CN106177407A - A kind of Qinghuozhimaipian and preparation method thereof - Google Patents
A kind of Qinghuozhimaipian and preparation method thereof Download PDFInfo
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- CN106177407A CN106177407A CN201610563581.9A CN201610563581A CN106177407A CN 106177407 A CN106177407 A CN 106177407A CN 201610563581 A CN201610563581 A CN 201610563581A CN 106177407 A CN106177407 A CN 106177407A
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- qinghuozhimaipian
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- tank body
- heat conduction
- jolting plate
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- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000012567 medical material Substances 0.000 claims abstract description 12
- 210000000845 cartilage Anatomy 0.000 claims abstract description 11
- 239000012141 concentrate Substances 0.000 claims abstract description 10
- 230000004663 cell proliferation Effects 0.000 claims abstract description 7
- 230000001629 suppression Effects 0.000 claims abstract description 7
- 241000746375 Andrographis Species 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 235000019640 taste Nutrition 0.000 claims abstract description 6
- 239000003814 drug Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 13
- 229940079593 drug Drugs 0.000 claims description 11
- 238000000605 extraction Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 9
- 238000007790 scraping Methods 0.000 claims description 9
- 230000000149 penetrating effect Effects 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 230000008602 contraction Effects 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 244000111489 Gardenia augusta Species 0.000 claims 1
- 235000018958 Gardenia augusta Nutrition 0.000 claims 1
- 206010061218 Inflammation Diseases 0.000 claims 1
- 238000009835 boiling Methods 0.000 claims 1
- 230000004054 inflammatory process Effects 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 14
- 229960004756 ethanol Drugs 0.000 description 12
- 238000002474 experimental method Methods 0.000 description 8
- BOJKULTULYSRAS-OTESTREVSA-N Andrographolide Chemical compound C([C@H]1[C@]2(C)CC[C@@H](O)[C@]([C@H]2CCC1=C)(CO)C)\C=C1/[C@H](O)COC1=O BOJKULTULYSRAS-OTESTREVSA-N 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- ASLUCFFROXVMFL-UHFFFAOYSA-N andrographolide Natural products CC1(CO)C(O)CCC2(C)C(CC=C3/C(O)OCC3=O)C(=C)CCC12 ASLUCFFROXVMFL-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 239000006144 Dulbecco’s modified Eagle's medium Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 239000012531 culture fluid Substances 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- IBFYXTRXDNAPMM-BVTMAQQCSA-N Geniposide Chemical compound O([C@@H]1OC=C([C@@H]2[C@H]1C(=CC2)CO)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O IBFYXTRXDNAPMM-BVTMAQQCSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 102000004142 Trypsin Human genes 0.000 description 2
- 108090000631 Trypsin Proteins 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 239000006285 cell suspension Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000012588 trypsin Substances 0.000 description 2
- WEEMDRWIKYCTQM-UHFFFAOYSA-N 2,6-dimethoxybenzenecarbothioamide Chemical compound COC1=CC=CC(OC)=C1C(N)=S WEEMDRWIKYCTQM-UHFFFAOYSA-N 0.000 description 1
- 206010051625 Conjunctival hyperaemia Diseases 0.000 description 1
- 238000002965 ELISA Methods 0.000 description 1
- XJMPAUZQVRGFRE-SCHFUKFYSA-N Gardenoside Natural products O=C(OC)C=1[C@H]2[C@H]([C@H](O[C@H]3[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O3)OC=1)[C@@](O)(CO)C=C2 XJMPAUZQVRGFRE-SCHFUKFYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229920002334 Spandex Polymers 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000010165 autogamy Effects 0.000 description 1
- FCPVYOBCFFNJFS-LQDWTQKMSA-M benzylpenicillin sodium Chemical compound [Na+].N([C@H]1[C@H]2SC([C@@H](N2C1=O)C([O-])=O)(C)C)C(=O)CC1=CC=CC=C1 FCPVYOBCFFNJFS-LQDWTQKMSA-M 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000004113 cell culture Methods 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010219 correlation analysis Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- -1 dehydrorographolide Chemical compound 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 231100000673 dose–response relationship Toxicity 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- XJMPAUZQVRGFRE-AYDWLWLASA-N methyl (1s,4as,7s,7as)-7-hydroxy-7-(hydroxymethyl)-1-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy-4a,7a-dihydro-1h-cyclopenta[c]pyran-4-carboxylate Chemical compound O([C@@H]1OC=C([C@@H]2[C@H]1[C@](C=C2)(O)CO)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O XJMPAUZQVRGFRE-AYDWLWLASA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- QEVHRUUCFGRFIF-MDEJGZGSSA-N reserpine Chemical compound O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C(C5=CC=C(OC)C=C5N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 QEVHRUUCFGRFIF-MDEJGZGSSA-N 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000004759 spandex Substances 0.000 description 1
