessel, antiallergy, anti-obesity, pre- anti-aging.It was reported that Polymethoxylated class is yellow
Ketone can activate longevity gene, and anti-aging effect is 15 times of white reed alcohol.
But due to Polymethoxylated flavonoids be liposoluble substance, and in black ginger in addition to containing more methyl oxygen flavones with
Outside, also contain the small polar substances such as big polar substances and essential oil, fat-soluble pigment such as pectin, protein, flavonoid glycoside, this
Black ginger extract is undoubtedly increased in the difficulty extracted and the later period isolates and purifies.
Application No. is 201580026991.3 patents of invention to disclose a kind of black gingerin extract and its manufacturing method,
It makes water, hydrophilic solvent or their mixture contact black ginger first, extracts methoxy flavone, obtains intermediate extract,
Then the greases such as soybean oil are made to contact intermediate extract, to achieve the purpose that extract methoxy flavone.But this method
The disadvantage is that the complicated component of grease introduces other impurity for being difficult to remove while this causes to extract methoxy flavone.
Summary of the invention
The first object of the present invention is to provide a kind of preparation method of anti-aging extract, using black ginger active component as
Raw material is broken into powder after black ginger active component liquid nitrogen frozen, obtains black ginger powder；Then it is extracted, is obtained using black ginger powder
Anti-aging black ginger extract.
The present invention discloses a kind of preparation method of anti-aging black ginger extract, comprising the following steps:
Step 1: using black ginger active component as raw material, black ginger active component being put into liquid nitrogen, keeps 3~10 points of freezing
Clock；Real black ginger active component will be frozen to take out, powder is broken into, is sieved, obtains black ginger powder；
Step 2: black ginger powder is weighed, according to solid-liquid ratio 1:(10~20) ethyl acetate is added in (g/mL), returns in 80~90 DEG C
Stream extracts 4~8 hours, collects extracting solution；Isometric water is added into extracting solution to extract 0.5~1.5 hour, separates upper layer
The water phase of ethyl acetate phase and lower layer；The ethyl acetate phase on upper layer is dried under reduced pressure removing ethyl acetate, then vacuum refrigeration is dry
It is dry, obtain the anti-aging black ginger extract.
The present invention discloses a kind of preparation method of anti-aging black ginger extract, comprising the following steps:
Step 1: using black ginger active component as raw material, black ginger active component being put into liquid nitrogen, keeps 3~10 points of freezing
Clock；Real black ginger active component will be frozen to take out, powder is broken into, is sieved, obtains black ginger powder；
Step 2: black ginger powder is weighed, according to solid-liquid ratio 1:(100~150) 0.5~1.5mol/ of molar concentration is added in (g/mL)
L pyridinium bromide saline solution, microwave abstracting 5~10 minutes under conditions of 300~400W of microwave power, 40~60 DEG C of temperature,
20~30 DEG C are then naturally cooling to, microwave abstracting liquid is collected；
Step 3: by microwave abstracting liquid vacuum freeze drying, obtaining microwave abstracting concentrate；By microwave abstracting concentrate column
Chromatography, using ethyl acetate as eluant, eluent, collects ethyl acetate eluent using silica gel as column packing；Ethyl acetate is eluted
Liquid is dried under reduced pressure removing ethyl acetate, then vacuum freeze drying, obtains the anti-aging black ginger extract.
The present invention discloses a kind of preparation method of anti-aging black ginger extract, comprising the following steps:
Step 1: using black ginger active component as raw material, black ginger active component being put into liquid nitrogen, keeps 3~10 points of freezing
Clock；Real black ginger active component will be frozen to take out, powder is broken into, is sieved, obtains black ginger powder；
Step 2: black ginger powder is weighed, according to solid-liquid ratio 1:(100~150) 0.5~1.5mol/ of molar concentration is added in (g/mL)
L pyridinium bromide saline solution, microwave abstracting 5~10 minutes under conditions of 300~400W of microwave power, 40~60 DEG C of temperature,
20~30 DEG C are then naturally cooling to, microwave abstracting liquid is collected；
Step 3: by microwave abstracting liquid vacuum freeze drying, obtaining microwave abstracting concentrate；By microwave abstracting concentrate column
Chromatography, using ethyl acetate as eluant, eluent, collects ethyl acetate eluent using silica gel as column packing；Ethyl acetate is eluted
Liquid is dried under reduced pressure removing ethyl acetate, then vacuum freeze drying, obtains ethyl acetate extract；
Step 4: by ethyl acetate extract n-hexane and the ethyl alcohol of volume fraction 40~90% with volume ratio 1:(0.5
~1.5) it extracts 2~4 hours, separates the n-hexane phase on upper layer and the ethyl alcohol phase of lower layer, the ethyl alcohol of lower layer is mutually dried under reduced pressure
After ethyl alcohol, vacuum freeze drying obtains the anti-aging black ginger extract.
