CN107296825A - A kind of skin is trembled with fear medicine medicinal extract or its pharmaceutical composition and preparation method thereof - Google Patents
A kind of skin is trembled with fear medicine medicinal extract or its pharmaceutical composition and preparation method thereof Download PDFInfo
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- CN107296825A CN107296825A CN201710744224.7A CN201710744224A CN107296825A CN 107296825 A CN107296825 A CN 107296825A CN 201710744224 A CN201710744224 A CN 201710744224A CN 107296825 A CN107296825 A CN 107296825A
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- skin
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- gueldenstaedtia
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- 239000000284 extract Substances 0.000 title claims abstract description 63
- 239000003814 drug Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000008194 pharmaceutical composition Substances 0.000 title description 2
- HUKSJTUUSUGIDC-ZBEGNZNMSA-N (-)-maackiain Chemical compound O1C2=CC=3OCOC=3C=C2[C@H]2[C@@H]1C1=CC=C(O)C=C1OC2 HUKSJTUUSUGIDC-ZBEGNZNMSA-N 0.000 claims abstract description 68
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000000463 material Substances 0.000 claims abstract description 48
- 229940124579 cold medicine Drugs 0.000 claims abstract description 43
- XCDMHEXDCIXKLK-UHFFFAOYSA-N Anhydrosophorol Natural products O1C2=CC=3OCOC=3C=C2C2=C1C1=CC=C(O)C=C1OC2 XCDMHEXDCIXKLK-UHFFFAOYSA-N 0.000 claims abstract description 34
- YLZYAUCOYZKLMA-UHFFFAOYSA-N O-Methyl-maackiain Natural products O1C2=CC=3OCOC=3C=C2C2C1C1=CC=C(OC)C=C1OC2 YLZYAUCOYZKLMA-UHFFFAOYSA-N 0.000 claims abstract description 34
- HUKSJTUUSUGIDC-UHFFFAOYSA-N Trifolirhizin-aglykon Natural products O1C2=CC=3OCOC=3C=C2C2C1C1=CC=C(O)C=C1OC2 HUKSJTUUSUGIDC-UHFFFAOYSA-N 0.000 claims abstract description 34
- CNHOGQMRRDHYGI-NJCGARBWSA-N beta-onocerin Chemical compound C([C@@]12C)C[C@H](O)C(C)(C)[C@@H]1CCC(C)=C2CCC1=C(C)CC[C@@H]2[C@]1(C)CC[C@H](O)C2(C)C CNHOGQMRRDHYGI-NJCGARBWSA-N 0.000 claims abstract description 34
- 241000505726 Gueldenstaedtia Species 0.000 claims abstract description 23
- 239000008187 granular material Substances 0.000 claims abstract description 21
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 239000006228 supernatant Substances 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 239000012141 concentrate Substances 0.000 claims abstract 4
- 238000000034 method Methods 0.000 claims description 46
- 239000002245 particle Substances 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 206010044565 Tremor Diseases 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 241000123871 Gueldenstaedtia verna Species 0.000 claims description 9
- 229920001353 Dextrin Polymers 0.000 claims description 8
- 239000004375 Dextrin Substances 0.000 claims description 8
- 235000019425 dextrin Nutrition 0.000 claims description 8
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
- 229920002472 Starch Polymers 0.000 claims description 6
- 239000008107 starch Substances 0.000 claims description 6
- 235000019698 starch Nutrition 0.000 claims description 6
- 241001529246 Platymiscium Species 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 230000008719 thickening Effects 0.000 claims description 4
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims 1
- 244000046052 Phaseolus vulgaris Species 0.000 claims 1
- 230000000202 analgesic effect Effects 0.000 claims 1
- 239000002574 poison Substances 0.000 claims 1
- 231100000614 poison Toxicity 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 8
- 230000036592 analgesia Effects 0.000 abstract description 3
- 229940079593 drug Drugs 0.000 abstract description 3
- 239000013618 particulate matter Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 17
- 239000000843 powder Substances 0.000 description 16
- 239000013558 reference substance Substances 0.000 description 16
- 238000001556 precipitation Methods 0.000 description 11
- 238000002844 melting Methods 0.000 description 10
- 230000008018 melting Effects 0.000 description 10
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 9
- 230000006837 decompression Effects 0.000 description 8
- 239000000080 wetting agent Substances 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- 239000011122 softwood Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000005469 granulation Methods 0.000 description 6
- 230000003179 granulation Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- 244000046101 Sophora japonica Species 0.000 description 5
- 235000010586 Sophora japonica Nutrition 0.000 description 5
- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 238000002955 isolation Methods 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 239000004480 active ingredient Substances 0.000 description 3
- 239000006286 aqueous extract Substances 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 241000411851 herbal medicine Species 0.000 description 3
- 238000003809 water extraction Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 206010022000 influenza Diseases 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 235000021251 pulses Nutrition 0.000 description 2
- 238000005464 sample preparation method Methods 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- 241001517368 Coelogyne Species 0.000 description 1
- 108010023832 Florigen Proteins 0.000 description 1
- 235000007171 Ononis arvensis Nutrition 0.000 description 1