- 229960002385 streptomycin sulfate Drugs 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 208000004371 toothache Diseases 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- 239000003643 water by type Substances 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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/19—Acanthaceae (Acanthus family)
-
- 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)
- A61K36/74—Rubiaceae (Madder family)
- A61K36/744—Gardenia
-
- 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)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
- A61K36/8968—Ophiopogon (Lilyturf)
-
- 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
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B11/00—Machines or apparatus for drying solid materials or objects with movement which is non-progressive
- F26B11/12—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in stationary drums or other mainly-closed receptacles with moving stirring devices
- F26B11/14—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in stationary drums or other mainly-closed receptacles with moving stirring devices the stirring device moving in a horizontal or slightly-inclined plane
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B23/00—Heating arrangements
- F26B23/04—Heating arrangements using electric heating
- F26B23/06—Heating arrangements using electric heating resistance heating
-
- 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
-
- 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
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- 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)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- Medicinal Chemistry (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Epidemiology (AREA)
- Botany (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Medical Informatics (AREA)
- Biotechnology (AREA)
- Alternative & Traditional Medicine (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sustainable Development (AREA)
- Medicinal Preparation (AREA)
Abstract
nullThe present invention provides the preparation method of a kind of Qinghuozhimaipian，Take Herba Andrographis 800g、Fructus Gardeniae 100g、Radix Ophiopogonis 100g，Above three tastes，Add the water of 10 times of weight of medical material，Soak 0.5h，Decoct 1 hour，Filter，Medicinal residues add the water of 8 times of weight of medical material，Decoct 1 hour，Medicinal liquid leaches，Merge twice decoction liquor，Being concentrated into 60 DEG C of relative densities is 1.05，Adding ethanol makes the percent by volume of alcohol content reach 75%，Stirring，Stand，Filter，When filtrate is concentrated into 65 DEG C, relative density is 1.25，And reclaim ethanol，Obtain concentrated solution，Use supercritical extraction，Obtain supercritical extract，Continue to concentrate，Concentrated solution is dried,Pelletize，Tabletting，Obtain Qinghuozhimaipian，And use distinctive concentration and drying equipment，The Qinghuozhimaipian extractive content prepared is high，Application in the concurrent suppression Mouse cartilage ATDC5 cell proliferation of preparation now.
Description
Technical field
The present invention relates to technical field of extraction of Chinese traditional medicine, be specifically related to a kind of Qinghuozhimaipian and preparation method thereof.
Background technology
Qinghuozhimaipian is heat-clearing formula, has heat-clearing and toxic substances removing, effect of removing heat from blood detumescence.Cure mainly the throat caused by exuberant lung-stomach heat
Swell and ache, heating, toothache, conjunctival congestion.Preparation method of the prior art, technique is coarse, backward, and impurity is many, and active constituent content is low,
Cause patient's consumption excessive, it has not been convenient to take, had a strong impact on this product and applied clinically.
Summary of the invention
Goal of the invention: in order to solve the problems referred to above, it is an object of the invention to provide a kind of Qinghuozhimaipian and preparation thereof
Method.
Technical scheme: it is an object of the invention to by following scheme realization:
A kind of Qinghuozhimaipian, preparation method is: takes Herba Andrographis 800g, Fructus Gardeniae 100g, 100g Radix Ophiopogonis, above three tastes, adds
The water of 10 times of weight of medical material, soaks 0.5h, decocts 1 hour, filters, and medicinal residues add the water of 8 times of weight of medical material, decoct 1 hour,
Medicinal liquid leaches, and merges twice decoction liquor, and being concentrated into 60 DEG C of relative densities is 1.05, adds ethanol and makes the percent by volume of alcohol content reach
75%, stirring, stand, filter, when filtrate is concentrated into 65 DEG C, relative density is 1.25, and reclaims ethanol, obtains concentrated solution, uses super
Critical extraction, obtains supercritical extract, continues to concentrate, is dried by concentrated solution, pelletizes, and tabletting obtains Qinghuozhimaipian.