The present invention discloses a kind of preparation method of anti-aging black ginger extract, comprising the following steps:
Step 1: using black ginger active component as raw material, black ginger active component being put into liquid nitrogen, keeps 3~10 points of freezing
Clock；Real black ginger active component will be frozen to take out, powder is broken into, is sieved, obtains black ginger powder；
Step 2: black ginger powder is weighed, according to solid-liquid ratio 1:(100~150) 0.5~1.5mol/ of molar concentration is added in (g/mL)
L pyridinium bromide saline solution, microwave abstracting 5~10 minutes under conditions of 300~400W of microwave power, 40~60 DEG C of temperature,
20~30 DEG C are then naturally cooling to, microwave abstracting liquid is collected；
Step 3: by microwave abstracting liquid vacuum freeze drying, obtaining microwave abstracting concentrate；By microwave abstracting concentrate column
Chromatography, using ethyl acetate as eluant, eluent, collects ethyl acetate eluent using silica gel as column packing；Ethyl acetate is eluted
Liquid is dried under reduced pressure removing ethyl acetate, then vacuum freeze drying, obtains ethyl acetate extract；
Step 4: being three equal parts by ethyl acetate extract parts by weights；By first part of ethyl acetate extract n-hexane
With the ethyl alcohol of the volume fraction 40~90% of pH2.0 with solid-to-liquid ratio 1:(20~40): (20~40) (g/mL/mL) extraction 2~4 is small
When, the n-hexane phase on upper layer and the ethyl alcohol phase of lower layer are separated, the ethyl alcohol of lower layer is mutually labeled as ethanol extract I；By second part
The ethyl alcohol of the volume fraction 40~90% of ethyl acetate extract n-hexane and pH7.5 is with solid-to-liquid ratio 1:(20~40): (20~
40) (g/mL/mL) is extracted 2~4 hours, separates the n-hexane phase on upper layer and the ethyl alcohol phase of lower layer, the ethyl alcohol of lower layer is mutually marked
For ethanol extract II；By the ethyl alcohol of the volume fraction 40~90% of third part ethyl acetate extract n-hexane and pH8.3
With solid-to-liquid ratio 1:(20~40): (20~40) (g/mL/mL) is extracted 2~4 hours, separates the n-hexane phase on upper layer and the second of lower layer
The ethyl alcohol of lower layer is mutually labeled as ethanol extract III by alcohol phase；Merge ethanol extract I, ethanol extract II and ethyl alcohol to extract
Liquid III, after being dried under reduced pressure removal ethyl alcohol, vacuum freeze drying obtains the anti-aging black ginger extract.
The ethyl alcohol of the volume fraction 70% of pH2.0 in the present invention, the ethyl alcohol and pH8.3 of the volume fraction 70% of pH7.5
Volume fraction 70% ethyl alcohol, adjust to obtain using the hydrochloric acid of 1mol/L or the sodium hydrate aqueous solution of 1mol/L.
The black ginger active component is one of black ginger leaves portion, flower portion, rhizome portion or a variety of mixtures.
The pyridinium bromide salt is bromination 1- ethylpyridine, 1butylpyridinium bromide, bromination 1- n-hexyl pyridine, bromination
One of 1- n-octyl pyridine, bromination 1- positive decyl pyridine, bromination 1- n-dodecane yl pyridines or a variety of mixtures.
Bromination 1- ethylpyridine, 1butylpyridinium bromide, bromination 1- n-hexyl pyridine, bromination 1- n-octyl is respectively adopted
Pyridine, bromination 1- positive decyl pyridine, bromination 1- n-dodecane yl pyridines are followed the steps below and are mentioned as pyridinium bromide salt
It takes: weighing black ginger powder, the pyridinium bromide saline solution of molar concentration 1mol/L is added according to solid-liquid ratio 1:130 (g/mL), micro-
Microwave abstracting 5 minutes under conditions of wave power 400W, temperature 50 C are then naturally cooling to 26 DEG C, collect microwave abstracting liquid；It will
Microwave abstracting liquid vacuum freeze drying, obtains microwave abstracting concentrate.According to following formula calculating recovery rate: recovery rate (%)=
Microwave abstracting concentrate weight/black ginger active component weight × 100%.Be computed, recovery rate is followed successively by 10.3%, 13.1%,
16.6%, 16.9%, 19.8%, 14.9%.Therefore conclude that the pyridinium bromide salt is preferably bromination 1- positive decyl pyrrole
Pyridine.This may be the length because of pyridinium bromide salt alkyl chain, the polarity of pyridinium bromide saline solution on the one hand be affected, into one
Step affects the dissolution of more methyl flavonoids effective components；The variation of another aspect alkyl chain length, leads to pyridinium bromide salt water
The broken wall ability of solution also changes；Both comprehensive collective effect, selects bromination 1- positive decyl pyridine as pyridinium bromide
Salt extracts.
The second object of the present invention is to provide a kind of anti-aging black ginger extract, using any of the above-described kind of anti-aging black ginger
The preparation method of extract processes to obtain.
The black ginger extract can be processed into black ginger extract soft capsule, black ginger extract hard capsule, black ginger extract
The form of granula, black ginger extract tablet.
In concrete application example of the invention, a kind of preparation method of black ginger extract granule is disclosed.The black ginger
Extract particles agent the preparation method comprises the following steps: weighing 2~3g of starch, 20~40g of filler, 0.5~1.5g of citric acid, menthol
0.1~0.3g after pulverizing and sieving, is uniformly mixed, obtains auxiliary material；Anti-aging black 70~100g of ginger extract is taken, auxiliary material is added to
In, after mixing, the polyvinylpyrrolidone of 1.5~4g is added as adhesive, is sufficiently mixed, using wet granulation,
Sieving carries out whole grain after dry, obtains the anti-aging black ginger extract granule.The filler be antierythrite and/or
Mannitol.Preferably, the filler is antierythrite and mannitol with weight ratio (1~3): 1 mixture formed.
The present invention has the advantage that compared with the existing technology
1, powder is beaten using liquid nitrogen frozen in the present invention to handle black ginger, beat its other party such as powder, broken homogenate with drying
Formula is compared, and liquid nitrogen frozen, which beats powder, can keep the stability of chemical component in black ginger, avoids polymethoxyflavone isoreactivity substance
Demethylation reaction occurs during drying, so that influencing it uses effect.