- 240000002598 Ononis spinosa Species 0.000 description 1
- 235000016054 Ononis spinosa subsp spinosa Nutrition 0.000 description 1
- 208000037386 Typhoid Diseases 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000000469 ethanolic extract Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000001261 florigenic effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 235000021374 legumes Nutrition 0.000 description 1
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- 238000005453 pelletization Methods 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 239000000651 prodrug Substances 0.000 description 1
- 229940002612 prodrug Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 201000008297 typhoid fever Diseases 0.000 description 1
- 241000712461 unidentified influenza virus Species 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/485—Gueldenstaedtia
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1617—Organic compounds, e.g. phospholipids, fats
- A61K9/1623—Sugars or sugar alcohols, e.g. lactose; Derivatives thereof; Homeopathic globules
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
- A61K9/1605—Excipients; Inactive ingredients
- A61K9/1629—Organic macromolecular compounds
- A61K9/1652—Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
-
- 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
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
-
- 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
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Chemical & Material Sciences (AREA)
- Epidemiology (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Pharmacology & Pharmacy (AREA)
- Alternative & Traditional Medicine (AREA)
- Mycology (AREA)
- Microbiology (AREA)
- Medical Informatics (AREA)
- Botany (AREA)
- Biotechnology (AREA)
- Biophysics (AREA)
- Molecular Biology (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
It is specific as follows the invention provides a kind of herba gueldenstaedtia extract and preparation method thereof：1) the cold medicine medicinal material of skin is taken, is smashed, 12 times of decoctings is added and boils 0.5, decoct as 2 times, filter, merging filtrate；Take step 1) gained filtrate, concentrate, add 50 70%V/V ethanol, precipitate 6 18h, take supernatant, concentrate, obtain extract.Wherein, maackiain content is 0.1978 0.2501mg/g in extract, and onocerin content is 0.2127 0.2958mg/g.It is specific as follows present invention also offers cold medicine granule of a kind of skin and preparation method thereof：Said extracted thing is taken, it is 15 to add with extract weight proportioning:1 auxiliary material and 55 95% ethanol, are stirred, and are dried, are produced.Prepared present invention also offers a kind of cold medicine particulate matter of skin with the purposes in the medicines such as clearing heat and detoxicating, analgesia.
Description
Technical field
The present invention relates to a kind of pharmaceutical preparation and preparation method thereof, and in particular to cold medicine preparation of skin and preparation method thereof.
Background technology
The cold medicine of skin is the dry of pulse family Gueldenstaedtia verna platymiscium river Yunnan Gueldenstaedtia verna Gueldenstaedtia delavayi Franch
Dry herb, conventional characteristic traditional herbal medicine, different name skin typhoid fever, Flaccid Coelogyne when being Panxi Area, Sichuan Province Anninghe Watershed treatment flu
Deng.《Xichang Chinese herbal medicine》Name is said:" skin tremble with fear medicine ", is Papilionaceae Gueldenstaedtia verna platymiscium, and the whole herb with root of health Yunnan Gueldenstaedtia verna is recorded
Its:" all herbal medicine, the four seasons can adopt；It is cold in nature, pungent hardship, clearing heat and detoxicating, analgesia ".
At present, existing patent report herba gueldenstaedtia extract and application thereof, as CN102641323A disclose skin tremble with fear medicine or
Purposes of its water extract in the medicine or health products of resisiting influenza virus is prepared, but it only trembles with fear to skin, medicine has been carried out simply
Abstract methods are not screened by water extraction, therefore can not be learnt and carried out water extraction under what conditions, can extract skin liquid medicine of trembling with fear
The amount of thing reaches maximum；CN102641324A discloses cold medicine ethanol extract of skin and application thereof, but it is not to alcohol extracting bar
Part is screened, therefore can not also be learnt and carried out alcohol extracting under what conditions, and the tremble with fear amount of medicine alcohol extracting thing of skin can be made to reach maximum.
Document《Zhao Furong Panxi Diqu characteristic resources skin is trembled with fear medicine matter evaluation study [D] Chengdu University of Traditional Chinese Medicines, 2012》Disclose
By medicine Extraction solvent, extracting method and the screening of extraction time of being trembled with fear to skin, the higher onocerin of content and Koryo are obtained
Chinese scholartree cellulose content, but the content of its gained maackiain is only 0.02925mg/g.
Therefore, it is badly in need of a kind of herba gueldenstaedtia extract that can extract high content active ingredient especially maackiain now
Method.
The content of the invention
In order to solve the above problems, the invention provides a kind of herba gueldenstaedtia extract or its granule and preparation method thereof.