Described Qinghuozhimaipian, in above-mentioned preparation method, supercritical extraction method is: joined by water extract-alcohol precipitation concentrated solution
In CO2 supercritical extraction device, ethanol is as entrainer, and it is 4-6% that entrainer accounts for the percent by volume of total extractant, extraction pressure
Power 15-30MPa, temperature 30-50 DEG C, CO2 flow 1-3m1/g crude drug min, extraction time 150-180min, obtain supercritical extraction
Taking thing, optimum condition is: the percent by volume that described CO2 supercritical extraction entrainer accounts for total extractant is 5%, described CO2
Extracting pressure 20MPa of supercritical extraction, temperature 40 DEG C, CO2 flow 2ml/g crude drug min, extraction time 160min.
Described Qinghuozhimaipian, concentrates for three times in above-mentioned preparation method and uses device, including tank body, be arranged on described tank body
On charging aperture and be arranged on the discharge nozzle of described tank base, described discharge nozzle is provided with discharge valve and filter,
It is provided with shaft in described tank body, described shaft is provided with stirring paddle, be provided with and described stirring at the top of described tank body
The stirring motor that axle is connected, the diapire in described tank body is provided with vibrations chamber, is provided with jolting plate at described vibrations intracavity, in institute
State and be provided with electromagnetic shaker between jolting plate and described vibrations chamber, the sidewall in described tank body is provided with cavity, at described jolting plate
End face be provided with scraper plate, between described scraper plate and described cavity, be provided with telescopic cylinder, described scraper plate is at described telescopic cylinder
Effect is lower realizes the scraping to jolting plate surface, is provided with the discharging being connected with described discharge nozzle at the center of described jolting plate
Mouthful.
Described Qinghuozhimaipian, in above-mentioned preparation method, jolting plate described in enrichment facility sets with the junction in described vibrations chamber
There is sealing metal bar, described tank body is provided with the shake control device being connected with described electromagnetic shaker.
Described Qinghuozhimaipian, in above-mentioned preparation method, the bottom of scraper plate described in enrichment facility is provided with metal scraping layer, institute
State metal scraping layer to be pressed on described jolting plate, described tank body is provided with the extension and contraction control being connected with described telescopic cylinder
Button.
Described Qinghuozhimaipian, is provided with water tester in tank body described in enrichment facility in above-mentioned preparation method, described
Cooler it is provided with in discharge nozzle.
Described Qinghuozhimaipian, is dried in above-mentioned preparation method and uses device, including body, be arranged in described body
Axis, the rotation being arranged on described axis outer wall holds dish, is provided with vibration motor in the lower end of described axis, at described body
Top be provided with vapours conveyance conduit, it is characterised in that: in described axis, be provided with cavity, be provided with at the top of described axis
Disk, described disk is arranged on described rotation and holds the top of dish, is provided with the most penetrating pore, described on described disk
It is provided with the heat conduction mast being connected with described cavity in disk, in described cavity, is provided with electrical heating block, on described heat conduction mast
Being provided with heat conduction thorn post, described heat conduction thorn post stretches in described pore, is provided with temperature sensor, at described cavity in described body
Inside being provided with the driver being connected with described temperature sensor, described driver switchs with the control of described electrical heating block and is connected
Connect.
Described Qinghuozhimaipian, in above-mentioned preparation method, pore described in dry use device is the loudspeaker that big bottom, top is little
Shape hole, described heat conduction thorn post stretches into the middle part in described horn-like hole, is provided with the most penetrating conduction net on described horn-like hole
Hole.
Described Qinghuozhimaipian, is dried in above-mentioned preparation method and uses the bottom surface of body described in device to be provided with chamber door, described
Chamber door is arranged on to rotate and holds the lowermost end of dish, and described heat conduction mast be silver-colored or aluminum or copper mast.
The application in preparation suppression Mouse cartilage ATDC5 cell proliferation of the described Qinghuozhimaipian.