2, it is different from the mode that conventionally employed ethyl acetate or ethyl alcohol directly extract, the present invention uses pyridinium bromide
Saline solution is obviously shortened as Extraction solvent, extraction time, this may be since pyridinium bromide saline solution can not only promote
Into the dissolution of Polymethoxylated flavonoids in black ginger, the broken wall of black ginger may also speed up.
3, the special composition in black ginger is Polymethoxylated flavonoids, is fat-soluble substance, is carried out using ionic liquid
It, simultaneously can the impurity such as water-soluble polysaccharide and colloid are molten simultaneously although extracting the dissolution that can promote Polymethoxylated flavonoids
Enter in extracting solution.Water-soluble polysaccharide is removed as eluant, eluent using moderately polar organic solvent ethyl acetate in the present invention
And colloid, reextraction is then carried out using n-hexane-ethyl alcohol, n-hexane extracts small polar essential oil and fat-soluble pigment
Out, there are relatively moderately polar Polymethoxylated flavonoid substances to be then enriched in alcohol phase.The present invention selects ethyl alcohol as two
Secondary extractant another is the reason is that, hydroxylating, hydroxylated more methyl can occur for more methyl flavonoids and ethyl alcohol contact
Flavonoids has better dissolubility and permeability.
4, pH2.0, pH7.5, pH8.3 are the body fluid acidity of human gastric juice, intestinal fluid, big intestinal juice respectively.It will in the present invention
The ethyl acetate extract of black ginger is extracted with the ethyl alcohol of different pH values, is then mixed, and imitates black ginger extract in people
Oral administration environment in body gastrointestinal tract, selects the ethyl alcohol of specific pH into being extracted, and it is mixed to be mixed to get active black ginger extract
Zoarium allows organism to realize the absorption to black ginger extract active constituent to the maximum extent.
The anti-aging black ginger extract that the present invention obtains is deep ace-high long-lived food materials, can be by inhibiting protein non-
Enzymatic conversion reaction prevents the generation of glycation product, to reduce the generation of age-related chronic disease and Protein degradation
Rate；In addition, also there is significant improvement result to learning memory disorder, enhance brain free radical Scavenging activity, improves hippocampal neural
The denaturation of member falls off.
Specific embodiment
Raw material is described below in embodiment:
Black ginger, scientific name Kaempferia parviflora Wall.Ex Braker, source area Thailand.
Bromination 1- positive decyl pyridine is purchased from Chengdu Jia Ye Biotechnology Co., Ltd, and carries out structural confirmation using nuclear-magnetism:
1H NMR (600MHz, DMSO) δ 9.24 (s, 2H, N=CH-), 8.65 (d, J=1.0Hz, 1H ,=CH-), 8.19 (d, J=
13.4Hz, 2H ,=CH-), 4.67 (t, J=10.4Hz, 2H ,=NCH2), 1.94-1.85 (m, 2H ,-CH2), 1.24 (m,
14H,-(CH2)7), 0.83 (t, J=5.3Hz ,-CH3)。
In the case where not illustrating in embodiment, vacuum freeze drying in embodiment specifically comprises the processes of: pre-freeze
- 80 DEG C of temperature, the pre-freeze time 1.5 hours, -70 DEG C of cryogenic temperature, absolute pressure 100Pa, cooling time 48 hours.
Embodiment 1
The preparation method of anti-aging black ginger extract, comprising the following steps:
Step 1: using black race stem as raw material, black race stem being put into liquid nitrogen, keeps freezing 10 minutes；Reality will be frozen
Black race stem takes out, and is broken into powder with pulverizer, crosses 80 meshes, obtain black ginger powder；
Step 2: black ginger powder is weighed, ethyl acetate is added according to solid-liquid ratio 1:10 (g/mL), it is small in 90 DEG C of refluxing extractions 8
When, collect extracting solution；Isometric water is added into extracting solution extract 1 hour, separates ethyl acetate phase and the lower layer on upper layer
Water phase；The ethyl acetate phase on upper layer is dried under reduced pressure removing ethyl acetate under conditions of 50 DEG C, absolute pressure 0.03MPa, so
Vacuum freeze drying afterwards obtains the anti-aging black ginger extract.
Embodiment 2
The preparation method of anti-aging black ginger extract, comprising the following steps:
Step 1: using black race stem as raw material, black race stem being put into liquid nitrogen, keeps freezing 10 minutes；Reality will be frozen
Black race stem takes out, and is broken into powder with pulverizer, crosses 80 meshes, obtain black ginger powder；
Step 2: weighing black ginger powder, the bromination 1- positive last of the ten Heavenly stems of molar concentration 1mol/L is added according to solid-liquid ratio 1:130 (g/mL)
Yl pyridines aqueous solution, microwave abstracting 5 minutes, is then naturally cooling to 26 DEG C under conditions of microwave power 400W, temperature 50 C,
Collect microwave abstracting liquid；
Step 3: by microwave abstracting liquid vacuum freeze drying, obtaining microwave abstracting concentrate；By microwave abstracting concentrate column
Chromatography, using silica gel as column packing, the weight ratio of microwave abstracting concentrate and silica gel is 1:1, using ethyl acetate as eluant, eluent,
The solid-to-liquid ratio of microwave abstracting concentrate and ethyl acetate is 1:5 (g/mL), and elution flow rate 1mL/min collects ethyl acetate and washes
De- liquid；Ethyl acetate eluent is dried under reduced pressure removing ethyl acetate under conditions of 50 DEG C, absolute pressure 0.03MPa, then
Vacuum freeze drying obtains the anti-aging black ginger extract.
