CN110393675A - A kind of chlorophyll freeze-dried powder and preparation method thereof - Google Patents

A kind of chlorophyll freeze-dried powder and preparation method thereof Download PDF

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Publication number
CN110393675A
CN110393675A CN201910750984.8A CN201910750984A CN110393675A CN 110393675 A CN110393675 A CN 110393675A CN 201910750984 A CN201910750984 A CN 201910750984A CN 110393675 A CN110393675 A CN 110393675A
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freeze
chlorophyll
dried powder
plate layer
water phase
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赵月美
邱晓颖
肖彤
田秀菊
董晓光
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Guangzhou Meikou Biotechnology Co Ltd
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Guangzhou Meikou Biotechnology Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0216Solid or semisolid forms
    • A61K8/022Powders; Compacted Powders
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/494Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
    • A61K8/4946Imidazoles or their condensed derivatives, e.g. benzimidazoles
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/58Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/735Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/88Polyamides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84Products or compounds obtained by lyophilisation, freeze-drying

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  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
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Abstract

The present invention relates to beautification product field, a kind of chlorophyll freeze-dried powder and preparation method thereof is provided, for improving the quality of chlorophyll freeze-dried powder.A kind of chlorophyll freeze-dried powder provided by the invention, the formula of the freeze-dried powder include: chlorophyll 0.05 ~ 0.15%, excipient 8 ~ 9.25%, water phase 90.75 ~ 91.85%.It is carried out preferably by the content to chlorophyll, excipient, available surfacing, uniform color, viscosity is smaller, the freeze-dried powder of greater homogeneity.

Description

A kind of chlorophyll freeze-dried powder and preparation method thereof
Technical field
The present invention relates to beautification product fields, and in particular to a kind of chlorophyll freeze-dried powder and preparation method thereof.
Background technique
Beauty industry has increased a new varieties newly again in recent years, that is, freeze-dried powder.Due to much having good beauty The product of effect such as polypeptide, polysaccharide, nucleic acid, protein isoreactivity ingredient are easy to inactivate, and are difficult to protect in common beauty product Their bioactivity is held, so, a part U.S. industry personage has devised this dose of freeze-dried powder using the freeze drying technology on drug The product of type.Freeze-dried powder can keep the activity of functional component well, since drying carries out under vacuum conditions, for some easy The substance of oxidation plays a very good protection.Product water content after freeze-drying is very low, improves the stability of product, Contaminated chance reduces, and facilitates the pot-life that transport also extends product.But freeze-dried powder quality in the market is irregular not Together, it is the product structure ratio using polypeptide, polysaccharide, nucleic acid, protein isoreactivity ingredient as effect additive that the product to do very well is also mostly It is more single.
Scientists had found the effect and effect of chlorophyll, SOD, P4-D1 and 2-O-GL that chlorophyll contains in recent years Equal anticancer components, have good antitumaous effect.SOD is a kind of powerful antioxidants, is discharged in the metabolic process of human body Harmful superoxide radical, they can not only destroy cell, even more aging and cause the arch-criminal of tumour, and SOD energy Protect body from the infringement of oxygen radical, antiradical activities are thousands of times of VA and VE, and P4-D1, then can repair The cell of damage resists the toxicity of carcinogen.Medical research shows that chlorophyll has significant liver protecting, hematopoiesis, solution Poison anticancer, delays senescence, prevents gene mutation, promote wound healing, deodorization, improve constipation, analgesic, reduce the function such as cholesterol Effect can also provide vitamin, maintain the effects of activity of enzyme.The product that many health products Co., Ltd all have developed chlorophyll supplies People take.The beauty product of chlorophyll class also continues to bring out, but shows all general.
Currently, the effect of freeze-drying beauty product in the market ingredient is usually the ingredients such as polypeptide, polysaccharide, nucleic acid, protein, Product structure is relatively simple.The freeze-dried powder that chlorophyll how is obtained using freeze drying technology is a technical problem to be solved urgently.
Summary of the invention
Present invention solves the technical problem that improve the quality of chlorophyll freeze-dried powder, provide a kind of chlorophyll freeze-dried powder and its Preparation method.
