CN110478437A - A kind of golden hairpin dendrobium extract and preparation method - Google Patents
A kind of golden hairpin dendrobium extract and preparation method Download PDFInfo
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- CN110478437A CN110478437A CN201910775215.3A CN201910775215A CN110478437A CN 110478437 A CN110478437 A CN 110478437A CN 201910775215 A CN201910775215 A CN 201910775215A CN 110478437 A CN110478437 A CN 110478437A
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- 239000000284 extract Substances 0.000 title claims abstract description 27
- 241001523681 Dendrobium Species 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000605 extraction Methods 0.000 title abstract description 8
- 239000003480 eluent Substances 0.000 claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000741 silica gel Substances 0.000 claims abstract description 17
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 17
- 238000004810 partition chromatography Methods 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 10
- 229920005989 resin Polymers 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000001953 recrystallisation Methods 0.000 claims abstract description 9
- 239000006071 cream Substances 0.000 claims abstract description 8
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 7
- 235000011116 calcium hydroxide Nutrition 0.000 claims abstract description 7
- 238000004064 recycling Methods 0.000 claims abstract description 5
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 39
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 13
- 239000004471 Glycine Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 10
- 239000005695 Ammonium acetate Substances 0.000 claims description 10
- 229940043376 ammonium acetate Drugs 0.000 claims description 10
- 235000019257 ammonium acetate Nutrition 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 229920006395 saturated elastomer Polymers 0.000 claims description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 230000005526 G1 to G0 transition Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000003672 processing method Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000013461 design Methods 0.000 claims description 4
- 238000010828 elution Methods 0.000 claims description 4
- 239000006210 lotion Substances 0.000 claims description 4
- 239000011236 particulate material Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 206010013786 Dry skin Diseases 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 229930013930 alkaloid Natural products 0.000 abstract description 21
- 150000003797 alkaloid derivatives Chemical class 0.000 abstract description 19
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000003960 organic solvent Substances 0.000 abstract description 7
- 230000006378 damage Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract 1
- 230000002588 toxic effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 6
- 239000003513 alkali Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 240000004638 Dendrobium nobile Species 0.000 description 4
- 238000004440 column chromatography Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- RYAHJFGVOCZDEI-UFFNCVEVSA-N Dendrobine Chemical compound C([C@H]1CC[C@@H]2[C@@]31C)N(C)[C@@H]3[C@H]1[C@@H](C(C)C)[C@@H]2C(=O)O1 RYAHJFGVOCZDEI-UFFNCVEVSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- RYAHJFGVOCZDEI-CZKZLRAZSA-N dendrobine Natural products O=C1O[C@@H]2[C@H](C(C)C)[C@H]1[C@H]1[C@@]3(C)[C@@H]2N(C)C[C@H]3CC1 RYAHJFGVOCZDEI-CZKZLRAZSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- -1 dendrobine Natural products 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002547 new drug Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000010175 APPswe/PSEN1dE9 Methods 0.000 description 1
- 208000024827 Alzheimer disease Diseases 0.000 description 1
- 201000001320 Atherosclerosis Diseases 0.000 description 1
- 206010018473 Glycosuria Diseases 0.000 description 1
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- 241000712431 Influenza A virus Species 0.000 description 1
- 241000699660 Mus musculus Species 0.000 description 1
- 206010039966 Senile dementia Diseases 0.000 description 1
- ZSJLQEPLLKMAKR-UHFFFAOYSA-N Streptozotocin Natural products O=NN(C)C(=O)NC1C(O)OC(CO)C(O)C1O ZSJLQEPLLKMAKR-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003178 anti-diabetic effect Effects 0.000 description 1
- 239000003472 antidiabetic agent Substances 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000009509 drug development Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 210000001320 hippocampus Anatomy 0.000 description 1
- 208000037797 influenza A Diseases 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000009191 jumping Effects 0.000 description 1
- 238000007726 management method Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000002569 neuron Anatomy 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000011552 rat model Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- ZSJLQEPLLKMAKR-GKHCUFPYSA-N streptozocin Chemical compound O=NN(C)C(=O)N[C@H]1[C@@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O ZSJLQEPLLKMAKR-GKHCUFPYSA-N 0.000 description 1
- 229960001052 streptozocin Drugs 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 238000011830 transgenic mouse model Methods 0.000 description 1
- 230000002792 vascular Effects 0.000 description 1
Classifications
-
- 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)
- A61K36/898—Orchidaceae (Orchid family)
- A61K36/8984—Dendrobium
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
-
- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention provides a kind of golden hairpin dendrobium extract and preparation methods, are raw material by the dry stem of HERBA DENDROBII, are impregnated after broken, diacolation obtains percolate；After milk of lime tune pH, upper macroporous resin column is simultaneously eluted, and eluent tune pH is neutrality, is concentrated under reduced pressure as clear cream；Clear cream is mixed thoroughly with silica gel, and silica gel column partition chromatography obtains eluent, and recrystallization, dry, crushing are after recycling solution to get golden hairpin dendrobium extract.The content of total alkaloid contained by golden hairpin dendrobium extract is greater than 50%.The present invention has advantage in terms of reducing the use of organic solvent, reducing toxic organic solvents to the risk of production technician's body harm, reduction production cost and energy consumption.