Embodiment 3
The preparation method of anti-aging black ginger extract, comprising the following steps:
Step 1: using black race stem as raw material, black race stem being put into liquid nitrogen, keeps freezing 10 minutes；Reality will be frozen
Black race stem takes out, and is broken into powder with pulverizer, crosses 80 meshes, obtain black ginger powder；
Step 2: weighing black ginger powder, the bromination 1- positive last of the ten Heavenly stems of molar concentration 1mol/L is added according to solid-liquid ratio 1:130 (g/mL)
Yl pyridines aqueous solution, microwave abstracting 5 minutes, is then naturally cooling to 26 DEG C under conditions of microwave power 400W, temperature 50 C,
Collect microwave abstracting liquid；
Step 3: by microwave abstracting liquid vacuum freeze drying, obtaining microwave abstracting concentrate；By microwave abstracting concentrate column
Chromatography, using silica gel as column packing, the weight ratio of microwave abstracting concentrate and silica gel is 1:1, using ethyl acetate as eluant, eluent,
The solid-to-liquid ratio of microwave abstracting concentrate and ethyl acetate is 1:5 (g/mL), and elution flow rate 1mL/min collects ethyl acetate and washes
De- liquid；Ethyl acetate eluent is dried under reduced pressure removing ethyl acetate under conditions of 50 DEG C, absolute pressure 0.03MPa, then
Vacuum freeze drying obtains ethyl acetate extract；
Step 4: ethyl acetate extract n-hexane and the ethyl alcohol of volume fraction 70% is small with volume ratio 1:1 extraction 2
When, the solid-to-liquid ratio of ethyl acetate extract and n-hexane is 1:30 (g/mL), separates the n-hexane phase on upper layer and the ethyl alcohol of lower layer
Phase, after the ethyl alcohol of lower layer is mutually dried under reduced pressure removal ethyl alcohol under conditions of 50 DEG C, absolute pressure 0.03MPa, vacuum refrigeration is dry
It is dry, obtain the anti-aging black ginger extract.
Embodiment 4
The preparation method of anti-aging black ginger extract, comprising the following steps:
Step 1: using black race stem as raw material, black race stem being put into liquid nitrogen, keeps freezing 10 minutes；Reality will be frozen
Black race stem takes out, and is broken into powder with pulverizer, crosses 80 meshes, obtain black ginger powder；
Step 2: weighing black ginger powder, the bromination 1- positive last of the ten Heavenly stems of molar concentration 1mol/L is added according to solid-liquid ratio 1:130 (g/mL)
Yl pyridines aqueous solution, microwave abstracting 5 minutes, is then naturally cooling to 26 DEG C under conditions of microwave power 400W, temperature 50 C,
Collect microwave abstracting liquid；
Step 3: by microwave abstracting liquid vacuum freeze drying, obtaining microwave abstracting concentrate；By microwave abstracting concentrate column
Chromatography, using silica gel as column packing, the weight ratio of microwave abstracting concentrate and silica gel is 1:1, using ethyl acetate as eluant, eluent,
The solid-to-liquid ratio of microwave abstracting concentrate and ethyl acetate is 1:5 (g/mL), and elution flow rate 1mL/min collects ethyl acetate and washes
De- liquid；Ethyl acetate eluent is dried under reduced pressure removing ethyl acetate under conditions of 50 DEG C, absolute pressure 0.03MPa, then
Vacuum freeze drying obtains ethyl acetate extract；
Step 4: being three equal parts by ethyl acetate extract parts by weights；By first part of ethyl acetate extract n-hexane
Ethyl alcohol with the volume fraction 70% of pH2.0 separates the n-hexane on upper layer with solid-to-liquid ratio 1:30:30 (g/mL/mL) extraction 2 hours
Mutually with the ethyl alcohol phase of lower layer, the ethyl alcohol of lower layer is mutually labeled as ethanol extract I；By second part of ethyl acetate extract use just oneself
The ethyl alcohol of the volume fraction 70% of alkane and pH7.5 with solid-to-liquid ratio 1:30:30 (g/mL/mL) extraction 2 hours, separate upper layer just oneself
The ethyl alcohol of lower layer is mutually labeled as ethanol extract II by the ethyl alcohol phase of alkane phase and lower layer；Third part ethyl acetate extract is used
The ethyl alcohol of the volume fraction 70% of n-hexane and pH8.3 separates upper layer with solid-to-liquid ratio 1:30:30 (g/mL/mL) extraction 2 hours
The ethyl alcohol of lower layer is mutually labeled as ethanol extract III by the ethanol water phase of n-hexane phase and lower layer；Merge ethanol extract I, second
Alcohol extract II and ethanol extract III, after removal ethyl alcohol is dried under reduced pressure under conditions of 50 DEG C, absolute pressure 0.03MPa, very
Vacuum freecing-dry obtains the anti-aging black ginger extract.
Test case 1
The inhibiting rate that black ginger extract anti-aging to Examples 1 to 4 generates nonenzymatic glycosylation of protein product detects.
Nonenzymatic glycosylation of protein refers under the conditions of non-enzymatic, the system that the aldehyde radical and protein amino of reducing sugar occur
Column reaction, ultimately forms non-metallocene single site catalyst.It is big that non-metallocene single site catalyst further can directly be crosslinked vivo biodistribution
Molecule causes its function to damage.When the collagen or elastin of the non-metallocene single site catalyst combination human body of accumulation,
It will lead to cutis laxa, colour of skin dimness again and the aging phenomenons such as wrinkle occur.