In order to solve the above technical problem, the present invention provides technical solution are as follows:
A kind of chlorophyll freeze-dried powder, the formula of the freeze-dried powder include: chlorophyll 0.05 ~ 0.15%, excipient 8 ~ 9.25%, water phase 90.75~91.85%。
It is soluble in the aqueous phase after chlorophyll is mixed with excipient, uniformly mixed freeze-drying can obtain the preferable freeze-dried powder of condition.
It being carried out preferably by the content to chlorophyll, excipient, available surfacing, uniform color, viscosity is smaller, The freeze-dried powder of greater homogeneity.
Preferably, the formula of the freeze-dried powder includes: chlorophyll 0.1%, excipient 9.15%, water phase 90.75%.
Preferably, the excipient includes mannitol, sucrose, trehalose, glucose, sodium chloride, lactose, histidine, essence Propylhomoserin, glycine, hyaluronic acid, polyglutamic acid are one such or several.The quality of excipient effects freeze-dried powder, by tax The content of shape agent carries out preferably, the freeze-dried powder of available high-quality.
Preferably, the water phase include water, PEG-400, TW-20 it is one of or several.
Preferably, the chlorophyll 0.05 ~ 0.15%, mannitol 3 ~ 5%, trehalose 3 ~ 5%, polyglutamic acid 0.4 ~ 0.5%, thoroughly Bright matter acid 0.1 ~ 0.2%, lysine 0.1 ~ 0.3%, arginine 0.2 ~ 0.3%, histidine 0.1 ~ 0.2%, water 90.8 ~ 91.85%.It is right The excipient of chlorophyll carries out preferably, the freeze-dried powder of available higher quality.
A kind of preparation method of chlorophyll freeze-dried powder, including
S11. excipient is added in water phase, 200 ~ 500 turns/min stirring and dissolving is complete, obtains mixed liquor;
S12. it sterilizes after mixed liquor being filtered, chlorophyll is added, obtains mother liquor;
S13. mother liquor is freeze-dried to obtain freeze-dried powder.
Preferably, the excipient in the S11 step includes mannitol, trehalose, polyglutamic acid, hyaluronic acid, relies ammonia Acid, arginine, histidine, it is described to include: by excipient addition water phase
S111. mannitol, trehalose, polyglutamic acid, hyaluronic acid are sequentially added in water phase, 200 ~ 500 turns/min stirring is molten Solution is complete;
S112. arginine, histidine, lysine are added.
Preferably, the water phase is water.
Preferably, the filtering are as follows: with 0.22 μm of membrane filtration at -0.09 ~ 0.1MPa;The sterilizing are as follows: will filter Liquid is under 110 ~ 130 degrees Celsius, 10 ~ 30min of high-temp steam sterilizing;Temperature≤45 degree Celsius when the addition chlorophyll.
Preferably, the freeze-drying are as follows: -35 ~ -30 DEG C of plate layer temperature of setting, 5 ~ 6h of pre-freeze time;After pre-freeze, When rear cabinet temperature reaches -50 ~ -40 DEG C, start to vacuumize, be started to warm up after vacuum degree drops to 0.6 ~ 0.8mbar;Once Drying stage first sets -20 ~ -10 DEG C, 8 ~ 12h of plate layer temperature, then resets -5 ~ 5 DEG C of plate layer temperature, continue 1 ~ 3h;Parsing Drying stage sets 8 ~ 15 DEG C, 1 ~ 3h of duration of plate layer temperature, resets 20 ~ 40 DEG C of plate layer temperature, continue 5 ~ 8h.
Compared with prior art, the device have the advantages that are as follows: carried out by content to chlorophyll, excipient excellent Choosing, available surfacing, uniform color, viscosity is smaller, the freeze-dried powder of greater homogeneity;The pH value of freeze-dried powder is the same as skin It is close, it is more mild to skin, easily by percutaneous absorption.
Specific embodiment
Following implementation column is to further explanation of the invention, is not limitation of the present invention.
Embodiment 1
A kind of chlorophyll freeze-dried powder, the formula of the freeze-dried powder include: chlorophyll 0.1%, mannitol 3%, trehalose 5%, poly- paddy Propylhomoserin 0.5%, hyaluronic acid 0.2%, lysine 0.05%, arginine 0.3%, histidine 0.1%, water 90.75%.