In prior art, Qinghuozhimaipian uses the method that water puies forward, and technique is coarse, backward, and impurity is many, causes patient's consumption
Excessive, it has not been convenient to take, andrographolide, dehydrorographolide, jasminoidin yield in Qinghuozhimaipian prepared by the present invention
Increasing, content is high, the concentrator simple in construction in the present invention, simple operation, and it is provided with jolting plate and electromagnetic shaker, and is additionally provided with
Scraper plate and the telescopic cylinder being connected with described scraper plate, can effectively prevent tank base from luming, be greatly improved to a certain extent
The efficiency of heating surface, efficiently solves caking bottom easily occurring in conventional art Chinese medicinal concentration equipment and affects the technology of the efficiency of heating surface
Deficiency, stability in use is good and the suitability strong, and the stable effective ingredients of medicine is not destroyed.This drying equipment structure is simple, behaviour
It is convenient to make, and is provided with disk at the top of axis, and is provided with pore on disk, and vapours can be made to pass through disk, and
It is provided with electrical heating block and heat conduction mast in axis, electrical heating block can be started as required, and realize temperature by heat conduction mast
Transmission, and mix with by the vapours of disk, thereby may be ensured that the temperature of vapours, regulation performance is good, uses steady
Qualitative by force, efficiently solve in conventional art the uncontrollable technical deficiency of temperature in vapours heating drier.And find institute
State Qinghuozhimaipian application in preparation suppression Mouse cartilage ATDC5 cell proliferation.
Accompanying drawing explanation
In order to make present disclosure be more likely to be clearly understood, below according to specific embodiment and combine accompanying drawing, right
The present invention is described in further detail, wherein:
Fig. 1 is the structural representation of enrichment facility of the present invention.
Fig. 2 is the structural representation of drying device of the present invention.
Detailed description of the invention
Form by the following examples, is described in further detail the foregoing of the present invention again, but should be by this
Being interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to Examples below, all technology realized based on foregoing of the present invention are equal
Belong to the scope of the present invention.
Embodiment 1
Take Herba Andrographis 800g, Fructus Gardeniae 100g, 100g Radix Ophiopogonis, above three tastes, add the water of 10 times of weight of medical material, soak 0.5h,
Decocting 1 hour, filter, medicinal residues add the water of 8 times of weight of medical material, decoct 1 hour, and medicinal liquid leaches, and merges twice decoction liquor, dense
Being reduced to 60 DEG C of relative densities is 1.05, adds ethanol and makes the percent by volume of alcohol content reach 75%, and stirring, standing, filtration, filtrate is dense
Being reduced to relative density when 65 DEG C is 1.25, and reclaims ethanol, obtains concentrated solution, uses supercritical extraction, obtains supercritical extract, continue
Continuous concentrate, concentrated solution is dried, pelletizes, tabletting, obtain Qinghuozhimaipian, every 0.5 gram.
The preparation method of described Qinghuozhimaipian, described supercritical extraction method is: joined by water extract-alcohol precipitation concentrated solution
In CO2 supercritical extraction device, ethanol is as entrainer, and it is 4% that entrainer accounts for the percent by volume of total extractant, extracting pressure
30MPa, temperature 30 DEG C, CO2 flow 3m1/g crude drug min, extraction time 150min, obtain supercritical extract.
See Fig. 1: the preparation method of described Qinghuozhimaipian, above-mentioned No. three enrichment facilities, including tank body 1, be arranged on described
Charging aperture on tank body 12 and be arranged on the discharge nozzle 3 bottom described tank body 1, is provided with discharge valve 4 He on described discharge nozzle 3
Filter 5, is provided with shaft 6 in described tank body 1, is provided with stirring paddle 7 on described shaft 6, at the top of described tank body 1
Being provided with the stirring motor 8 being connected with described shaft 6, the diapire in described tank body 1 is provided with vibrations chamber 9, in described vibrations
It is provided with jolting plate 10 in chamber 9, between described jolting plate 10 and described vibrations chamber 9, is provided with electromagnetic shaker 11, permissible by electromagnetic shaker
Make jolting plate shake, thus can effectively prevent drug particles from concentrating on jolting plate, thus drug particles can be prevented at jolting plate
Upper caking, the sidewall in described tank body 1 is provided with cavity 12, and the end face at described jolting plate 10 is provided with scraper plate 13, described
It is provided with telescopic cylinder 14 between scraper plate 13 and described cavity 12, telescopic cylinder can be controlled as required, make scraper plate at jolting plate
Surface scrape, thus part is concentrated at the drug particles on jolting plate surface and scrapes, described scraper plate 13 is at described telescopic cylinder
The effect of 14 is lower realizes the scraping to jolting plate 10 surface, is provided with at the center of described jolting plate 10 and is connected with described discharge nozzle 3
Logical discharging opening 15.
It is provided with sealing metal bar 16 in the junction of described jolting plate 10 with described vibrations chamber 9, described tank body is provided with
The shake control device 17 being connected with described electromagnetic shaker.
Be provided with metal scraping layer 18 in the bottom of described scraper plate, described metal scraping layer is pressed on described jolting plate,
Described tank body is provided with the extension and contraction control button 19 being connected with described telescopic cylinder.