The invention provides a kind of herba gueldenstaedtia extract, it is to be prepared from by the following method：
1) the cold medicine medicinal material of skin is taken, is smashed, 8-12 times of decocting is added and boils 0.5-1.5h, decoct as 1-3 times, filter, merge and filter
Liquid；
2) step 1 is taken) gained filtrate, relative density 1.10 is concentrated into, 50-70%V/V ethanol is added, 6-18h is precipitated, takes
Supernatant, it is 1.23 ± 0.03 to be concentrated into relative density, produces extract.
Further, above-mentioned steps 1) in, the amount of water is 12 times of the cold medicine medicinal material of skin, and decocting time is 0.5h, is decocted
Number of times is boiled for 2 times；
Above-mentioned steps 2) in, the thickening temperature is 70 DEG C, and concentration of alcohol is 60%V/V, and the sedimentation time is 18h.
Further, maackiain content is 0.1978-0.2501mg/g in above-mentioned herba gueldenstaedtia extract, and onocerin contains
Measure as 0.2127-0.2958mg/g.
Further, described skin trembles with fear medicine from pulse family Gueldenstaedtia verna platymiscium river Yunnan Gueldenstaedtia verna Gueldenstaedtia
Delavayi Franch drying herb.
Present invention also offers a kind of cold medicine granule of skin, it is to be prepared from by the following method：The cold medicine of above-mentioned skin is taken to carry
Thing is taken, the weight proportion added with extract is 1-5:1 auxiliary material, 55-95%V/V ethanol is stirred, and is dried, is produced.
Further, the weight proportion of the auxiliary material and extract is 4:1；Concentration of alcohol is 75%V/V；Auxiliary material is paste
One kind in essence, DEXTROSE ANHYDROUS, soluble starch.
The invention provides a kind of method for preparing herba gueldenstaedtia extract, comprise the following steps：
1) the cold medicine medicinal material of skin is taken, is smashed, 8-12 times of decocting is added and boils 0.5-1.5h, decoct as 1-3 times, filter, merge and filter
Liquid；
2) step 1 is taken) gained filtrate, relative density 1.10 is concentrated into, 50-70%V/V ethanol is added, 6-18h is precipitated, takes
Supernatant, it is 1.23 ± 0.03 to be concentrated into relative density, produces medicinal extract.
Further, the step 1) in, the amount of water is 12 times of the cold medicine medicinal material of skin, and decocting time is 0.5h, is decocted
Number of times is boiled for 2 times；
Further, the step 2) in, the thickening temperature is 70 DEG C, and concentration of alcohol is 60%V/V, and the sedimentation time is
18h。
The invention provides a kind of method for preparing herba gueldenstaedtia extract, comprise the following steps：
Above-mentioned herba gueldenstaedtia extract is taken, the weight proportion added with extract is 1-5:1 auxiliary material, 55-95%V/V second
Alcohol, is stirred, and is dried, is produced.
Further, the weight proportion of the auxiliary material and extract is 4:1；Concentration of alcohol is 75%V/V；Auxiliary material is paste
One kind in essence, DEXTROSE ANHYDROUS, soluble starch.
Prepared the invention provides a kind of cold medicine particle of above-mentioned skin with the purposes in the medicines such as clearing heat and detoxicating, analgesia.
Obviously, according to the above of the present invention, according to the ordinary technical knowledge and customary means of this area, do not departing from
Under the premise of the above-mentioned basic fundamental thought of the present invention, the modification of other diversified forms can also be made, replaces or changes.
The embodiment of form, remakes further specifically to the above of the invention by the following examples
It is bright.But the scope that this should not be interpreted as to above-mentioned theme of the invention is only limitted to following example.It is all to be based on the above of the present invention
The technology realized belongs to the scope of the present invention.
Embodiment
The raw material that is used in the specific embodiment of the invention, equipment are known product, are obtained by buying commercially available prod.
Instrument：High performance liquid chromatograph (Agilent companies, model：Technologies1260)；Air dry oven (north
Jing Zhongxing great achievements Instrument Ltd.)；Electronic balance (Beijing Sai Duolisi balances Co., Ltd, model：BS200S)；Electronic constant
Warm water bath (Beijing Zhong Xing great achievements Instrument Ltd., model：DZKW-4)；Microphyte sample pulverizer (Xing Wei in Beijing
Industry Instrument Ltd., model：FZ102)；Regulating temperature electrothermal cover (Hebei province Huanghua City Zhong Xing Instrument Ltd., model：
ZDHW)；And other glass apparatus, screen cloth etc..
Reagent：The cold medicine of skin picks up from Liangshan, Sichuan Xichang City Li Zhou towns, is identified through Chengdu University of Traditional Chinese Medicine professor Jiang Guihua
For legume river Yunnan Gueldenstaedtia verna Gueldenstaedtia delavayi Franch. drying herb；Maackiain reference substance
(Chengdu Man Site bio tech ltd, Chengdu Inst. of Biology, Chinese Academy of Sciences, lot number：MUST-15071610), awns handle
Florigen reference substance (Chengdu Man Site bio tech ltd, Chengdu Inst. of Biology, Chinese Academy of Sciences, lot number：MUST-
16031005), DEXTROSE ANHYDROUS (the pure AR Chengdu Ke Long chemical reagents factory of analysis).