A kind of preparation method of chlorophyll freeze-dried powder, comprising:
S111. mannitol, trehalose, polyglutamic acid, hyaluronic acid are sequentially added in water phase, 200 ~ 500 turns/min stirring is molten Solution is complete;
S112. arginine, histidine, lysine are added;
S11.200 ~ 500 turn/min stirring and dissolving is complete, obtains mixed liquor;
S12. mixed liquor is stirred evenly, with 0.22 μm of membrane filtration at -0.09 ~ 0.1MPa;Filtrate is taken, filtrate is existed Under 120 degrees Celsius, high-temp steam sterilizing 20min after cooling when system temperature≤45 degree Celsius, is added chlorophyll, stirs evenly, Obtain mother liquor;
S13. mother liquor is freeze-dried to obtain freeze-dried powder.The freeze-drying are as follows: -35 DEG C of temperature of plate layer of setting, pre-freeze time 5h; After pre-freeze, when rear cabinet temperature reaches -45 DEG C, starts to vacuumize, be started to warm up after vacuum degree drops to 0.8mbar; The primary drying stage first sets -15 DEG C of temperature of plate layer, then 10h resets 0 DEG C of plate layer temperature, continues 2h;Parsing-desiccation rank Section sets 10 DEG C, duration 1.5h of plate layer temperature, resets 30 DEG C of plate layer temperature, continues 7h.
It is soluble in the aqueous phase after chlorophyll is mixed with excipient, uniformly mixed freeze-drying can obtain the preferable freeze-dried powder of condition.Pass through The content of chlorophyll, excipient is carried out preferably, available surfacing, uniform color, viscosity is smaller, the jelly of greater homogeneity Dry powder.The quality of excipient effects freeze-dried powder carries out the preferably freeze-drying of available high-quality by the content to excipient Powder.The excipient of chlorophyll is carried out preferably, the freeze-dried powder of available higher quality.
Embodiment 2
A kind of chlorophyll freeze-dried powder, the formula of the freeze-dried powder include: chlorophyll 0.15%, mannitol 4%, trehalose 3%, poly- paddy Propylhomoserin 0.4%, hyaluronic acid 0.2%, lysine 0.1%, arginine 0.2%, histidine 0.1%, water 91.85%.
A kind of preparation method of chlorophyll freeze-dried powder, comprising:
S111. mannitol, trehalose, polyglutamic acid, hyaluronic acid are sequentially added in water phase, 200 ~ 500 turns/min stirring is molten Solution is complete;
S112. arginine, histidine, lysine are added;
S11.200 ~ 500 turn/min stirring and dissolving is complete, obtains mixed liquor;
S12. mixed liquor is stirred evenly, with 0.22 μm of membrane filtration at -0.09 ~ 0.1MPa;Filtrate is taken, filtrate is existed Under 120 degrees Celsius, high-temp steam sterilizing 20min after cooling when system temperature≤45 degree Celsius, is added chlorophyll, stirs evenly, Obtain mother liquor;
S13. mother liquor is freeze-dried to obtain freeze-dried powder.The freeze-drying are as follows: -35 DEG C of temperature of plate layer of setting, pre-freeze time 6h; After pre-freeze, when rear cabinet temperature reaches -45 DEG C, starts to vacuumize, be started to warm up after vacuum degree drops to 0.8mbar; The primary drying stage first sets -15 DEG C of temperature of plate layer, then 10h resets 0 DEG C of plate layer temperature, continues 2h;Parsing-desiccation rank Section sets 10 DEG C, duration 1.5h of plate layer temperature, resets 30 DEG C of plate layer temperature, continues 6h.
