CN110141605A - A kind of preparation method of snowpoppy total alkaloid nanoparticle - Google Patents
A kind of preparation method of snowpoppy total alkaloid nanoparticle Download PDFInfo
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- CN110141605A CN110141605A CN201910316392.5A CN201910316392A CN110141605A CN 110141605 A CN110141605 A CN 110141605A CN 201910316392 A CN201910316392 A CN 201910316392A CN 110141605 A CN110141605 A CN 110141605A
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- 229930013930 alkaloid Natural products 0.000 title claims abstract description 66
- 150000003797 alkaloid derivatives Chemical class 0.000 title claims abstract description 65
- 241001247804 Eomecon chionantha Species 0.000 title claims abstract description 53
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002425 crystallisation Methods 0.000 claims abstract description 16
- 230000008025 crystallization Effects 0.000 claims abstract description 15
- 230000002411 adverse Effects 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 230000001376 precipitating effect Effects 0.000 claims abstract description 8
- 238000005057 refrigeration Methods 0.000 claims abstract description 8
- 239000007921 spray Substances 0.000 claims abstract description 8
- 239000003814 drug Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 230000008719 thickening Effects 0.000 claims abstract description 4
- 229940079593 drug Drugs 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 9
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 7
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 235000013402 health food Nutrition 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 2
- 230000000149 penetrating effect Effects 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000003860 storage Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 24
- 238000000605 extraction Methods 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 4
- 239000000047 product Substances 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 12
- 238000001514 detection method Methods 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 6
- 238000005070 sampling Methods 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
- 238000011084 recovery Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000002955 isolation Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 241000411851 herbal medicine Species 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 241001233914 Chelidonium majus Species 0.000 description 1
- 108010034145 Helminth Proteins Proteins 0.000 description 1
- 241000218180 Papaveraceae Species 0.000 description 1
- 235000016319 Paullinia asiatica Nutrition 0.000 description 1
- 241001529246 Platymiscium Species 0.000 description 1
- 244000093732 Toddalia asiatica Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 229940068560 greater celandine Drugs 0.000 description 1
- 244000000013 helminth Species 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004262 preparative liquid chromatography Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K10/00—Animal feeding-stuffs
- A23K10/30—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- 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)
- A61K36/66—Papaveraceae (Poppy family), e.g. bloodroot
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P33/00—Antiparasitic agents
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
-
- 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
Abstract
The present invention provides a kind of preparation methods of snowpoppy total alkaloid nanoparticle.Preparation step is as follows: a) crushing snowpoppy medicinal part, mixes with alkaline matter, add water and mix, stands overnight；B) pH is adjusted, precipitating is collected, is dried, using alcohol extracting, thickening filtration；C) filtrate sprays into super-critical crystallization kettle and is produced by refrigeration, adverse current；D) bottom nano particle is collected to get snowpoppy total alkaloid nanoparticle.Alkaloid is changed into ion pair mainly to the alkaloid extraction purification in the active component of the medicinal material of snowpoppy by this method, is filtered, and product total alkaloid content reaches 60% or more, and the minimum diameter 500nm of nanoparticle obtained, main body branch is 1-15 μm.Environmental friendly pollution-free, process is succinct, is suitable for mass production.The nanoparticle absorptivity of total alkaloid is high, and bioavilability is high, and will have wider application in feed addictive, drug and field of food.
Description
Technical field
The present invention relates to pharmaceutical technology fields, and in particular to a kind of preparation method of snowpoppy total alkaloid nanoparticle.
Background technique
Natural products and its derivative are one of the main sources of world today's clinical application, and Chinese herbal medicine seek it is new
The precious resources of active component.Alkaloid is the active constituent that a major class is important in Chinese herbal medicine, with huge quantity, complicated
Structure and physiological function abundant.
Traditional alkaloid extracting method generallys use the methods of dipping, reflux, diacolation, decoction, these methods are substantially
Belong to solvent method.With the rapid development of modern separation technology, some new technologies, new method are also applied to mentioning for alkaloid
Taking technique.Such as ultrasound assisted extraction technology, Microwave Assisted Extraction Technique, supercritical liquid extraction technique, these are modern
The application of extractive technique, is expected to solve that energy consumption is high present in traditional extraction process, pollution weight, impurity is more, efficiency is more low asks
Topic, therefore the significant new method of these advantages also becomes the research hotspot of current isolation technics.