The preparation of embodiment 1, herba gueldenstaedtia extract of the present invention
Take the skin after immersion 40min to tremble with fear medicine medicinal material 1000g, crush as coarse powder, add water to cook secondary, add water every time 12 times,
0.5h is decocted every time, and decocting liquid filtration, filtrate merges, and is concentrated into relative density 1.10 (70 DEG C), plus ethanol makes alcohol content up to 60%,
18h is staticly settled, supernatant is taken, ethanol is reclaimed and is concentrated into relative density for 1.20-1.25 (70 DEG C), produce extract.
Embodiment 2, the craft screening for preparing herba gueldenstaedtia extract
1st, the cold medicine medicine materical crude slice absorbent time of skin and water absorption rate
Skin trembles with fear medicine after soak time is more than 40min, and water absorption rate change is no longer obvious, and now the water absorption of medicinal material reaches
The 127.8% of medicinal material weight.Therefore, extracted after medicinal material is soaked into 40min before testing.
2nd, maackiain, the HPLC of awns handle Chinese scholartree element are determined in the cold liquid medicine extract of skin
(1) preparation of standard liquid
Maackiain reference substance is taken, accurately weighed, methanol dissolving is settled to 10ml, 1.002mg/ml maackiains are made
Reference substance storing solution.Dilute 5 times of 1ml1.002mg/ml maackiains are taken again.For 0.2004mg/ml.Make standard curve.
Onocerin reference substance is taken, accurately weighed, methanol dissolving is settled to 10ml, 0.999mg/ml onocerins are made
Reference substance storing solution.Take 1ml 0.999mg/ml onocerin reference substances storing solution to dilute 10 times again, be 0.0999mg/ml.System
Make standard curve.
(2) chromatographic condition
Chromatographic column：DiamonsilTMC18HPLC chromatogram post (4.6 × 250mm, 5ul, Ser.No.:8132964.) flowing
Phase：Acetonitrile-water (40:60), flow velocity：1.0mL/min, column temperature：30 DEG C, sample size：10 μ l, Detection wavelength：210nm, during analysis
Between：25min.
(3) drafting of standard curve
Maackiain standard curve：It is accurate respectively to draw the μ l of maackiain reference substance solution 2,4 μ l, 8 μ l, 12 μ l, 16 μ l,
Analyzed according to above-mentioned chromatographic condition.Using peak area as ordinate, the sample size of maackiain is abscissa, draws recurrence side
Journey.Analyze calibration curve equation is：Y=718.91x-34.353, R2=0.9992.It is high between 0.4008-3.2060 μ g
The peak area of beautiful Chinese scholartree element and sample size are in good linear relationship.
Onocerin standard curve：It is accurate respectively to draw the μ l of onocerin reference substance solution 2,4 μ l, 10 μ l, 12 μ l, 16 μ
L, is analyzed according to above-mentioned chromatographic condition.Using peak area as ordinate, the sample size of onocerin is abscissa, draws and returns
Equation.Analyze calibration curve equation is：Y=705.19x-16.675, R2=0.9993.Between 0.1998-1.9980 μ g
The peak area of onocerin is in good linear relationship with sample size.
(4) precision is investigated
Onocerin reference substance solution (0.999mg/ml) 10 μ l continuous sample introductions are drawn respectively 5 times；Koryo Chinese scholartree is drawn respectively
Plain 10 μ l continuous sample introductions of reference substance solution (1.002mg/ml) 5 times.Measure onocerin RSD=0.64%, maackiain RSD=
0.68%, show that this method precision is good.
(5) sample stability is investigated
Skin is taken to tremble with fear medicine medicinal material coarse powder about 10g, it is accurately weighed, handled by sample preparation methods, produce need testing solution.
Determined once in 0h, 2h, 4h, 8h, 12h, 24h respectively.Result is investigated to show：Onocerin RSD=2.15%, maackiain
RSD=3.07%.Test sample place 12 hours in, onocerin, maackiain content it is basicly stable, extension over time
It can decline, therefore test sample is preferably detected within 8 hours.
(6) reference substance study on the stability
Precision draws onocerin reference substance solution (0.0999mg/ml) 10 μ l, respectively at 0h, 2h, 4h, 8h, 12h, 24h
Determine once；Precision draws maackiain reference substance solution (1.002mg/ml) 10 μ l, respectively at 0h, 2h, 4h, 8h, 12h, 24h
Determine once.Measure onocerin RSD=1.02%, maackiain RSD=1.09%.Reference substance solution maackiain stability
Start to have declined after 8 hours to be detected, onocerin change is little, therefore test sample is preferably examined within 8 hours
Survey.