Embodiment 3
A kind of chlorophyll freeze-dried powder, a kind of chlorophyll freeze-dried powder, the formula of the freeze-dried powder include: chlorophyll 0.05%, sweet dew Alcohol 5%, trehalose 3%, polyglutamic acid 0.4%, hyaluronic acid 0.1%, lysine 0.1%, arginine 0.2%, histidine 0.1%, water 91.05%。
A kind of preparation method of chlorophyll freeze-dried powder, comprising:
S111. mannitol, trehalose, polyglutamic acid, hyaluronic acid are sequentially added in water phase, 200 ~ 500 turns/min stirring is molten Solution is complete;
S112. arginine, histidine, lysine are added;
S11.200 ~ 500 turn/min stirring and dissolving is complete, obtains mixed liquor;
S12. mixed liquor is stirred evenly, with 0.22 μm of membrane filtration at -0.09 ~ 0.1MPa;Filtrate is taken, filtrate is existed Under 120 degrees Celsius, high-temp steam sterilizing 20min after cooling when system temperature≤45 degree Celsius, is added chlorophyll, stirs evenly, Obtain mother liquor;
S13. mother liquor is freeze-dried to obtain freeze-dried powder.The freeze-drying are as follows: -30 DEG C of temperature of plate layer of setting, pre-freeze time 5h; After pre-freeze, when rear cabinet temperature reaches -45 DEG C, starts to vacuumize, be started to warm up after vacuum degree drops to 0.8mbar; The primary drying stage first sets -15 DEG C of temperature of plate layer, then 9h resets 0 DEG C of plate layer temperature, continues 2h;Parsing-desiccation rank Section sets 10 DEG C, duration 1.5h of plate layer temperature, resets 30 DEG C of plate layer temperature, continues 5h.
Embodiment 4
A kind of chlorophyll freeze-dried powder, the formula of the freeze-dried powder include: chlorophyll 0.15%, mannitol 5%, trehalose 3%, poly- paddy Propylhomoserin 0.4%, hyaluronic acid 0.2%, lysine 0.1%, arginine 0.2%, histidine 0.2%, water 90.75%.
A kind of preparation method of chlorophyll freeze-dried powder, comprising:
S111. mannitol, trehalose, polyglutamic acid, hyaluronic acid are sequentially added in water phase, 200 ~ 500 turns/min stirring is molten Solution is complete;
S112. arginine, histidine, lysine are added;
S11.200 ~ 500 turn/min stirring and dissolving is complete, obtains mixed liquor;
S12. mixed liquor is stirred evenly, with 0.22 μm of membrane filtration at -0.09 ~ 0.1MPa;Filtrate is taken, filtrate is existed Under 120 degrees Celsius, high-temp steam sterilizing 20min after cooling when system temperature≤45 degree Celsius, is added chlorophyll, stirs evenly, Obtain mother liquor;
S13. mother liquor is freeze-dried to obtain freeze-dried powder.The freeze-drying are as follows: -35 DEG C of temperature of plate layer of setting, pre-freeze time 5h; After pre-freeze, when rear cabinet temperature reaches -45 DEG C, starts to vacuumize, be started to warm up after vacuum degree drops to 0.8mbar; The primary drying stage first sets -15 DEG C of temperature of plate layer, then 10h resets 0 DEG C of plate layer temperature, continues 2h;Parsing-desiccation rank Section sets 10 DEG C, duration 1.5h of plate layer temperature, resets 30 DEG C of plate layer temperature, continues 7h.
Embodiment 5
A kind of chlorophyll freeze-dried powder, the formula of the freeze-dried powder include: chlorophyll 0.1%, mannitol 3%, sucrose 2%, lactose 2%, Glucose 1%, polyglutamic acid 0.5%, hyaluronic acid 0.2%, lysine 0.05%, arginine 0.3%, histidine 0.1%, water 90.75%。
A kind of preparation method of chlorophyll freeze-dried powder, comprising:
S111. mannitol, sucrose, lactose, glucose, polyglutamic acid, hyaluronic acid are sequentially added in water phase, 200 ~ 500 turns/ Min stirring and dissolving is complete;
S112. arginine, histidine, lysine are added;
S11.200 ~ 500 turn/min stirring and dissolving is complete, obtains mixed liquor;
S12. mixed liquor is stirred evenly, with 0.22 μm of membrane filtration at -0.09 ~ 0.1MPa;Filtrate is taken, filtrate is existed Under 120 degrees Celsius, high-temp steam sterilizing 20min after cooling when system temperature≤45 degree Celsius, is added chlorophyll, stirs evenly, Obtain mother liquor;
S13. mother liquor is freeze-dried to obtain freeze-dried powder.The freeze-drying are as follows: -35 DEG C of temperature of plate layer of setting, pre-freeze time 5h; After pre-freeze, when rear cabinet temperature reaches -45 DEG C, starts to vacuumize, be started to warm up after vacuum degree drops to 0.8mbar; The primary drying stage first sets -15 DEG C of temperature of plate layer, then 10h resets 0 DEG C of plate layer temperature, continues 2h;Parsing-desiccation rank Section sets 10 DEG C, duration 1.5h of plate layer temperature, resets 30 DEG C of plate layer temperature, continues 7h.