Description
Technical field
The invention belongs to Chinese medical extract fields, and in particular to a kind of golden hairpin dendrobium extract and preparation method.
Background technique
HERBA DENDROBII medicinal material is the drying stem of orchid dendrobium nobile (Dendrobium nobile Lindl), has beneficial stomach
Promote the production of body fluid, nourishing Yin and clearing heat the effect of.HERBA DENDROBII contains a variety of composition of alkaloids such as dendrobine, modern research shows that golden hairpin stone
Dry measure used in former times total alkaloid have anti-diabetic, lipidemia, (Huang Qi HERBA DENDROBII total alkaloid is to glycosuria for anti-senile dementia isoreactivity
Protective effect Zunyi Medical College of sick rat model, 2009.；Chen Jing HERBA DENDROBII total alkaloid is to ApoE-/-Mouse hyperlipidemia
With influence Zunyi Medical College of vascular atherosclerosis, 2016.；Jiang Linshan, Li Fei, Nie Jing wait HERBA DENDROBII always biological
Influence Zunyi Medical College journal of the alkali to APP/PS1 transgenic mice ability of learning and memory, 2016,39 (3): 246-249.；Bar
It gets the better of, Cai Rui, Yin Caixia wait HERBA DENDROBII total alkaloid to improve injury of neurons in hippocampus China caused by streptozotocin
New drug and clinical journals, 2017,36 (6): 340-346.), there are also anti-for the main component dendrobine in HERBA DENDROBII total alkaloid
Activity (Li R, Liu T, Liu M, the et al.Anti-influenza A virus activity of of influenza A virus
dendrobine and its mechanism of action[J].Journal of agricultural and food
chemistry,2017,65(18):3665-3674.).As it can be seen that HERBA DENDROBII total alkaloid has well in terms of new drug development
Potentiality.According to " drug registration management method " attachment 1 " Chinese medicine, natural drug registration classification and declaration material requirement " regulation,
5th kind new medicine, active component content should account for 50% of extract or more.Therefore, the extraction of HERBA DENDROBII total alkaloid is developed
Purification process is meaningful.About the method for extraction and purification of dendrobium stem alkali, have some technical solution (CN
101653563 B；CN 101537128 B；CN 108175831 A；101735231 B of CN), but its defect is to use greatly
Organic solvent is measured, high production cost, energy consumption is high；And chloroform is used in the technical solution having and handles (101537128 B of CN；
CN 104557956A；Zhao Fukun, Wu Qin, Lu Yuanfu wait the improvement of the extraction of HERBA DENDROBII total alkaloid and content assaying method
Zunyi Medical College's journal, 2015,38 (5): 532-535.；Alkaloid extracts in Cao Yunli, Pan Zihong, Zhao Xiaojun HERBA DENDROBII
The table mountain dynamic analysis institute journal, 2017,32 (5): 44-49.), defect is that chloroform has larger toxicity, harm life
Produce the very risky of technical staff's body.