In described tank body, it is provided with water tester 21, in described discharge nozzle, is provided with cooler 20.
See Fig. 2, the preparation method of described Qinghuozhimaipian, above-mentioned dry use device, including body 1, be arranged on described
Axis 2 in body 1, the rotation being arranged on described axis 2 outer wall holds dish 3, is provided with vibrations electricity in the lower end of described axis 2
Machine 4, is provided with vapours conveyance conduit 5 at the top of described body 1, is provided with cavity 6 in described axis 2, at described axis 2
Top is provided with disk 7, and described disk 7 is arranged on described rotation and holds the top of dish 3, is provided with the most penetrating on described disk 7
Pore 8, vapours through disk, enters rotation and holds dish, be provided with and leading that described cavity 6 is connected in described disk 7
Plume bar 9, is provided with electrical heating block 10 in described cavity 6, and described heat conduction mast 9 is provided with heat conduction thorn post 11, and described heat conduction is stung
Post 11 stretches in described pore 8, can be greatly improved the temperature mixing between vapours and electrical heating block, improves temperature controlled
Efficiency, is provided with temperature sensor 12 in described body 1, is provided with is connected with described temperature sensor 12 in described cavity 6
Driver 13, the control of described driver 13 and described electrical heating block 10 switchs and is connected.Temperature sensor in the present embodiment
Being the most already present product with driver, it has only to be attached according to the corresponding description of product in use.
Described pore is the horn-like hole that big bottom, top is little, and described heat conduction thorn post stretches into the middle part in described horn-like hole,
Described horn-like hole is provided with the most penetrating conduction mesh 14.
Be provided with chamber door 15 in the bottom surface of described body, described chamber door is arranged on and rotates the lowermost end holding dish.
Described heat conduction mast is silver or aluminum or copper mast.
Embodiment 2
Take Herba Andrographis 800g, Fructus Gardeniae 100g, 100g Radix Ophiopogonis, above three tastes, add the water of 10 times of weight of medical material, soak 0.5h,
Decocting 1 hour, filter, medicinal residues add the water of 8 times of weight of medical material, decoct 1 hour, and medicinal liquid leaches, and merges twice decoction liquor, dense
Being reduced to 60 DEG C of relative densities is 1.05, adds ethanol and makes the percent by volume of alcohol content reach 75%, and stirring, standing, filtration, filtrate is dense
Being reduced to relative density when 65 DEG C is 1.25, and reclaims ethanol, obtains concentrated solution, uses supercritical extraction, obtains supercritical extract, continue
Continuous concentrate, concentrated solution is dried, pelletizes, tabletting, obtain Qinghuozhimaipian, every 0.5 gram.
The preparation method of described Qinghuozhimaipian, described supercritical extraction method is: joined by water extract-alcohol precipitation concentrated solution
In CO2 supercritical extraction device, ethanol is as entrainer, and it is 6% that entrainer accounts for the percent by volume of total extractant, extracting pressure
15MPa, temperature 50 C, CO2 flow 1m1/g crude drug min, extraction time 180min, obtain supercritical extract.
Concentrate with drying device ibid.
Embodiment 3
Take Herba Andrographis 800g, Fructus Gardeniae 100g, 100g Radix Ophiopogonis, above three tastes, add the water of 10 times of weight of medical material, soak 0.5h,
Decocting 1 hour, filter, medicinal residues add the water of 8 times of weight of medical material, decoct 1 hour, and medicinal liquid leaches, and merges twice decoction liquor, dense
Being reduced to 60 DEG C of relative densities is 1.05, adds ethanol and makes the percent by volume of alcohol content reach 75%, and stirring, standing, filtration, filtrate is dense
Being reduced to relative density when 65 DEG C is 1.25, and reclaims ethanol, obtains concentrated solution, uses supercritical extraction, obtains supercritical extract, continue
Continuous concentrate, concentrated solution is dried, pelletizes, tabletting, obtain Qinghuozhimaipian, every 0.5 gram.
The preparation method of described Qinghuozhimaipian, described supercritical extraction method is: joined by water extract-alcohol precipitation concentrated solution
In CO2 supercritical extraction device, ethanol is as entrainer, and it is 5% that entrainer accounts for the percent by volume of total extractant, described CO2
Extracting pressure 20MPa of supercritical extraction, temperature 40 DEG C, CO2 flow 2ml/g crude drug min, extraction time 160min, obtain super
Critical extract.
Concentrate with drying device ibid.