Embodiment 6
A kind of chlorophyll freeze-dried powder, the formula of the freeze-dried powder include: chlorophyll 0.1%, mannitol 3%, sodium chloride 5%, poly- paddy Propylhomoserin 0.5%, hyaluronic acid 0.2%, lysine 0.05%, arginine 0.3%, histidine 0.1%, water 90.75%.
A kind of preparation method of chlorophyll freeze-dried powder, comprising:
S111. mannitol, sodium chloride, polyglutamic acid, hyaluronic acid are sequentially added in water phase, 200 ~ 500 turns/min stirring is molten Solution is complete;
S112. arginine, histidine, lysine are added;
S11.200 ~ 500 turn/min stirring and dissolving is complete, obtains mixed liquor;
S12. mixed liquor is stirred evenly, with 0.22 μm of membrane filtration at -0.09 ~ 0.1MPa;Filtrate is taken, filtrate is existed Under 120 degrees Celsius, high-temp steam sterilizing 20min after cooling when system temperature≤45 degree Celsius, is added chlorophyll, stirs evenly, Obtain mother liquor;
S13. mother liquor is freeze-dried to obtain freeze-dried powder.The freeze-drying are as follows: -35 DEG C of temperature of plate layer of setting, pre-freeze time 5h; After pre-freeze, when rear cabinet temperature reaches -45 DEG C, starts to vacuumize, be started to warm up after vacuum degree drops to 0.8mbar; The primary drying stage first sets -15 DEG C of temperature of plate layer, then 10h resets 0 DEG C of plate layer temperature, continues 2h;Parsing-desiccation rank Section sets 10 DEG C, duration 1.5h of plate layer temperature, resets 30 DEG C of plate layer temperature, continues 7h.
Embodiment 7
A kind of chlorophyll freeze-dried powder, the formula of the freeze-dried powder include: chlorophyll 0.1%, mannitol 3%, trehalose 5%, poly- paddy Propylhomoserin 0.5%, hyaluronic acid 0.2%, lysine 0.05%, arginine 0.3%, glycine 0.1%, water 90.75%.
A kind of preparation method of chlorophyll freeze-dried powder, comprising:
S111. mannitol, trehalose, polyglutamic acid, hyaluronic acid are sequentially added in water phase, 200 ~ 500 turns/min stirring is molten Solution is complete;
S112. arginine, glycine, lysine are added;
S11.200 ~ 500 turn/min stirring and dissolving is complete, obtains mixed liquor;
S12. mixed liquor is stirred evenly, with 0.22 μm of membrane filtration at -0.09 ~ 0.1MPa;Filtrate is taken, filtrate is existed Under 120 degrees Celsius, high-temp steam sterilizing 20min after cooling when system temperature≤45 degree Celsius, is added chlorophyll, stirs evenly, Obtain mother liquor;
S13. mother liquor is freeze-dried to obtain freeze-dried powder.The freeze-drying are as follows: -35 DEG C of temperature of plate layer of setting, pre-freeze time 5h; After pre-freeze, when rear cabinet temperature reaches -45 DEG C, starts to vacuumize, be started to warm up after vacuum degree drops to 0.8mbar; The primary drying stage first sets -15 DEG C of temperature of plate layer, then 10h resets 0 DEG C of plate layer temperature, continues 2h;Parsing-desiccation rank Section sets 10 DEG C, duration 1.5h of plate layer temperature, resets 30 DEG C of plate layer temperature, continues 7h.