Summary of the invention
The present invention is to overcome defect described in the above-mentioned prior art, provides and a kind of is mainly extracted point with aqueous solvent
From, the preparation method of the auxiliary golden hairpin dendrobium extract handled with small amount organic solvent, in obtained extract, Jin Chai
The content of dendrobium total alkaloids reaches 50% or more.
The technical solution of the present invention is as follows:
Using the drying stem of orchid dendrobium nobile (Dendrobium nobile Lindl) as raw material, by the step of following sequences
Suddenly extract is prepared:
(1) HERBA DENDROBII medicinal material is broken into graininess；
(2) feed particulate material is taken, solubilizer impregnates diacolation after 6~12h, collects 10~50 times of amount volumes of raw material weight
Percolate；
The solvent is the aqueous hydrochloric acid solution of the pH 1~4 containing 1%~5% glycine of mass ratio and ammonium acetate mixture,
In glycine and ammonium acetate mixture, the two molar ratio is 1:1~1:3；
(3) taking percolate milk of lime tune pH is 6~7, and upper D101 or AB-8 or similar polar macroporous resin column are first used
The pure water of 3 times of bed volumes is washed, and is discarded water lotion, then eluted with the aqueous hydrochloric acid solution of the pH 1~4 of 3~6 times of bed volumes, is received
Collect eluent A；
(4) eluent A is taken, is neutrality with saturated aqueous sodium carbonate tune pH, is concentrated under reduced pressure as clear cream；
(5) qinghuo reagent is mixed thoroughly with 80 mesh silica gel of equivalent, silica gel column partition chromatography is then carried out, with 3~6 times of bed volumes
Ethyl acetate elution, obtain eluent B；
The Partition Chromatography, supporting agent are 80 mesh silica gel, and stationary phase is that saturated aqueous sodium carbonate (uses ethyl acetate in advance
Saturation), eluant, eluent is ethyl acetate；
(6) eluent B is taken, after recycling design, by recrystallization processing method, with methyl alcohol process 1~3 time；
(7) it learns from else's experience recrystallization treated solid, 60 DEG C of dryings crush to get golden hairpin dendrobium extract.
Preferably, in step (2), 8h is impregnated, collects the percolate of 30 times of amount volumes of raw material weight.
Preferably, in step (2), the solvent is that the hydrochloric acid of the pH 2 containing 3% glycine and ammonium acetate mixture is water-soluble
Liquid, in glycine and ammonium acetate mixture, the two molar ratio is 1:1.
It preferably, is 6.5 with milk of lime tune pH in step (3), upper D101 macroporous resin column, with 4.5 times of bed volumes
The aqueous hydrochloric acid solution of pH 2 elutes.
Preferably, it in step (5), is eluted with the ethyl acetate of 4 times of bed volumes.
Preferably, in step (6), with methyl alcohol process 2 times.
In above-mentioned steps (2), whens seepage pressure effects, can also be aided with microwave or ultrasonic treatment.
In above-mentioned steps (6), methanol can also be changed to ethyl alcohol or ethyl acetate.
Dendrobium stem alkali components are mostly lipophilic, and the present invention is mentioned by sour water and alkaloid at salt
Out；The glycine and ammonium acetate added in a solvent, the two are hydrogen bond donor and hydrogen bond receptor, can make dendrobium stem alkali shape
At hydrogen bond, to reach solubilization-aid effect.The present invention makes dendrobium stem alkali be in salification or dissociate by adjusting pH value
State, to facilitate it to dissolve or be adsorbed.The present invention by macroporous resin column chromatography, washing can remove carbohydrate, amino acids and
The impurity such as protein.The present invention is the silica gel column partition chromatography of saturated aqueous sodium carbonate by stationary phase, can make some phenolic acid
Property impurity enters stationary phase and separates with dendrobium stem alkali.
The amount of organic solvent used in the present invention is far below prior art, and the cost of organic solvent itself is low, Er Qiexu
The link to be heated is few, therefore low energy consumption.