Above-described embodiment Chinese medicine all meets standards of pharmacopoeia.
Embodiment 4: active constituent content measuring experimentation data in Qinghuozhimaipian of the present invention
1.1 Experimental agents: Qinghuozhimaipian of the present invention: prepare by embodiment 1-3 method.Matched group uses the commonly side of concentration
Method prepares Qinghuozhimaipian.
1.2 instruments: high performance liquid chromatograph system includes high performance liquid chromatograph (Waters 515)；P200 high-pressure pump；
Waters2487 UV-detector and GJ605 type high pressure six-way injection valve；Chromatographic column be Hypersil ODSC18 post (4.6mm ×
250mm,5μm)；Data acquisition and process use HS Data Processing in Chromatography Workstation V4.0+ (Hangzhou English spectrum science and technology)
1.3 condition determinations: use high performance liquid chromatography, by version official method in 2015, are bonded with octadecylsilane
Silica gel is filler；With acetonitrile as mobile phase A, water is that flowing carries out gradient by the regulation in pharmacopeia (Qinghuozhimaipian) table mutually and washes
De-；Andrographolide, dehydrorographolide detection wavelength is 225nm, jasminoidin detection wavelength is 238nm.Number of theoretical plate is pressed
Andrographolide peak and dehydrorographolide peak calculate and all should be not less than 2000.
1.4 experimental result
Active constituent content measuring result in Qinghuozhimaipian prepared by each embodiment
| Sample source | Andrographolide peak and Determination of Dehydroandrographoliin (mg/ sheet) | Determination of Gardenoside (mg/ sheet) |
| Embodiment 1 | 3.70 | 3.12 |
| Embodiment 2 | 4.36 | 3.68 |
| Embodiment 3 | 3.93 | 2.89 |
| Matched group | 2.17 | 1.34 |
According to the result of the test of upper table, in Qinghuozhimaipian prepared by embodiment of the present invention 1-3, peaceful effective ingredient contains
Amount is apparently higher than matched group.
Embodiment 5: the experimentation data of Qinghuozhimaipian of the present invention suppression Mouse cartilage ATDC5 cell proliferation
1 experiment material
1.1 experiment cell strains
Mouse cartilage ATDC5 cell, Nanjing Medical University's laboratory cell storehouse, DMEM+10%FBS cellar culture.
1.2 Experimental agents
Drugs: Qinghuozhimaipian of the present invention: prepare by embodiment 1 method.
Medicinal liquid liquid storage: weigh 100mg Qinghuozhimaipian, is dissolved in 5ml dehydrated alcohol, and 0.2 μm filter filters, 500 μ l
Doff pipe subpackage ,-20 DEG C of storages, 0.2 μm filter filters dehydrated alcohol in case matched group is used simultaneously.
1.3 experiment reagent
DMEM (GIBCO company Cat.No.12100-061Lot.No.758137)；Hyclone (Hangzhoupro, sky, Zhejiang biology section
Skill company limited Lot.No.100419)；NaHCO3 (the long hundred million chemical reagent company limited Cat.No.11810-in Shanghai
033Lot.No.1088387)；Trypsin (AMRESCO company lot number: 2010/04)；EDTA (AMRESCO company lot number:
2009/10)；Penicillin G Sodium Salt (AMRESCO company lot number: 2010242)；Streptomycin
Sulfate (AMRESCO company lot number: 2010382)；Dehydrated alcohol (Nanjing Chemistry Reagent Co., Ltd.'s lot number:
080310182)；MTT (Biosharp lot number: 0793)；PBS (laboratory autogamy)；
1.4 experiment equipment
Lycra inverted microscope (Germany Leica model: DM1L)；Visible-ultraviolet light microwell plate detector (MD company of the U.S.
Model: SPECTRA MAX 190)；CO2 incubator (FORMA model: 3111)；Super-clean bench (safe and sound company of Su Jing group manufacture type
Number: SW-CJ-ZFD)；Pure water instrument (Spring company of U.S. model: S/N 020579)；Accurate pipettor (Gilson Inc of France
Model: P2)；Electronic balance (Sai Duolisi company limited of Germany model: BT323S)；Full-automatic high-pressure autoclave (Japan SANYO
Company's model: MLS-3020)；Table electrothermal air dry oven (Shanghai precision experimental facilities company model: DHG9123A)；Refrigerator
(Siemens Company's model: KG18V21TI)；Liquid nitrogen container (CBS model: 2001)；Low speed centrifuge (Anting Scientific Instrument Factory, Shanghai
Model: KA-1000)；0.2 μm filter (MILLIPORE model: SLGP033RB)；10cm culture dish (NEST company), 96 hole trainings
Support plate (NEST company)；Cell counting count board；Centrifuge tube, pipet, Tips are some.