Also there are many classical methods, such as solvent extraction, the precipitation method and crystallisation with purification for the separation of alkaloid.To the greatest extent
It is more mature but inefficient to manage these technologies, cost-benefit ratio is lower, and therefore, some advanced separating and purifying technologies are also
It comes into being, quickly grows.In recent years the new technology occurred includes chromatographic separation technology such as preparative liquid chromatography, high-speed counter-current color
Spectrum, gel column chromatography etc., resin adsorption technology macroporous resin adsorption, ion exchange resin absorption, molecular engram, membrane separation technique
Deng.These emerging isolation technics overcome the big and inefficient problem of solvent, energy consumption existing for conventional method, effectively
Ground improves the isolation and purification effect of alkaloid, develops the preparation of alkaloid towards efficient, energy saving, scale direction.
Snowpoppy is Papaveraceae Chelidonieae snowpoppy platymiscium, be China solely belong to, only kind of endemic species, be perennial
Herbaceous plant, is distributed widely in each provinces and regions in the south such as China Zhejiang, Jiangxi, Sichuan, Hunan, and root and rhizome is used as medicine.The country is to blood
In terms of chemical component and pharmacology are more common in the research of water plant, the report for extracting separation and purifying process to its total alkaloid is seldom.
Long Lina solvent covers usage and extracts, and simulates the total alkaloid that the extraction process extraction snowpoppy of tank is organized in industrial production, product
Quality is undesirable, and efficiency is lower.Extraction process (application number or the patent No. of a kind of snowpoppy total alkaloid of Chinese invention patent
CN201010182943.2), method (application number or the patent of a kind of separation greater celandine, snowpoppy or toddalia asiatica total alkaloids
Number CN CN200710098448.1) etc. be all made of conventional extracting mode, it is not high to the recovery rate of alkaloid and time-consuming, be not easy
Industrialization etc..
Summary of the invention
Technical problems to be solved: the object of the present invention is to provide a kind of preparation sides of snowpoppy total alkaloid nanoparticle
Method by changing spe medium polarity, and changes the property of ion pair by the way of the non-medicinal ingredient of overcritical back extraction
Obtain the total alkaloid in snowpoppy.The method is nearly free from waste water, environmentally friendly in the process, and recovery rate is high.
A kind of technical solution: preparation method of snowpoppy total alkaloid nanoparticle, comprising the following steps:
A) snowpoppy medicinal part is crushed, is mixed with alkaline matter, added water and mixed, stood overnight；
B) pH is adjusted, precipitating is collected, is dried, using alcohol extracting, thickening filtration；
C) filtrate sprays into super-critical crystallization kettle and is produced by refrigeration, adverse current；
D) bottom nano particle is collected to get snowpoppy total alkaloid nanoparticle.
Further, in the step a) snowpoppy medicinal part be aerial position, be crushed to partial size be 60 ~
100 mesh.
Further, step a) the neutral and alkali substance is Ca (OH)2、NaHCO3, one of NaOH, KOH or several
Kind, adding proportion is 0.1 ~ 2%；The adding proportion of the water is 30 ~ 60%.
Further, pH is adjusted to 3 ~ 4 in the step b), and the alcohol is 90-95% ethanol solution, and Extracting temperature is
60-72℃。
Further, refrigerated storage temperature is 5 ~ 8 DEG C in the step c), cold preservation time 8-12h；The penetrating mode
It is sprayed for bottom to top, flow velocity 0.01-1L/min.
Further, in the step c) super-critical crystallization kettle condition are as follows: temperature be 15 ~ 25 DEG C, pressure be 15 ~
35MPa, medium CO2Or 2 ~ 10% ethyl alcohol-CO2Fluid-mixing, flow direction are flow velocity 0.5-3L/min from top to bottom.
Further, prepared snowpoppy total alkaloid nanoparticle size is minimum diameter 500nm, and main body branch is
1-15 μm, the content of prepared total alkaloid is greater than 60%.
Further, the snowpoppy total alkaloid nano particle of the preparation can be used for feed addictive, health food and
Drug.
Further, prepared total alkaloid detection method uses HPLC-DAD, condition are as follows: chromatographic column: C18
(200mm × 4.6mm, 5 μm)；Mobile phase: acetonitrile+water=30+70(V/V) (in every 100ml water plus 0.1ml phosphoric acid)；Flow velocity:
1.0ml/min；Column temperature: 35 DEG C；Detection wavelength: 270 nm；Sampling volume: 20 μ l.