The foundation of nonenzymatic glycosylation of protein reaction system
Aseptically, with the 0.1mol/ containing 8mmol/L EDTA, 100U/mL penicillin and 100U/mL streptomysin
L, the PBS buffer solution dissolution bovine serum albumin(BSA) and glucose of pH7.4, so that bovine serum albumin(BSA) concentration is 20g/L, glucose
Concentration is 400mmol/L.Control group is set simultaneously: (1) anti-aging black ginger extract is not added and is completely saccharified reaction system；(2)
Bovine serum albumin(BSA) control；(3) add anti-aging black ginger extract that the saccharification system of bovine serum albumin(BSA) is not added；(4) plus it is anti-aging
The saccharification system of glucose is not added in black ginger extract；(5) plus anti-aging black ginger extract is completely saccharified reaction system.Above-mentioned
Anti-aging black ginger extract or aminoguanidine sulfate (positive controls) are added in nonenzymatic glycosylation of protein reaction system, makes its end
Concentration is 0.1mg/mL, is placed in 37 DEG C of thermostatic drying chambers and is protected from light incubation.Measure absorbance A at each pipe 530nm after 20 days, 40 days
After measure each pipe fluorescence intensity F, according to following equation calculate separately out to saccharification early stage product, advanced glycosylation end products suppression
Rate processed.
The measurement of saccharification early stage product
It takes 200 μ L of each group reaction solution in tool plug test tube, adds 8mL 0.1g/LNBT solution (with 0.1mol/L, p H=
10.8 sodium carbonate-bicarbonate buffer solution configuration) it is uniformly mixed to be placed in 37 DEG C of thermostatic drying chambers and reacts 15 minutes, so
15% acetic acid of 0.4mL is added afterwards and is terminated with cold bath and reacts, it is cooling after with ultraviolet/visible spectrophotometer record its
Absorbance value A at 530nm.
The calculation formula for the early stage Product inhibiton rate that is saccharified is as follows: IR={ 1- [medicine group (5) A- control group (3) A- control group
(4) A]/[control group (1) A- control group (2) A] } × 100%.
Specific test result is shown in Table 1.
The inhibiting rate that the anti-aging black ginger extract of table 1 generates saccharification early stage product
The measurement of Advanced glycation end products
It is anti-that each group is measured under the conditions of excitation wavelength 370nm, launch wavelength 440nm, slit 5nm with sepectrophotofluorometer
Answer the fluorescence intensity F of liquid.
The calculation formula of Advanced glycation end products inhibiting rate is as follows: IR={ 1- [medicine group (5) F- control group (3) F- control group
(4) F]/[control group (1) F- control group (2) F] } × 100%.
Specific test result is shown in Table 2.
The inhibiting rate that the anti-aging black ginger extract of table 2 generates Advanced glycation end products
| Group | Inhibiting rate (%) |
| Positive controls | 47.65 |
| Embodiment 1 | 38.01 |
| Embodiment 2 | 51.70 |
| Embodiment 3 | 56.95 |
| Embodiment 4 | 62.33 |
As can be seen from the above experimental data, anti-aging black ginger extract of the present invention is to saccharification early stage product and saccharification
The generation of dead end product has certain inhibiting effect, this proves that anti-aging black ginger extract can inhibit external nonenzymatic glycosylation,
With being used as natural and immunomodulator and anti-saccharification skin care item, health care product, the potentiality in drug.
Test case 2
Black ginger extract anti-aging to Examples 1 to 4 is to ability of learning and memory in mice, superoxide dismutase activity and third
Dialdehyde content is detected.
Experimental animal: Kunming mouse, 18~22g of weight, half male and half female are purchased from Beijing dimension tonneau China experimental animal technology
Co., Ltd.
The foundation of memory consolidation obstacle mouse model and Mice water maze experiment: Kunming mouse is randomly divided into blank pair
According to group, the test group of model control group and embodiment 1-4, totally 6 groups, every group 10, every group of half male and half female.Test group stomach-filling is given
The anti-aging black ginger extract of 6.66mg/kg dosage, blank control, model control group give the distilled water of equivalent respectively, and daily 1
It is secondary, continuous 13 days.Start within medicine feed the 10th day to carry out water maze laboratory: water maze laboratory continues 4 days, daily test 1 time, wraps every time
Include 2 place of entry；When test, the place of entry without platform quadrant is randomly choosed, into the water towards pool wall by mouse, allows its freedom
Platform is found, and is stopped 20 seconds on platform, its escape latency is recorded；It, will if mouse does not find platform in 90 seconds
It leads to platform, and escape latency is denoted as 90 seconds.Take the average value of 2 escape latencies of every mouse as one day daily
School grade；Daily after training, in addition to blank control group gives physiological saline, remaining each group mouse is injected intraperitoneally immediately
Sodium nitrite 120mg/kg.
Specific test result is shown in Table 3.
Influence of the anti-aging black ginger extract of table 3 to memory consolidation obstacle water maze test in mice escape latency
Can be seen that anti-aging black ginger extract from above-mentioned test data can significantly shorten memory consolidation obstacle mouse water
Labyrinth orients the escape latency of swimming test, improves the ability of learning and memory that sodium nitrite causes memory consolidation obstacle mouse.
The measurement of superoxide dismutase activity and mda content in Mice brain tissues
After water maze is tested, broken end takes brain, and with pre-cooling normal saline flushing surface blood, filter paper is wiped dry, takes one
4 DEG C of physiological saline is added with weight ratio 1:9, the homogenate of mass fraction 10% is made, with 4000 revs/min in 4 for half brain tissue
It DEG C centrifugation 15 minutes, takes supernatant, measures superoxide dismutase activity and mda content.
Superoxide dismutase (SOD) kit, is purchased from Nanjing and builds up Bioengineering Research Institute.
Malonaldehyde (MDA) kit, is purchased from Nanjing and builds up Bioengineering Research Institute.
Specific test result is shown in Table 4.