Organic solvent used in the present invention is only alcohols solvent and ethyl acetate, does not use common chloroform processing method,
Therefore endangering production technician's body, there is very little risk.
Macroporous resin column chromatography, silica gel column partition chromatography in the present invention, it is reusable, to can also make production cost
It reduces.
In golden hairpin dendrobium extract of the present invention, the content of total alkaloid up to 50% or more, higher active component content, compared with
Low production cost is outstanding advantage of the invention.
Specific embodiment
By following specific embodiments, present invention be described in more detail, it should be understood that specific implementation described herein
Example for explaining only the invention, is not intended to limit the present invention, and can carry out various change in the range of right of the present invention limits
Become.
Embodiment 1
A kind of golden hairpin dendrobium extract, preparation method are to prepare by the step of following sequences:
(1) HERBA DENDROBII medicinal material 200g is taken, graininess is broken into；
(2) feed particulate material is taken, solubilizer impregnates diacolation after 8h, collects the percolate of 30 times of amount volumes of raw material weight；
The solvent is the aqueous hydrochloric acid solution of the pH 2 containing 3% glycine and ammonium acetate mixture, glycine and ammonium acetate
In mixture, the two molar ratio is 1:1.
(3) taking percolate milk of lime tune pH is 6.5, upper D101 macroporous resin column, first with the pure water of 3 times of bed volumes
It washes, discards water lotion, then eluted with the aqueous hydrochloric acid solution of the pH 2 of 4.5 times of bed volumes, collect eluent A；
(4) eluent A is taken, is neutrality with saturated aqueous sodium carbonate tune pH, is concentrated under reduced pressure as clear cream；
(5) qinghuo reagent is mixed thoroughly with 80 mesh silica gel of equivalent, silica gel column partition chromatography is then carried out, with the second of 4 times of bed volumes
Acetoacetic ester elution, obtains eluent B；
The Partition Chromatography, supporting agent are 80 mesh silica gel, and stationary phase is that saturated aqueous sodium carbonate (uses ethyl acetate in advance
Saturation), eluant, eluent is ethyl acetate.
(6) eluent B is taken, after recycling design, by recrystallization processing method, with methyl alcohol process 2 times；
(7) it learns from else's experience recrystallization treated solid, 60 DEG C of dryings crush to get golden hairpin dendrobium extract.
Embodiment 2
A kind of golden hairpin dendrobium extract, preparation method are to prepare by the step of following sequences:
(1) HERBA DENDROBII medicinal material 200g is taken, graininess is broken into；
(2) feed particulate material is taken, solubilizer impregnates diacolation after 12h, collects the percolate of 50 times of amount volumes of raw material weight；
The solvent is the aqueous hydrochloric acid solution of the pH 1.5 containing 4% glycine and ammonium acetate mixture, glycine and acetic acid
In ammonium mixture, the two molar ratio is 1:1.5.
(3) taking percolate milk of lime tune pH is 7, and upper D101 macroporous resin column is first washed with the pure water of 3 times of bed volumes,
Water lotion is discarded, then is eluted with the aqueous hydrochloric acid solution of the pH 1.5 of 6 times of bed volumes, eluent A is collected；
(4) eluent A is taken, is neutrality with saturated aqueous sodium carbonate tune pH, is concentrated under reduced pressure as clear cream；
(5) qinghuo reagent is mixed thoroughly with 80 mesh silica gel of equivalent, silica gel column partition chromatography is then carried out, with the second of 5 times of bed volumes
Acetoacetic ester elution, obtains eluent B；
The Partition Chromatography, supporting agent are 80 mesh silica gel, and stationary phase is that saturated aqueous sodium carbonate (uses ethyl acetate in advance
Saturation), eluant, eluent is ethyl acetate.
Subsequent processing is the same as embodiment 1.
Comparative example 1
Compared with Example 1, difference is only that: in step (2), solvent is the aqueous hydrochloric acid solution of pH 2, is not added with sweet ammonia
Acid and ammonium acetate.
Comparative example 2
Compared with Example 1, difference is only that: in step (3), take percolate milk of lime tune pH be 6.5 after, without
Macroporous resin column chromatography jumps directly to step (4) " being concentrated under reduced pressure is clear cream ".