(7) reappearance test is investigated
Taking skin to tremble with fear, medicinal material coarse powder is parallel 5 parts, and every part of 10g is accurately weighed, is handled according to sample preparation methods, obtains for examination
Product part.According to sample assay method, peak area is measured, onocerin, the content of maackiain is calculated.Measure onocerin
RSD=1.23%, maackiain RSD=2.81%.The content that this method measures onocerin and maackiain in sample is reappeared
Property is good.
(8) average recovery is investigated
Using average recovery method, the onocerin that the cold medicine medicinal material coarse powder of skin is measured as stated above contains with maackiain
Amount.Precision adds the onocerin and maackiain reference substance with coarse powder content equivalent.Operated by sample assay method, measure sample
The content of onocerin, maackiain in product, calculates the rate of recovery.Rate of recovery %=[contents in measured amount (mg)-medicinal material
(mg)]/onocerin or maackiain addition * 100%.Measure onocerin average recovery rate=100.14%, RSD=
1.46%, maackiain average recovery rate=100.27%, RSD=1.72%.Therefore this method maackiain, onocerin are reclaimed
Rate is good.
3rd, the cold medicine extraction process by water of skin
(1) the cold liquid medicine of skin carries technological experiment
The cold medicine medicinal material 270g of skin is taken, 9 parts are divided into.With dried cream yield in Aqueous extracts, water-soluble extractives maackiain
Content, onocerin content are index, using HPLC detection methods, with the multiple that adds water (A), extraction time (B), extraction time h
(C), 4 factors of granularity (D), each factor takes 3 levels, tested, and understands that it is coarse powder to work as process conditions by experimental result,
Add water 12 times, extract 2 times, when extracting 30min every time, dried cream yield in gained Aqueous extracts, water-soluble extractives maackiain contains
Amount, onocerin content are higher, and table 1 is the repeated the result to optimal extraction process by water.
The optimal extraction process by water experimental result of the cold medicine of the skin of table 1
As seen from Table 1：Using coarse powder, plus 12 times of water, extract 2 times, 30min reappearances are extracted every time good.So water extraction
It is stable process conditions, controllable.
4th, isolation and purification technical study
(1) isolation and purification method is investigated
The cold medicine coarse powder 80g of skin is taken, 4 parts are divided into.The cold medicine sample of skin is prepared by above selection process.Investigate conventional separation
The active constituent content of purification process (centrifugation, filtering, alcohol precipitation), selects rational isolation and purification method.It the results are shown in Table 2.
The cold liquid medicine of the skin of table 2 carries decoction purification process and investigates result
| Sample ID | Maackiain content mg/g (X1) | Onocerin content mg/g (X2) | Overall merit (Y) |
| Stoste | 0.3001 | 0.3156 | 94.3 |
| Centrifugate | 0.2594 | 0.3038 | 85.9 |
| 60% precipitation solution | 0.3002 | 0.3560 | 100 |
| Filtered fluid | 0.1680 | 0.2103 | 57.5 |
Note：Overall merit formula：Y=50* (X1/X1max)+50* (X2/X2max)
As shown in Table 2：After three of the above is often handled with isolation and purification method, it is according to overall merit active constituent content
60% precipitation solution>Filtered fluid>Stoste>Centrifugate.And decoction is more sticky, filter more intractable.Therefore herba gueldenstaedtia extract is pure
Change method selection alcohol deposition method.
(2) the cold medicine alcohol precipitation process experiment of skin
The cold medicine medicinal material 270g of skin is taken, 9 parts are divided into.The cold medicine sample of skin is prepared by above selection process.With water solubility leaching
Go out thing maackiain content, onocerin content for index, using HPLC detection methods, with relative density of medicine liquid (A), alcohol precipitation concentration
(B), 3 factors of alcohol precipitation time h (C), each factor takes 3 levels, tested, and understands to work as alcohol precipitation process bar by experimental result
Part is relative density 1.10, alcohol precipitation concentration 60%, pure heavy time 18h, and water-soluble extractives maackiain contains in gained Aqueous extracts
Amount, onocerin content are higher, and table 3 is the repeated the result to optimal alcohol precipitation process.
The optimal alcohol precipitation process experimental result of the cold medicine of the skin of table 3
As a result show：Using the decoction of relative density 1.10, plus 60% ethanol, alcohol precipitation 18h, reappearance is good.So alcohol
It is heavy stable process conditions, controllable.The medicine Preparation Technology of Granules that can be trembled with fear for skin provides reference.