The anti-aging black ginger extract of table 4 is to memory consolidation obstacle Mice brain tissues superoxide dismutase activity and malonaldehyde
The influence of content
Can be seen that anti-aging black ginger extract from above-mentioned test data can significantly reduce memory consolidation obstacle mouse the third two
Aldehyde improves superoxide dismutase activity, reaches the ability that enhancing mouse removes free radical.
In conclusion anti-aging black ginger extract can improve the learning and memory energy that sodium nitrite causes memory consolidation obstacle mouse
Power, mechanism of action it is related may to reduce Free Radical Level with raising body radicals scavenging power.
The present invention is different from the prior art, and has the following characteristics that
1, powder is beaten using liquid nitrogen frozen to handle black ginger, compared with the other modes such as powder, broken homogenate are beaten in drying, liquid
Chilled nitrogen, which beats powder, can keep the stability of chemical component in black ginger, avoid polymethoxyflavone isoreactivity substance in dry mistake
Demethylation reaction occurs in journey, so that influencing it uses effect.
2, it is different from the mode that conventionally employed ethyl acetate or ethyl alcohol directly extract, the present invention uses pyridinium ion
Saline solution is obviously shortened as Extraction solvent, extraction time, this may be since pyridinium ion saline solution can not only promote
Into the dissolution of Polymethoxylated flavonoids in black ginger, the broken wall of black ginger may also speed up.
3, the special composition in black ginger is Polymethoxylated flavonoids, is fat-soluble substance, is carried out using ionic liquid
It, simultaneously can the impurity such as water-soluble polysaccharide and colloid are molten simultaneously although extracting the dissolution that can promote Polymethoxylated flavonoids
Enter in extracting solution.Water-soluble polysaccharide is removed as eluant, eluent using moderately polar organic solvent ethyl acetate in the present invention
And colloid, reextraction is then carried out using n-hexane-ethyl alcohol, n-hexane extracts small polar essential oil and fat-soluble pigment
Out, there are relatively moderately polar Polymethoxylated flavonoid substances to be then enriched in alcohol phase.The present invention selects ethyl alcohol as two
Secondary extractant another is the reason is that, hydroxylating, hydroxylated more methyl can occur for more methyl flavonoids and ethyl alcohol contact
Flavonoids has better dissolubility and permeability.
4, pH2.0, pH7.5, pH8.3 are the body fluid acidity of human gastric juice, intestinal fluid, big intestinal juice.By black ginger in the present invention
Ethyl acetate extract extracted with the ethyl alcohol of different pH values, then mix, imitate black ginger extract in organism
Oral administration environment in gastrointestinal tract, selects the ethyl alcohol of specific pH into being extracted, and is mixed to get the mixing of active black ginger extract
Body meets organism absorption of drugs characteristic, effective substance can be made farthest to extract, and keeps organism maximum
Realize to limit the absorption to black ginger extract active constituent.
Application examples 1
The preparation of anti-aging black ginger extract granule
Starch 2g, antierythrite 30g, mannitol 10g, citric acid 1.5g, menthol 0.3g are weighed, crushed 60 meshes
Afterwards, it is uniformly mixed, obtains auxiliary material；The anti-aging black ginger extract 80g of Example 4, is added in auxiliary material, after mixing,
The polyvinylpyrrolidone of 1.5g is added as adhesive, is sufficiently mixed, using wet granulation, crosses 60 meshes, 40 DEG C of dryings 5
Whole grain is carried out after hour, obtains the anti-aging black ginger extract granule.
Application examples 2
The preparation of anti-aging black ginger extract granule
Starch 2g, mannitol 40g, citric acid 1.5g, menthol 0.3g are weighed, after crushed 60 meshes, is uniformly mixed, obtains
To auxiliary material；The anti-aging black ginger extract 80g of Example 4, is added in auxiliary material, after mixing, adds the poly- of 1.5g
Vinylpyrrolidone is sufficiently mixed as adhesive, using wet granulation, crosses 60 meshes, 40 DEG C carry out after drying 5 hours it is whole
Grain, obtains the anti-aging black ginger extract granule.
Application examples 3
The preparation of anti-aging black ginger extract granule
Starch 2g, antierythrite 40g, citric acid 1.5g, menthol 0.3g are weighed, after crushed 60 meshes, is uniformly mixed,
Obtain auxiliary material；The anti-aging black ginger extract 80g of Example 4, is added in auxiliary material, after mixing, adds 1.5g's
Polyvinylpyrrolidone is sufficiently mixed as adhesive, using wet granulation, crosses 60 meshes, 40 DEG C carry out after drying 5 hours it is whole
Grain, obtains the anti-aging black ginger extract granule.
Starch, food-grade, No. CAS: 9005-25-8.
Antierythrite, food-grade, No. CAS: 149-32-6.
Mannitol, food-grade, No. CAS: 87-78-5.
Citric acid, food-grade, No. CAS: 5949-29-1.
Menthol, food-grade, No. CAS: 89-78-1.
Polyvinylpyrrolidone, food-grade, No. CAS: 9003-39-8.
Male SD rat (200~220g of weight, be purchased from Shanghai Slac Experimental Animal Co., Ltd.) is taken, random point
Group is respectively labeled as blank group, model group, anti-aging black ginger extract granule group, to the other groups of rats in addition to blank group
Stomach-filling hypoxanthine suspension and intraperitoneal injection Oteracil Potassium emulsion are carried out, hyperuricemia model is established；1 hour after modeling
The anti-aging black ginger extract granule aqueous solution of stomach-filling again, then (be administered after 2 hours) starts to take 3 hours after modeling respectively
Blood will dilute 3 times of 20 μ L of sample introduction under the conditions of following HPLC chromatogram after rat plasma sample.Blank group is recorded respectively, model group, is resisted
The peak area of aging black ginger extract granule group peak area and internal standard compound alpha-Naphthol, calculates separately model group according to standard curve
And the content of galangal alcohol extracting group blood uric acid.