The utility model has the advantages that
1. the method for the present invention is nearly free from waste water, environmentally friendly in the process, recovery rate is high.
2. the content that the method for the present invention obtains product total alkaloid is more than 60%, recovery rate is greater than 60%.
3. the alkaloid nano particle of the method for the present invention preparation can be used for feed addictive, health food and medicine field,
It is used especially for the fields such as treatment pet helminth.
Specific embodiment
Embodiment 1
A kind of preparation method of snowpoppy total alkaloid nanoparticle, comprising the following steps:
A) snowpoppy aerial position is crushed to partial size is 100 mesh, with 0.1wt%Ca (OH)2It is mixed that 30wt% water is added in mixing
It is even, it stands overnight；
B) pH to 3 is adjusted, precipitating is collected, is dried, is extracted using 95% ethanol solution, Extracting temperature is 60 DEG C, concentrated
Filter；
C) filtrate passes through 5 DEG C of refrigeration 8h, and adverse current is sprayed into super-critical crystallization kettle and produced, and the mode that sprays into is that bottom is sprayed to top
It penetrates, flow velocity 0.01L/min；The condition of super-critical crystallization kettle are as follows: temperature is 15 DEG C, pressure 15MPa, medium CO2, flowing
Direction is flow velocity 0.5L/min from top to bottom；
D) bottom nano particle is collected to get snowpoppy total alkaloid nanoparticle.
Total alkaloid detection method uses HPLC-DAD, condition are as follows: chromatographic column: C18 (200mm × 4.6mm, 5 μm)；Stream
Dynamic phase: acetonitrile: water=30:70(V/V) (in every 100ml water plus 0.1ml phosphoric acid)；Flow velocity: 1.0ml/min；Column temperature: 35 DEG C；Detection
Wavelength: 270 nm；Sampling volume: 20 μ l.
Prepared snowpoppy total alkaloid nanoparticle size is minimum diameter 500nm, and main body branch is 1-15 μm, institute
The content of the total alkaloid of preparation is 60.5%.
Embodiment 2
A kind of preparation method of snowpoppy total alkaloid nanoparticle, comprising the following steps:
A) snowpoppy aerial position is crushed to partial size is 60 mesh, with 0.5wt%NaHCO3It is mixed that 40wt% water is added in mixing
It is even, it stands overnight；
B) pH to 3 is adjusted, precipitating is collected, is dried, is extracted using 90% ethanol solution, Extracting temperature is 63 DEG C, concentrated
Filter；
C) filtrate passes through 6 DEG C of refrigeration 9h, and adverse current is sprayed into super-critical crystallization kettle and produced, and the mode that sprays into is that bottom is sprayed to top
It penetrates, flow velocity 0.05L/min；The condition of super-critical crystallization kettle are as follows: temperature is 17 DEG C, pressure 20MPa, and medium is 2% ethyl alcohol-
CO2Fluid-mixing, flow direction are flow velocity 1L/min from top to bottom；
D) bottom nano particle is collected to get snowpoppy total alkaloid nanoparticle.
Total alkaloid detection method uses HPLC-DAD, condition are as follows: chromatographic column: C18 (200mm × 4.6mm, 5 μm)；Stream
Dynamic phase: acetonitrile: water=30:70(V/V) (in every 100ml water plus 0.1ml phosphoric acid)；Flow velocity: 1.0ml/min；Column temperature: 35 DEG C；Detection
Wavelength: 270 nm；Sampling volume: 20 μ l.
Prepared snowpoppy total alkaloid nanoparticle size is minimum diameter 500nm, and main body branch is 1-13.5 μm,
The content of prepared total alkaloid is 60.9%.