Embodiment 8
A kind of chlorophyll freeze-dried powder, the formula of the freeze-dried powder include: chlorophyll 0.1%, mannitol 3%, trehalose 5%, poly- paddy Propylhomoserin 0.5%, hyaluronic acid 0.2%, lysine 0.05%, arginine 0.3%, histidine 0.1%, water 90.75%.
A kind of preparation method of chlorophyll freeze-dried powder, comprising:
S111. mannitol, trehalose, polyglutamic acid, hyaluronic acid are sequentially added in water phase, 200 ~ 500 turns/min stirring is molten Solution is complete;
S112. arginine, histidine, lysine are added;
S11.200 ~ 500 turn/min stirring and dissolving is complete, obtains mixed liquor;
S12. mixed liquor is stirred evenly, with 0.22 μm of membrane filtration at -0.09 ~ 0.1MPa;Filtrate is taken, filtrate is existed Under 120 degrees Celsius, high-temp steam sterilizing 20min after cooling when system temperature≤45 degree Celsius, is added chlorophyll, stirs evenly, Obtain mother liquor;
S13. mother liquor is freeze-dried to obtain freeze-dried powder.The freeze-drying are as follows: -35 DEG C of temperature of plate layer of setting, pre-freeze time 5h; After pre-freeze, when rear cabinet temperature reaches -35 DEG C, starts to vacuumize, be started to warm up after vacuum degree drops to 0.8mbar; The primary drying stage first sets -15 DEG C of temperature of plate layer, then 10h resets 0 DEG C of plate layer temperature, continues 2h;Parsing-desiccation rank Section sets 10 DEG C, duration 1.5h of plate layer temperature, resets 20 DEG C of plate layer temperature, continues 7h.
Comparative example 1
Comparative example 1 with embodiment 1 the difference is that, a kind of chlorophyll freeze-dried powder, the formula of the freeze-dried powder includes: that leaf is green Element 0.1%, mannitol 9.15%, water 90.75%.A kind of preparation method of chlorophyll freeze-dried powder, comprising: mannitol is added S111. In water phase, stirring and dissolving is complete;S11.200 ~ 500 turn/min stirring and dissolving is complete, obtains mixed liquor.Remaining is the same as embodiment 1.
Comparative example 2
Comparative example 2 with embodiment 1 the difference is that, a kind of chlorophyll freeze-dried powder, the formula of the freeze-dried powder includes: that leaf is green Element 0.1%, trehalose 9.15%, water 90.75%.A kind of preparation method of chlorophyll freeze-dried powder, comprising: trehalose is added S111. In water phase, stirring and dissolving is complete;S11.200 ~ 500 turn/min stirring and dissolving is complete, obtains mixed liquor.Remaining is the same as embodiment 1.
Comparative example 3
Comparative example 3 with embodiment 1 the difference is that, the formula of the freeze-dried powder includes: chlorophyll 0.1%, arginine 3.3%, Lysine 3.15%, histidine 3%, water 90.75%.A kind of preparation method of chlorophyll freeze-dried powder, comprising: S111. by arginine, Lysine, histidine are added in water phase, and stirring and dissolving is complete;S11.200 ~ 500 turn/min stirring and dissolving is complete, is mixed Liquid.Remaining is the same as embodiment 1
Experimental example 1
The performance of testing example 1 ~ 8 and comparative example 1 ~ 3, as shown in table 1.
1 freeze-dried powder performance of table
As known from Table 1, the appearance of embodiment and comparative example, dissolubility are substantially qualification, show the figuration using the application The quality of product, but the friability > 1% of the freeze-dried powder in comparative example 1 ~ 3, freeze-dried powder can be effectively ensured with chlorophyll compounding for agent It is frangible, influence product appearance.The formula and preparation method of embodiment 1 easily absorb skin, and product appearance is more exquisite.
Experimental example 2
Freeze-dried powder in embodiment 1 ~ 7 and comparative example 1 ~ 3 is measured to the removal rate of free radical using spectrophotometry.Such as 2 institute of table Show.
2 free radical removal rate of table
From table 2 it can be seen that the freeze-dried powder in embodiment 1 ~ 4 has preferable elimination effect to hydroxyl radical free radical.In comparative example Excipient has biggish difference with the excipient in embodiment, and content also has difference, and the effect for removing free radical is relatively poor.