2 experimental techniques
1) Mouse cartilage ATDC5 cell DMEM+10%FBS in 37 DEG C, 5%CO2 carry out cellar culture (10cm cultivate
Ware), when cell grows to logarithmic (log) phase, collect cell, discard culture fluid, PBS rinses 3 times, adds 3ml 0.25% Trypsin
Enzyme-0.04%EDTA, after 37 DEG C of digestion 2min, is added thereto in 5ml complete medium and reacts, by its turn after piping and druming cell
Entering in centrifuge tube, 1000rpm is centrifuged 5min, adjusts 3 × 104/ml of concentration of cell suspension.
2) entering in 96 well culture plates by cell kind, every hole adds cell suspension 180 μ l, and culture plate is put in cell culture incubator
(37 DEG C, 5%CO2) cellar culture.
3) according to cell growth status, general long to 50%-70%, add Qinghuozhimaipian solution, continue to cultivate 24h.
4) add 20 μ l MTT solution (5mg/ml, i.e. 0.5%MTT) after 24h, continue to cultivate 4h.
5) after 4h, buckle method removes supernatant, pats dry gently with absorbent paper, and every hole adds 200 μ l dimethyl sulfoxide, puts shaking table
Upper low-speed oscillation 10min, makes crystal fully dissolve.The light absorption value in each hole is measured at enzyme-linked immunosorbent assay instrument 490nm.
6) arranging background (being not added with cell, only add culture fluid), (cell, the medicine dissolution of same concentrations are situated between control wells simultaneously
Matter, culture fluid, MTT, dimethyl sulfoxide), often group sets 6 multiple holes.
7) suppression ratio of cell is represented by result with medicine:
Cell proliferation suppression ratio (%)=(control wells OD value-dosing holes OD value)/control wells OD value × 100%.Experiment weight
Multiple 3 times.
3 statistical dispositions
Use the correlation analysis in Microsoft Excel 2003 software and Student t inspection, data with mean ±
S.D. represent.
4 experimental results
Statistical result showed after mtt assay experiment, compares with matched group, when dosage reaches 5mg/ml, to Mouse cartilage
ATDC5 cell inhibitory effect variant (P < 0.05), dosage this difference when 10mg/ml has significance (P < 0.01), works as agent
Amount reaches there is pole significant difference (P < 0.001) during 15-20mg/ml.
Qinghuozhimaipian is to Mouse cartilage ATDC5 cell inhibitory effect influence research
Note: compare with matched group, * P < 0.01；**P<0.001
5 experiment conclusion
Qinghuozhimaipian can suppress Mouse cartilage ATDC5 cell proliferation, and the cell reducing Mouse cartilage ATDC5 cell is raw
Long number, this effect is dose dependent.
Claims (10)
1. a Qinghuozhimaipian, it is characterised in that preparation method is: take Herba Andrographis 800g, Fructus Gardeniae 100g, 100g Radix Ophiopogonis, above
Three tastes, add the water of 10 times of weight of medical material, soak 0.5h, decoct 1 hour, filter, and medicinal residues add the water of 8 times of weight of medical material, decoct
Boiling 1 hour, medicinal liquid leaches, and merges twice decoction liquor, and being concentrated into 60 DEG C of relative densities is 1.05, adds ethanol and makes the volume of alcohol content
Percentage ratio reaches 75%, and stirring, standing, filtration, when filtrate is concentrated into 65 DEG C, relative density is 1.25, and reclaims ethanol, obtains concentration
Liquid, uses supercritical extraction, obtains supercritical extract, continues to concentrate, is dried by concentrated solution, pelletizes, and tabletting, must relieve inflammation or internal heat Cape jasmine
Oatmeal.
Qinghuozhimaipian the most according to claim 1, it is characterised in that in described preparation method, supercritical extraction method is: will
Water extract-alcohol precipitation concentrated solution joins CO2In supercritical extraction device, ethanol is as entrainer, and entrainer accounts for the volume of total extractant
Percentage ratio is 4-6%, extracting pressure 15-30MPa, temperature 30-50 DEG C, CO2Flow 1-3m1/g crude drug min, extraction time
150-180min, obtains supercritical extract, and optimum condition is: described CO2Supercritical extraction entrainer accounts for the body of total extractant
Long-pending percentage ratio is 5%, described CO2Extracting pressure 20MPa of supercritical extraction, temperature 40 DEG C, CO2Flow 2ml/g crude drug min,
Extraction time 160min.