Comparative example 3
Compared with Example 1, difference is only that: not being included step (5), " clear cream " of step (4) jumps directly to step (6)
" by recrystallization processing method ".
Comparative example 4
Compared with Example 1, difference is only that: in step (6), after recycling design, jumping directly to step (7), " 60 DEG C dry
Dry, crushing ".
Embodiment is shown in Table 1 compared with the extract obtained yield of comparative example, total alkaloid content.
Weight percent of the yield by extract and throwing raw material.
The content assaying method of the total alkaloid: (Shi Dongjun, Yang Wenyu, Tang Sheng wait gold hairpin stone to reference literature method
Dry measure used in former times decoct cook paste during the variation of polysaccharide and total alkaloid content when treasure's traditional Chinese medical science traditional Chinese medicines, 2016,27 (2): 355-358.) survey
It is fixed.
1 total alkaloid content test result table of table
| Extract sample | HERBA DENDROBII medicinal material weight | Extract weight | Yield | Total alkaloid content |
| Embodiment 1 | 200g | 1.2653g | 0.63% | 76.7% |
| Embodiment 2 | 200g | 1.2047g | 0.60% | 72.18% |
| Comparative example 1 | 200g | 1.0878g | 0.54% | 76.36% |
| Comparative example 2 | 200g | 2.5145g | 1.26% | 35.85% |
| Comparative example 3 | 200g | 1.8416g | 0.92% | 46.54% |
| Comparative example 4 | 200g | 1.4275g | 0.71% | 58.61% |
Embodiment 1 compared with embodiment 2 it is found that when technological parameter changes on the basis of preferred parameter, extract yield,
Total alkaloid content can be reduced slightly.Comparative example 1~4 is compared with embodiment 1 it is found that adding glycine and acetic acid in Extraction solvent
Ammonium mixture, macroporous resin column chromatography, silica gel column partition chromatography, 4 kinds of recrystallization operation processing, to the receipts of golden hairpin dendrobium extract
Rate/total alkaloid content has certain beneficial effect.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (3)
1. a kind of preparation method of golden hairpin dendrobium extract, which comprises the following steps:
(1) it is raw material by the dry stem of HERBA DENDROBII, is broken into graininess；
(2) feed particulate material is taken, solubilizer impregnates diacolation after 6~12h, collects the diacolation of 10~50 times of amount volumes of raw material weight
Liquid；
(3) taking percolate milk of lime tune pH is 6~7, and upper macroporous resin column is first washed with the pure water of 3 times of bed volumes, discards water
Washing lotion, then eluted with the aqueous hydrochloric acid solution of the pH 1~4 of 3~6 times of bed volumes, collect eluent A；
(4) eluent A is taken, is neutrality with saturated aqueous sodium carbonate tune pH, is concentrated under reduced pressure as clear cream；
(5) qinghuo reagent is mixed thoroughly with 80 mesh silica gel of equivalent, silica gel column partition chromatography is then carried out, with the second of 3~6 times of bed volumes
Acetoacetic ester elution, obtains eluent B；
The Partition Chromatography, supporting agent are 80 mesh silica gel, and stationary phase is saturated aqueous sodium carbonate, full with ethyl acetate in advance
With eluant, eluent is ethyl acetate；
(6) it takes eluent B, after recycling design, by recrystallization processing method, is handled 1~3 time with methanol, ethyl alcohol or ethyl acetate；
(7) it learns from else's experience recrystallization treated solid, 60 DEG C of dryings crush to get golden hairpin dendrobium extract.
2. a kind of preparation method of golden hairpin dendrobium extract according to claim 1, which is characterized in that step (2) is described
Solvent is the aqueous hydrochloric acid solution of the pH 1~4 containing 1%~5% glycine of mass ratio and ammonium acetate mixture, glycine and acetic acid
In ammonium mixture, the two molar ratio is 1:1~1:3.
3. a kind of golden hairpin dendrobium extract, which is characterized in that prepare gained by the preparation method of claims 1 or 2.
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