Above-listed detailed description is illustrating for possible embodiments of the present invention, and above embodiments are not to limit this The scope of the patents of invention, all equivalence enforcements or change without departing from carried out by the present invention, is intended to be limited solely by the scope of the patents of this case.

Claims (10)

1. a kind of chlorophyll freeze-dried powder, which is characterized in that the formula of the freeze-dried powder includes: chlorophyll 0.05 ~ 0.15%, figuration Agent 8 ~ 9.25%, water phase 90.75 ~ 91.85%.
2. a kind of chlorophyll freeze-dried powder according to claim 1, which is characterized in that the formula of the freeze-dried powder includes: leaf Green plain 0.1%, excipient 9.15%, water phase 90.75%.
3. a kind of chlorophyll freeze-dried powder according to claim 1, which is characterized in that the excipient includes mannitol, sugarcane Sugar, trehalose, glucose, sodium chloride, lactose, histidine, arginine, glycine, hyaluronic acid, polyglutamic acid are one such Or it is several.
4. a kind of chlorophyll freeze-dried powder according to claim 1, which is characterized in that the water phase include water, PEG-400, TW-20's is one of or several.
5. a kind of chlorophyll freeze-dried powder according to claim 1, which is characterized in that the chlorophyll 0.05 ~ 0.15%, it is sweet Reveal alcohol 3 ~ 5%, trehalose 3 ~ 5%, polyglutamic acid 0.4 ~ 0.5%, hyaluronic acid 0.1 ~ 0.2%, lysine 0.1 ~ 0.3%, arginine 0.2 ~ 0.3%, histidine 0.1 ~ 0.2%, water 90.8 ~ 91.85%.
6. a kind of preparation method of chlorophyll freeze-dried powder, which is characterized in that including
S11. excipient is added in water phase, 200 ~ 500 turns/min stirring and dissolving is complete, obtains mixed liquor;
S12. it sterilizes after mixed liquor being filtered, chlorophyll is added, obtains mother liquor;
S13. mother liquor is freeze-dried to obtain freeze-dried powder.
7. a kind of chlorophyll freeze-dried powder according to claim 1, which is characterized in that the excipient packet in the S11 step Mannitol, trehalose, polyglutamic acid, hyaluronic acid, lysine, arginine, histidine are included, it is described that water phase packet is added in excipient It includes:
S111. mannitol, trehalose, polyglutamic acid, hyaluronic acid are sequentially added in water phase, 200 ~ 500 turns/min stirring is molten Solution is complete;
S112. arginine, histidine, lysine are added.
8. a kind of chlorophyll freeze-dried powder according to claim 1, which is characterized in that the water phase is water.
9. a kind of chlorophyll freeze-dried powder according to claim 1, which is characterized in that the filtering are as follows: -0.09 ~ With 0.22 μm of membrane filtration under 0.1MPa;The sterilizing are as follows: by filtrate 110 ~ 130 degrees Celsius of lower high-temp steam sterilizings 10 ~ 30min;Temperature≤45 degree Celsius when the addition chlorophyll.
10. a kind of chlorophyll freeze-dried powder according to claim 1, which is characterized in that the freeze-drying are as follows: setting plate layer Temperature -35 ~ -30 DEG C, 5 ~ 6h of pre-freeze time;After pre-freeze, when rear cabinet temperature reaches -50 ~ -40 DEG C, start to vacuumize, when Vacuum degree starts to warm up after dropping to 0.6 ~ 0.8mbar;The primary drying stage first sets -20 ~ -10 DEG C, 8 ~ 12h of plate layer temperature, Then -5 ~ 5 DEG C of plate layer temperature is reset, 1 ~ 3h is continued;The parsing-desiccation stage, 8 ~ 15 DEG C of plate layer temperature of setting, the duration 1 ~ 3h resets 20 ~ 40 DEG C of plate layer temperature, continues 5 ~ 8h.
CN201910750984.8A 2019-08-14 2019-08-14 A kind of chlorophyll freeze-dried powder and preparation method thereof Pending CN110393675A (en)

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CN114533570A (en) * 2020-11-27 2022-05-27 广州美蔻生物科技有限公司 Fullerene freeze-dried powder with repairing and anti-aging effects
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