The preparation of anti-aging black ginger extract granule aqueous solution: taking anti-aging black ginger extract granule 25g, and water is added
5mL is stirred 1 minute with 80 revs/min, and filtering obtains anti-aging black ginger extract granule aqueous solution.
The processing of rat plasma: take rat blank blood 0.5mL in 1.5mL Eppendorf pipe water-bath after twenty minutes,
3700 revs/min are centrifuged 10 minutes, obtain rat blank plasma；100 μ L rat blank plasmas are measured later in 1.5mL's
In Eppendorf pipe, then it is sequentially added into the inner mark solution (i.e. 0.2mg/mL, alpha-Naphthol solution) of 20 μ L, 50 μ L uric acid marks
It is added 900 μ L chromatography methanol after quasi- product solution, is vortexed and mixes, 10000 revs/min of high speed centrifugations take that 400 μ L's is upper after ten minutes
Clear liquid finally adds 400 μ L, 0.2% acetic acid aqueous solution to be vortexed again and mixes, crosses 0.22 μm of organic filter membrane of one-shot injector formula, obtain
Treated rat plasma.
Chromatographic condition is as follows:
Chromatographic column: Shimadzu Shim-pack CLC-C8 (M) (150 × 4.6mm L.D)；
Mobile phase: methanol: 0.2% acetic acid aqueous solution=6:94 (v/v)；
Flow velocity: 1.0mL/min；
Column temperature: 37 DEG C；
Detection wavelength: 288nm；
Sample volume: 20 μ L；
Internal standard: alpha-Naphthol.
Specific test result is shown in Table 5.
Influence of the anti-aging black ginger extract granule of table 5 to serum uric acid level content
Above-mentioned experimental data shows that uric acid can be significantly reduced in anti-aging black ginger extract granule, and wherein application examples 1 drops
Inefficient fruit is the most significant.Since the active constituent majority of anti-aging black ginger extract is fat-soluble, so present invention selection is water-soluble
The preferable filler of property.Mannitol, which has, is easy to crystallize pleasantly sweet, glycometabolism that is not easy to moisture absorption and being not involved in human body, antierythrite
Heat is lower and high temperature resistant, has no toxic side effect.Mannitol and antierythrite are mixed in a certain proportion as filler in the present invention,
It has been surprisingly found that the dissolution that can promote anti-aging black ginger extract, improves the bioavilability of anti-aging black ginger extract.
It should be appreciated that although this specification is described in terms of embodiments, but not each embodiment only includes one
A independent technical solution, for the sake of this narrating mode of specification is used for the purpose of clearly, those skilled in the art should be incited somebody to action
As a whole, the technical solutions in the various embodiments may also be suitably combined for specification, and forming those skilled in the art can
With the other embodiments of understanding.
Claims (10)
1. the preparation method of anti-aging black ginger extract, which is characterized in that using black ginger active component as raw material, black ginger is effective
After the liquid nitrogen frozen of position, it is broken into powder, obtains black ginger powder；Then it is extracted using black ginger powder, obtains anti-aging black ginger and extract
Object.
2. the preparation method of anti-aging black ginger extract according to claim 1, which comprises the following steps:
Step 1: using black ginger active component as raw material, black ginger active component being put into liquid nitrogen, keeps freezing 3~10 minutes；
Real black ginger active component will be frozen to take out, powder is broken into, is sieved, obtains black ginger powder；
Step 2: black ginger powder is weighed, according to solid-liquid ratio 1:(100~150) 0.5~1.5mol/L of molar concentration bromine is added in (g/mL)
Change pyridine saline solution, microwave abstracting 5~10 minutes under conditions of 300~400W of microwave power, 40~60 DEG C of temperature, then
20~30 DEG C are naturally cooling to, microwave abstracting liquid is collected；
Step 3: by microwave abstracting liquid vacuum freeze drying, obtaining microwave abstracting concentrate；Microwave abstracting concentrate column is chromatographed
Separation, using ethyl acetate as eluant, eluent, collects ethyl acetate eluent using silica gel as column packing；Ethyl acetate eluent is subtracted
Pressure dries and removes ethyl acetate, and then vacuum freeze drying, obtains the anti-aging black ginger extract.
3. the preparation method of anti-aging black ginger extract according to claim 1, which comprises the following steps:
Step 1: using black ginger active component as raw material, black ginger active component being put into liquid nitrogen, keeps freezing 3~10 minutes；
Real black ginger active component will be frozen to take out, powder is broken into, is sieved, obtains black ginger powder；
Step 2: black ginger powder is weighed, according to solid-liquid ratio 1:(100~150) 0.5~1.5mol/L of molar concentration bromine is added in (g/mL)
Change pyridine saline solution, microwave abstracting 5~10 minutes under conditions of 300~400W of microwave power, 40~60 DEG C of temperature, then
20~30 DEG C are naturally cooling to, microwave abstracting liquid is collected；
Step 3: by microwave abstracting liquid vacuum freeze drying, obtaining microwave abstracting concentrate；Microwave abstracting concentrate column is chromatographed
Separation, using ethyl acetate as eluant, eluent, collects ethyl acetate eluent using silica gel as column packing；Ethyl acetate eluent is subtracted
Pressure dries and removes ethyl acetate, and then vacuum freeze drying, obtains ethyl acetate extract；
Step 4: by ethyl acetate extract n-hexane and the ethyl alcohol of volume fraction 40~90% with volume ratio 1:(0.5~
1.5) it extracts 2~4 hours, separates the n-hexane phase on upper layer and the ethyl alcohol phase of lower layer, the ethyl alcohol of lower layer is mutually dried under reduced pressure removal
After ethyl alcohol, vacuum freeze drying obtains the anti-aging black ginger extract.