Qinghuozhimaipian the most according to claim 1, it is characterised in that concentrate for three times in described preparation method and use device, bag
Include tank body, the charging aperture being arranged on described tank body and the discharge nozzle being arranged on described tank base, described discharge nozzle sets
There are discharge valve and filter, in described tank body, are provided with shaft, described shaft is provided with stirring paddle, at described tank body
Top be provided with the stirring motor being connected with described shaft, the diapire in described tank body be provided with vibrations chamber, in described shake
Dynamic intracavity is provided with jolting plate, is provided with electromagnetic shaker, on the sidewall in described tank body between described jolting plate and described vibrations chamber
Being provided with cavity, the end face at described jolting plate is provided with scraper plate, is provided with telescopic cylinder between described scraper plate and described cavity, described
Scraper plate realizes the scraping to jolting plate surface under the effect of described telescopic cylinder, is provided with described at the center of described jolting plate
The discharging opening that discharge nozzle is connected.
Qinghuozhimaipian the most according to claim 3, it is characterised in that jolting plate described in enrichment facility in described preparation method
It is provided with sealing metal bar with the junction in described vibrations chamber, described tank body is provided with the vibrations control being connected with described electromagnetic shaker
Device processed.
Qinghuozhimaipian the most according to claim 3, it is characterised in that scraper plate described in enrichment facility in described preparation method
Bottom is provided with metal scraping layer, and described metal scraping layer is pressed on described jolting plate, is provided with and stretches with described on described tank body
The extension and contraction control button that contracting cylinders connects.
Qinghuozhimaipian the most according to claim 3, it is characterised in that in described preparation method in tank body described in enrichment facility
It is provided with water tester, in described discharge nozzle, is provided with cooler.
Qinghuozhimaipian the most according to claim 1, it is characterised in that be dried in described preparation method and use device, including machine
Body, is arranged on the axis in described body, and the rotation being arranged on described axis outer wall holds dish, sets in the lower end of described axis
There is vibration motor, be provided with vapours conveyance conduit at the top of described body, it is characterised in that: in described axis, it is provided with sky
Chamber, is provided with disk at the top of described axis, and described disk is arranged on described rotation and holds the top of dish, sets on described disk
There is the most penetrating pore, in described disk, be provided with the heat conduction mast being connected with described cavity, be provided with in described cavity
Electrical heating block, described heat conduction mast is provided with heat conduction thorn post, and described heat conduction thorn post stretches in described pore, sets in described body
Having temperature sensor, be provided with the driver being connected with described temperature sensor in described cavity, described driver is with described
The control switch of electrical heating block is connected.
Qinghuozhimaipian the most according to claim 7, it is characterised in that be dried described in use device thin in described preparation method
Hole is the horn-like hole that big bottom, top is little, and described heat conduction thorn post stretches into the middle part in described horn-like hole, in described horn-like hole
It is provided with the most penetrating conduction mesh.
Qinghuozhimaipian the most according to claim 7, it is characterised in that be dried in described preparation method and use machine described in device
The bottom surface of body is provided with chamber door, and described chamber door is arranged on and rotates the lowermost end holding dish, and described heat conduction mast is silver or aluminum or copper
Mast.
Qinghuozhimaipian answering in preparation suppression Mouse cartilage ATDC5 cell proliferation the most according to claim 1
With.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108085751A (en) * | 2017-12-13 | 2018-05-29 | 刘翠玲 | A kind of silk cocoon digesting drier |
Citations (1)
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| CN104606477A (en) * | 2015-01-28 | 2015-05-13 | 广西日田药业集团有限责任公司 | Fire-clearing jasmine and radix ophiopogonis film-coated tablets and preparation method thereof |
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2016
- 2016-07-16 CN CN201610563581.9A patent/CN106177407A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104606477A (en) * | 2015-01-28 | 2015-05-13 | 广西日田药业集团有限责任公司 | Fire-clearing jasmine and radix ophiopogonis film-coated tablets and preparation method thereof |
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| 国家药典委员会: "《中华人民共和国药典：2010年版：第二增补本》", 30 September 2013, 中国医药科技出版社 * |
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| CN108085751A (en) * | 2017-12-13 | 2018-05-29 | 刘翠玲 | A kind of silk cocoon digesting drier |
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