Embodiment 3
A kind of preparation method of snowpoppy total alkaloid nanoparticle, comprising the following steps:
A) snowpoppy aerial position is crushed to partial size is 80 mesh, is mixed with 1wt%NaOH, and 45wt% water is added and mixes, quiet
It sets overnight；
B) pH to 3.5 is adjusted, precipitating is collected, is dried, is extracted using 95% ethanol solution, Extracting temperature is 65 DEG C, concentrated
Filter；
C) filtrate passes through 6 DEG C of refrigeration 10h, and adverse current is sprayed into super-critical crystallization kettle and produced, and the mode that sprays into is bottom to top
Injection, flow velocity 0.5L/min；The condition of super-critical crystallization kettle are as follows: temperature is 20 DEG C, pressure 25MPa, and medium is 6% ethyl alcohol-
CO2Fluid-mixing, flow direction are flow velocity 1.5L/min from top to bottom；
D) bottom nano particle is collected to get snowpoppy total alkaloid nanoparticle.
Total alkaloid detection method uses HPLC-DAD, condition are as follows: chromatographic column: C18 (200mm × 4.6mm, 5 μm)；Stream
Dynamic phase: acetonitrile: water=30:70(V/V) (in every 100ml water plus 0.1ml phosphoric acid)；Flow velocity: 1.0ml/min；Column temperature: 35 DEG C；Detection
Wavelength: 270 nm；Sampling volume: 20 μ l.
Prepared snowpoppy total alkaloid nanoparticle size is minimum diameter 500nm, and main body branch is 1-13.5 μm,
The content of prepared total alkaloid is 61.7%.
Embodiment 4
A kind of preparation method of snowpoppy total alkaloid nanoparticle, comprising the following steps:
A) snowpoppy aerial position is crushed to partial size is 80 mesh, is mixed with 1.5wt%KOH, and 50wt% water is added and mixes, quiet
It sets overnight；
B) it adjusts pH to 4 and collects precipitating, be dried, extracted using 95% ethanol solution, Extracting temperature is 68 DEG C, thickening filtration；
C) filtrate passes through 7 DEG C of refrigeration 11h, and adverse current is sprayed into super-critical crystallization kettle and produced, and the mode that sprays into is bottom to top
Injection, flow velocity 0.8L/min；The condition of super-critical crystallization kettle are as follows: temperature is 22 DEG C, pressure 30MPa, and medium is 8% ethyl alcohol-
CO2Fluid-mixing, flow direction are flow velocity 2.5L/min from top to bottom；
D) bottom nano particle is collected to get snowpoppy total alkaloid nanoparticle.
Total alkaloid detection method uses HPLC-DAD, condition are as follows: chromatographic column: C18 (200mm × 4.6mm, 5 μm)；Stream
Dynamic phase: acetonitrile: water=30:70(V/V) (in every 100ml water plus 0.1ml phosphoric acid)；Flow velocity: 1.0ml/min；Column temperature: 35 DEG C；Detection
Wavelength: 270 nm；Sampling volume: 20 μ l.
Prepared snowpoppy total alkaloid nanoparticle size is minimum diameter 500nm, and main body branch is 1-14 μm, institute
The content of the total alkaloid of preparation is greater than 61.5%.
Embodiment 5
A kind of preparation method of snowpoppy total alkaloid nanoparticle, comprising the following steps:
A) snowpoppy aerial position is crushed to partial size is 100 mesh, with 0.5wt%Ca (OH)2、0.5wt%NaHCO3、
0.5wt%NaOH, 0.5wt%KOH mixing are added 60wt% water and mix, stands overnight；
B) pH to 3 ~ 4 is adjusted, precipitating is collected, is dried, is extracted using 95% ethanol solution, Extracting temperature is 72 DEG C, concentrated
Filter；
C) filtrate passes through 8 DEG C of refrigeration 12h, and adverse current is sprayed into super-critical crystallization kettle and produced, and the mode that sprays into is bottom to top
Injection, flow velocity 1L/min；The condition of super-critical crystallization kettle are as follows: temperature is 25 DEG C, pressure 35MPa, and medium is 10% ethyl alcohol-
CO2Fluid-mixing, flow direction are flow velocity 3L/min from top to bottom；
D) bottom nano particle is collected to get snowpoppy total alkaloid nanoparticle.
Total alkaloid detection method uses HPLC-DAD, condition are as follows: chromatographic column: C18 (200mm × 4.6mm, 5 μm)；Stream
Dynamic phase: acetonitrile: water=30:70(V/V) (in every 100ml water plus 0.1ml phosphoric acid)；Flow velocity: 1.0ml/min；Column temperature: 35 DEG C；Detection
Wavelength: 270 nm；Sampling volume: 20 μ l.