4. the preparation method of anti-aging black ginger extract according to claim 1, which comprises the following steps:
Step 1: using black ginger active component as raw material, black ginger active component being put into liquid nitrogen, keeps freezing 3~10 minutes；
Real black ginger active component will be frozen to take out, powder is broken into, is sieved, obtains black ginger powder；
Step 2: black ginger powder is weighed, according to solid-liquid ratio 1:(100~150) 0.5~1.5mol/L of molar concentration bromine is added in (g/mL)
Change pyridine saline solution, microwave abstracting 5~10 minutes under conditions of 300~400W of microwave power, 40~60 DEG C of temperature, then
20~30 DEG C are naturally cooling to, microwave abstracting liquid is collected；
Step 3: by microwave abstracting liquid vacuum freeze drying, obtaining microwave abstracting concentrate；Microwave abstracting concentrate column is chromatographed
Separation, using ethyl acetate as eluant, eluent, collects ethyl acetate eluent using silica gel as column packing；Ethyl acetate eluent is subtracted
Pressure dries and removes ethyl acetate, and then vacuum freeze drying, obtains ethyl acetate extract；
Step 4: being three equal parts by ethyl acetate extract parts by weights；By first part of ethyl acetate extract n-hexane and
The ethyl alcohol of the volume fraction 40~90% of pH2.0 is with solid-to-liquid ratio 1:(20~40): (20~40) (g/mL/mL) extraction 2~4 is small
When, the n-hexane phase on upper layer and the ethyl alcohol phase of lower layer are separated, the ethyl alcohol of lower layer is mutually labeled as ethanol extract I；By second part
The ethyl alcohol of the volume fraction 40~90% of ethyl acetate extract n-hexane and pH7.5 is with solid-to-liquid ratio 1:(20~40): (20~
40) (g/mL/mL) is extracted 2~4 hours, separates the n-hexane phase on upper layer and the ethyl alcohol phase of lower layer, the ethyl alcohol of lower layer is mutually marked
For ethanol extract II；By the ethyl alcohol of the volume fraction 40~90% of third part ethyl acetate extract n-hexane and pH8.3
With solid-to-liquid ratio 1:(20~40): (20~40) (g/mL/mL) is extracted 2~4 hours, separates the n-hexane phase on upper layer and the second of lower layer
The ethyl alcohol of lower layer is mutually labeled as ethanol extract III by alcohol phase；Merge ethanol extract I, ethanol extract II and ethyl alcohol to extract
Liquid III, after being dried under reduced pressure removal ethyl alcohol, vacuum freeze drying obtains the anti-aging black ginger extract.
5. the preparation method of anti-aging black ginger extract according to claim 1, which is characterized in that the black effective portion of ginger
Position is one of black ginger leaves portion, flower portion, rhizome portion or a variety of mixtures.
6. the preparation method of anti-aging black ginger extract according to any one of claim 2~4, which is characterized in that institute
Stating pyridinium bromide salt is bromination 1- ethylpyridine, 1butylpyridinium bromide, bromination 1- n-hexyl pyridine, bromination 1- n-octyl pyrrole
One of pyridine, bromination 1- positive decyl pyridine, bromination 1- n-dodecane yl pyridines or a variety of mixtures.
7. the preparation method of anti-aging black ginger extract according to claim 6, which is characterized in that the pyridinium bromide salt
For bromination 1- positive decyl pyridine.
8. anti-aging black ginger extract, which is characterized in that mentioned using anti-aging black ginger according to any one of claims 1 to 7
The preparation method of object is taken to process to obtain.
9. anti-aging black ginger extract according to claim 8, which is characterized in that the black ginger extract can be processed into black
Ginger extract soft capsule, black ginger extract hard capsule, the form of black ginger extract granule, black ginger extract tablet.
10. anti-aging black ginger extract according to claim 9, it is characterised in that: the black ginger extract granule
The preparation method comprises the following steps: weighing 2~3g of starch, 20~40g of filler, 0.5~1.5g of citric acid, 0.1~0.3g of menthol, crushed
After sieve, it is uniformly mixed, obtains auxiliary material；Anti-aging black 70~100g of ginger extract is taken, is added in auxiliary material, after mixing, then
The polyvinylpyrrolidone of 1.5~4g is added as adhesive, is sufficiently mixed, using wet granulation, sieving carries out whole after dry
Grain, obtains the anti-aging black ginger extract granule.
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| CN110214952A (en) * | 2019-06-19 | 2019-09-10 | 河南省科学院 | A kind of black ginger powder and preparation method thereof |
| CN113694155A (en) * | 2021-09-24 | 2021-11-26 | 清华大学 | Kaempferia galanga total flavone extract and preparation method and application thereof |
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| CN106455665A (en) * | 2014-05-09 | 2017-02-22 | 三得利控股株式会社 | Fat or oil extract of black ginger and method for producing same |
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| CN106455665A (en) * | 2014-05-09 | 2017-02-22 | 三得利控股株式会社 | Fat or oil extract of black ginger and method for producing same |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110214952A (en) * | 2019-06-19 | 2019-09-10 | 河南省科学院 | A kind of black ginger powder and preparation method thereof |
| CN113694155A (en) * | 2021-09-24 | 2021-11-26 | 清华大学 | Kaempferia galanga total flavone extract and preparation method and application thereof |
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