5th, concentration technology is studied
This experiment is main to different temperatures, the lower different temperatures of decompression under normal pressure, and different pressures are carried out under same temperature
Investigate.The cold medicine coarse powder 100g of skin is taken, the scheme preferably gone out more than is extracted, decoction will be obtained and be divided into 5 parts, respectively
Concentrated at 100 DEG C of normal pressure, 80 DEG C of normal pressure, 80 DEG C of decompression, 70 DEG C of decompression, 60 DEG C of decompression.With water-soluble extractives Koryo
Chinese scholartree cellulose content, onocerin content are index, are determined using HPLC methods.Experimental result is shown in Table 4.
The cold medicine granule method for concentration of the skin of table 4 investigates result
| Method for concentration | Maackiain content mg/g (X1) | Onocerin content mg/g (X2) | Overall merit (Y) |
| 100 DEG C of normal pressure | 0.2198 | 0.2431 | 85.0 |
| 80 DEG C of normal pressure | 0.2443 | 0.2507 | 91.2 |
| 80 DEG C of decompression | 0.2417 | 0.2958 | 98.4 |
| 70 DEG C of decompression | 0.2501 | 0.2943 | 99.8 |
| 60 DEG C of decompression | 0.1978 | 0.2127 | 75.5 |
Note：Overall merit formula：Y=50* (X1/X1max)+50* (X2/X2max)
As shown in table 4：When depressurizing 70 DEG C, maackiain, onocerin content highest.And the method for being concentrated under reduced pressure has speed
It hurry up, active ingredient influences small advantage, therefore this experiment is concentrated using 70 DEG C of decompression.
As a result show：The present invention obtains maackiain content and rest-harrow by screening herba gueldenstaedtia extract preparation technology
Cellulose content higher herba gueldenstaedtia extract, for extract the herba gueldenstaedtia extract of high content active ingredient provide one it is excellent
Method.
The preparation of the cold medicine granule of embodiment 3, skin of the present invention
The gained herba gueldenstaedtia extract of Example 1, adds DEXTROSE ANHYDROUS, and auxiliary material and extract ratio are 4:1, plus 75%
Ethanol is that wetting agent is appropriate, and particle is made, and in temperature 60 C, drying time 2h, it is 1000g that particle, which is made,.
Embodiment 4, the craft screening for preparing the cold medicine granule of skin of the present invention
1st, the cold medicine granule granulating process research method of skin
(1) the evaluation index comprehensive grading rule of the cold medicine granule of skin
This experiment uses unitary variant method, in governance process, observes and records softwood, particle situation.Meanwhile, with particle
Ratio of briquetting, hydroscopicity, melting are evaluation index comprehensive grading.Comprehensive grading=ratio of briquetting * 50+ (1- hydroscopicities) * 25+ dissolve
Property * 25, preferably goes out optimised process.
(2) measure of ratio of briquetting
The cold medicine granule of obtained skin is crossed into a sieve (200 μm) and No. five sieves (180 μm) respectively, weighed.It is required that obstructed
Cross No. one and sieve 15% must not exceed with the summations that can cross No. five sieves for the amount of showing.3 repeated experiments.A ratio of briquetting=sieve can be crossed
But but No. five sieve granular mass/sieving before granular mass * 100%.
(3) melting inspection
Accurately weighed prescription particulate samples 0.5g obtained in proportion is added into the 10ml centrifuge tubes of constant weight in drying,
Precision adds 10ml boiling water, is sufficiently stirred for vibrating 5min, 3000rmin-1, centrifuges 15min, abandoning supernatant will at 80 DEG C
Residue is dried to constant weight, accurately weighed, and rate is dissolved in calculating.Dissolve rate=dissolve particle weight/total particle weight
(4) measure of hydroscopicity
The drier room temperature that bottom is filled into sodium chloride supersaturated solution places 48h and reaches balance, and relative humidity is
75%.Sample particle 2g is weighed, is laid in the measuring cup after constant weight, measuring cup lid is opened and is put into drier, after 24h
Taking-up is weighed, and calculates hydroscopicity.Medicinal powder quality * after hydroscopicity=(medicinal powder quality-moisture absorption prodrug silty amount after moisture absorption)/moisture absorption
100%.
2nd, the selection of supplementary product kind
Take 3 parts of embodiments 1 extract obtained, every part of 30g, by extract and auxiliary material 1:4 weight is used with well mixed
85% ethanol is pelletized for wetting agent, adds the appropriate of wetting agent.Granulation, dries 2h in 60 DEG C of drying boxes.Particle situation is observed,
It is preferred that optimal auxiliary material.It the results are shown in Table 5.