Prepared snowpoppy total alkaloid nanoparticle size is minimum diameter 500nm, and main body branch is 1-15 μm, institute
The content of the total alkaloid of preparation is 61.5%.
Claims (8)
1. a kind of preparation method of snowpoppy total alkaloid nanoparticle, it is characterised in that: the following steps are included:
A) snowpoppy medicinal part is crushed, is mixed with alkaline matter, added water and mixed, stood overnight；
B) pH is adjusted, precipitating is collected, is dried, using alcohol extracting, thickening filtration；
C) filtrate sprays into super-critical crystallization kettle and is produced by refrigeration, adverse current；
D) bottom nano particle is collected to get snowpoppy total alkaloid nanoparticle.
2. a kind of preparation method of snowpoppy total alkaloid nanoparticle according to claim 1, it is characterised in that: described
Step a) in snowpoppy medicinal part be aerial position, be crushed to partial size be 60 ~ 100 mesh.
3. a kind of preparation method of snowpoppy total alkaloid nanoparticle according to claim 1, it is characterised in that: described
Step a) neutral and alkali substance be Ca (OH)2、NaHCO3, one or more of NaOH, KOH, adding proportion is 0.1 ~ 2%；Institute
The adding proportion for stating water is 30 ~ 60%.
4. a kind of preparation method of snowpoppy total alkaloid nanoparticle according to claim 1, it is characterised in that: described
Step b) in pH be adjusted to 3 ~ 4, the alcohol is 90-95% ethanol solution, and Extracting temperature is 60-72 DEG C.
5. a kind of preparation method of snowpoppy total alkaloid nanoparticle according to claim 1, it is characterised in that: described
Step c) in refrigerated storage temperature be 5 ~ 8 DEG C, cold preservation time 8-12h；The penetrating mode is that bottom is sprayed to top, flow velocity
For 0.01-1L/min.
6. a kind of preparation method of snowpoppy total alkaloid nanoparticle according to claim 1, it is characterised in that: described
Step c) in super-critical crystallization kettle condition are as follows: temperature be 15 ~ 25 DEG C, pressure be 15 ~ 35MPa, medium CO2Or 2 ~ 10%
Ethyl alcohol-CO2Fluid-mixing, flow direction are flow velocity 0.5-3L/min from top to bottom.
7. a kind of preparation method of snowpoppy total alkaloid nanoparticle according to claim 1, it is characterised in that: made
Standby snowpoppy total alkaloid nanoparticle size is minimum diameter 500nm, and main body branch is 1-15 μm, prepared total biology
The content of alkali is greater than 60%.
8. a kind of preparation method of snowpoppy total alkaloid nanoparticle according to claim 7, it is characterised in that: described
The snowpoppy total alkaloid nano particle of preparation can be used for feed addictive, health food and drug.
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| CN110484367A (en) * | 2019-08-27 | 2019-11-22 | 广东省金叶科技开发有限公司 | A kind of preparation method of nicotine essence particle |
| WO2020211264A1 (en) * | 2019-04-19 | 2020-10-22 | 南京康齐生物科技有限公司 | Method for preparing nanoparticles of total eomecon chionantha alkaloid |
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| CN101953898A (en) * | 2010-05-26 | 2011-01-26 | 南京泽朗医药科技有限公司 | Process for extracting Eomecon chionantha Hance total alkaloids |
| CN105311119A (en) * | 2014-08-04 | 2016-02-10 | 上海医药工业研究院 | Refined rhizoma corydalis decumbentis total alkaloid product, preparation method thereof, pharmaceutical composition and application of refined rhizoma corydalis decumbentis total alkaloid product and pharmaceutical composition |
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| CN1292750C (en) * | 2003-06-02 | 2007-01-03 | 张平 | Total alkaloid composition from plant and its pharmaceutical preparation |
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| CN110141605A (en) * | 2019-04-19 | 2019-08-20 | 南京康齐生物科技有限公司 | A kind of preparation method of snowpoppy total alkaloid nanoparticle |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020211264A1 (en) * | 2019-04-19 | 2020-10-22 | 南京康齐生物科技有限公司 | Method for preparing nanoparticles of total eomecon chionantha alkaloid |
| CN110484367A (en) * | 2019-08-27 | 2019-11-22 | 广东省金叶科技开发有限公司 | A kind of preparation method of nicotine essence particle |
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