The cold medicine granule supplementary product kind of the skin of table 5 investigates result
| Auxiliary material | Particle situation | Ratio of briquetting (%) | Hydroscopicity (%) | Melting (%) | Overall merit |
| Dextrin | Fine powder is more | 91.63 | 0.07 | 61.78 | 88.31 |
| DEXTROSE ANHYDROUS | Particle is moderate | 92.13 | 1.46 | 97.71 | 96.73 |
| Soluble starch | Fine powder is more | 83.67 | 4.25 | 47.46 | 80.66 |
Table 5 is investigated result and shown：The cohesive force of dextrin is substantially inadequate, softwood do, dry after particle turn white, and fine powder compared with
It is many, add water and wash rear solution muddiness open, wadding collection forms white precipitate at cup bottom after a period of time.With particle made from soluble starch
Same fine powder is more, and melting is not good, and expensive.Strong, the obtained particle with softwood cohesive force made from DEXTROSE ANHYDROUS
Granularity is moderate, and particle is clearly demarcated, and without excessive fine powder, golden yellow color adds water and washes solution clear open.Therefore use anhydrous grape
Sugar is auxiliary material, and the hydroscopicity of dextrin is preferable, it is considered to which dextrin and DEXTROSE ANHYDROUS are mixed into mixed accessories according to a certain percentage.
3rd, the investigation of ratio of adjuvant
Take 50g embodiments 1 extract obtained, mixed respectively with the mixed accessories of different proportion, matched between mixed accessories
For dextrin：DEXTROSE ANHYDROUS 1:1,1:2,1:3,1:4,1:5, compare 1 with auxiliary material and extract:4,85% ethanol wet agent is added,
Granulation.2h is dried in 60 DEG C of drying boxes.Particle situation is observed, preferably optimal mixed accessories proportioning.It the results are shown in Table 6.
The cold medicine granule ratio of adjuvant of the skin of table 6 investigates result
| Dextrin：Powdered glucose | Particle situation | Ratio of briquetting | Melting | Hydroscopicity | Overall merit |
| 1：1 | Granule fines are more | 90.1 | 52.00 | 3.43 | 83.81 |
| 1：2 | Granule fines are more | 98.1 | 75.52 | 1.9 | 92.46 |
| 1：3 | Granule fines are more | 98.4 | 79.71 | 2.42 | 93.32 |
| 1：4 | Particle is moderate | 97.3 | 89.53 | 2.45 | 95.48 |
| 1：5 | Particle is moderate | 94.6 | 89.20 | 2.88 | 94.51 |
Table 6 is investigated result and shown：Particle is prepared with mixed accessories, the overall melting of particle is all not so good, and particle melts
Afterwards, solution has slight muddiness, and cup bottom has white precipitate after a period of time.The problem of in view of melting, so to paste
The auxiliary material that essence and glucose are mixed is infeasible, uses the single auxiliary material of glucose instead and prepares particle.
4th, the selection of single auxiliary material and extract ratio
According to the preferred result of auxiliary material, take 5 parts of embodiments 1 extract obtained, every part of 10g distinguishes extract and auxiliary material
By 1:1,1:2,1:3,1:4,1:5 different proportion mixing granulations, add 85% ethanol wet agent, granulation.In 60 DEG C of drying boxes
Dry 2h.Observe particle situation, preferably optimal auxiliary material and extract ratio.It the results are shown in Table 7.
The cold medicine granule auxiliary material of the skin of table 7 investigates result with extract proportioning
Result is investigated to show：Extract is 1 with auxiliary material proportion:1,1:Softwood is excessively dilute when 2, and 1:It can be pelletized when 3, but mouldability
It is not good.1:Obtained softwood meets " hand pinches agglomerating, and flicking is to dissipate " when 4.1:Softwood is more dry made from 5, and partial particulate is through drying
After cohere it is blocking.Extract and auxiliary material 1:4 comprehensive scores are matched higher than other, therefore with extract and auxiliary material 1:4 granulations.
5th, concentration of wetting agent and consumption are investigated
According to above-mentioned experimental result, take 50g embodiments 1 extract obtained, extract and DEXTROSE ANHYDROUS are pressed 1:4 ratios
Mixing, is divided into 5 equal portions, respectively using 55%, 65%, 75%, 85%, 95% ethanol as wetting agent, granulation.In 60 DEG C of drying boxes
Middle dry 2h.Observe particle situation, preferably suitable concentration of wetting agent.It the results are shown in Table 8.
The cold medicine granule concentration of wetting agent of the skin of table 8 investigates result
| Concentration | Particle situation | Ratio of briquetting (%) | Hydroscopicity (%) | Melting (%) | Overall merit |
| 55% | Particle is more loose | 97.6. | 1.36 | 97.3 | 98.05 |
| 65% | Particle is more loose | 95.9 | 1.13 | 98.8 | 98.09 |
| 75% | Particle is moderate | 97.5 | 0.95 | 99.0 | 98.65 |
| 85% | Particle is slightly bonded | 98.2 | 1.30 | 98.7 | 98.58 |
| 95% | Particle is slightly bonded | 99.1 | 1.68 | 98.7 | 98.61 |
Result is investigated to show：According to the ratio of briquetting of particle, hydroscopicity, melting, it is believed that 75% ethanol is suitable profit
Humectant concentration.The consumption of wetting agent then should be depending on the situation according to softwood in pelletization.
6th, granulating process is verified
In order to verify the accuracy of above-mentioned experiment, to ensure the reasonable of moulding process, with the optimal shaping preferably gone out
Technique, arranges 3 groups to repeat to test.
The cold medicine Preparation Technology of Granules checking of the skin of table 9
As a result show：The grain forming rate that optimal granulating process according to preferably going out is prepared, hydroscopicity, melting, water
The indices that grade are qualified, and repeatability is good, and granulating process is feasible, stably and controllable.
To sum up, present invention preparation herba gueldenstaedtia extract and its stable process conditions of particulate matter, controllable, recovery rate are high, can
The Chinese medicine preparation for preventing and treating influenza for exploitation further studies offer reference.
Claims (11)
1. a kind of herba gueldenstaedtia extract, it is characterized in that：It is to be prepared from by the following method：
1) the cold medicine medicinal material of skin is taken, is smashed, 8-12 times of decocting is added and boils 0.5-1.5h, decoct as 1-3 times, filter, merging filtrate；
2) step 1 is taken) gained filtrate, concentrate, add 50-70%V/V ethanol, precipitate 6-18h, take supernatant, concentrate, produce and carry
Take thing.
2. herba gueldenstaedtia extract according to claim 1, it is characterized in that：
The step 1) in, the amount of water is 12 times of the cold medicine medicinal material of skin；Decocting time is 0.5h；It is 2 times to decoct number of times.
The step 2) in, the thickening temperature is 70 DEG C, and concentration of alcohol is 60%V/V；Sedimentation time is 18h.
3. herba gueldenstaedtia extract according to claim 1 or 2, it is characterized in that：Maackiain content is 0.1978-
0.2501mg/g, onocerin content is 0.2127-0.2958mg/g.
4. the herba gueldenstaedtia extract according to claim 1-3 any one, it is characterized in that：Described skin trembles with fear medicine from beans
Section's Gueldenstaedtia verna platymiscium river Yunnan Gueldenstaedtia verna Gueldenstaedtia delavayi Franch drying herb.
The medicine granule 5. a kind of skin is trembled with fear, it is characterized in that：It is that following method is prepared from：Take claim 1-4 any one institute
The herba gueldenstaedtia extract stated, it is 1-5 to add with extract weight proportioning:1 auxiliary material, 55-95%V/V ethanol is stirred, and is dried,
Produce.
The medicine granule 6. skin according to claim 5 is trembled with fear, it is characterized in that：The weight proportion of the auxiliary material and extract is 4:
1；Concentration of alcohol is 75%V/V；Auxiliary material is one kind in dextrin, DEXTROSE ANHYDROUS, soluble starch.
7. a kind of method for preparing herba gueldenstaedtia extract, it is characterized in that：Comprise the following steps：
1) the cold medicine medicinal material of skin is taken, is smashed, 8-12 times of decocting is added and boils 0.5-1.5h, decoct as 1-3 times, filter, merging filtrate；
2) step 1 is taken) gained filtrate, relative density 1.10 is concentrated into, 50-70%V/V ethanol is added, 6-18h is precipitated, takes supernatant
Liquid, it is 1.23 ± 0.03 to be concentrated into relative density, produces medicinal extract.
8. method according to claim 7, it is characterized in that：
The step 1) in, the amount of water is 12 times of the cold medicine medicinal material of skin, and decocting time is 0.5h, and it is 2 times to decoct number of times；
The step 2) in, the thickening temperature is 70 DEG C, and concentration of alcohol is 60%V/V, and the sedimentation time is 18h.
9. a kind of method for preparing the cold medicine granule of skin, it is characterized in that：The cold medicine of the skin described in claim 1-4 any one is taken to carry
Thing is taken, it is 1-5 to add with extract weight proportioning:1 auxiliary material, 55-95%V/V ethanol is stirred, and is dried, is produced.
10. method according to claim 9, it is characterized in that：The weight proportion of the auxiliary material and extract is 4:1；Ethanol
Concentration is 75%V/V；Auxiliary material is one kind in dextrin, DEXTROSE ANHYDROUS, soluble starch.
11. the skin described in extract, claim 5 or 6 described in claim 1 or 2 is trembled with fear, medicine particle is being prepared with heat-clearing solution
Purposes in poison or analgesic medicine.
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Citations (1)
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| CN102641324A (en) * | 2011-05-16 | 2012-08-22 | 成都中医药大学 | Herba gueldenstaedtia extract and uses thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102641324A (en) * | 2011-05-16 | 2012-08-22 | 成都中医药大学 | Herba gueldenstaedtia extract and uses thereof |
| CN102645497A (en) * | 2011-05-16 | 2012-08-22 | 成都中医药大学 | Method for inspecting quality of Gueldenstaedtia delavayi Franch. |
| CN102641323A (en) * | 2011-05-16 | 2012-08-22 | 成都中医药大学 | New application of Gueldenstaedtia delavayi Franch or extracts thereof |
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