CN115554365A - Freeze-dried preparation containing gastrodia elata extract and preparation method and application thereof - Google Patents

Freeze-dried preparation containing gastrodia elata extract and preparation method and application thereof Download PDF

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CN115554365A
CN115554365A CN202110753111.XA CN202110753111A CN115554365A CN 115554365 A CN115554365 A CN 115554365A CN 202110753111 A CN202110753111 A CN 202110753111A CN 115554365 A CN115554365 A CN 115554365A
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extract
gastrodia elata
freeze
preparation
binder
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李和伟
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/88—Liliopsida (monocotyledons)
    • A61K36/898—Orchidaceae (Orchid family)
    • A61K36/8988—Gastrodia
    • 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
    • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/385—Concentrates of non-alcoholic beverages
    • A23L2/39—Dry compositions
    • 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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K45/00—Medicinal preparations containing active ingredients not provided for in groups A61K31/00 - A61K41/00
    • A61K45/06—Mixtures of active ingredients without chemical characterisation, e.g. antiphlogistics and cardiaca
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9794—Liliopsida [monocotyledons]
    • 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
    • A61K9/0012—Galenical forms characterised by the site of application
    • A61K9/0053—Mouth and digestive tract, i.e. intraoral and peroral administration
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/10—Laxatives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/14—Prodigestives, e.g. acids, enzymes, appetite stimulants, antidyspeptics, tonics, antiflatulents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P13/00—Drugs for disorders of the urinary system
    • A61P13/12—Drugs for disorders of the urinary system of the kidneys
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P7/00—Drugs for disorders of the blood or the extracellular fluid
    • A61P7/06—Antianaemics
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/08—Anti-ageing preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00—Preparations for care of the hair
    • A61Q5/02—Preparations for cleaning the hair
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q7/00—Preparations for affecting hair growth
    • 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
    • A61K2236/30—Extraction of the material
    • A61K2236/31—Extraction of the material involving untreated material, e.g. fruit juice or sap obtained from fresh plants
    • 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
    • A61K2236/51—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
    • A61K2236/55—Liquid-liquid separation; Phase separation
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84—Products or compounds obtained by lyophilisation, freeze-drying
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The invention provides a freeze-dried preparation containing a gastrodia elata extract, wherein the gastrodia elata extract accounts for 0.004wt% -95wt% of the freeze-dried preparation in percentage by mass, and the gastrodia elata extract contains at least one of iridoid and glycosides thereof, lignan glycosides, phenylethanoid glycosides, flavonoids and alkaloids. The freeze-dried preparation containing the gastrodia elata extract has the advantages of high disintegration speed, short dissolution time and high dissolution speed, and the freeze-dried preparation is high in drug loading capacity. The obtained rhizoma Gastrodiae extract has good pharmacological properties, and can be added into lyophilized preparation to retain good pharmacological properties.

Description

Freeze-dried preparation containing gastrodia elata extract and preparation method and application thereof
Technical Field
The invention relates to the field of freeze-dried preparations, in particular to a freeze-dried preparation containing a gastrodia elata extract, and a preparation method and application thereof.
Background
The rhizoma Gastrodiae is rhizoma Gastrodiae or rhizoma Gastrodiae belonging to Orobanchaceae, and has effects of invigorating kidney yang, replenishing essence and blood, and loosening bowel to relieve constipation. Modern pharmacological research shows that the main components of rhizoma Gastrodiae include phenylethanoid glycosides, iridoids, their glycosides, lignin, polysaccharides, etc. In the first pharmacopoeia of China, 2015, the production area of gastrodia elata is processed by digging in spring when seedlings come out of the soil or before frozen soil in autumn, removing stem tips, cutting into sections and drying in the sun. The ancient books are relatively simple in related records, as in famous physicians' book: collected in the shade five months and five days; "Shu Ben Cao" (Shu materia Medica) year: three and four inches of the root is dug in March and April, and the central one is cut, and the root is dried in the shade after the rope is threaded. August and Happy; "materia Medica Mongolian fish pot": "pluck dryly at noon"; the book Ben Cao Pin Hui Jing Yao (materia Medica essence essences): roots are taken in March and May for five days and dried in the shade, so that the ancient gastrodia elata is directly dried in the shade after being collected in 3 and 4 months in the lunar calendar. However, the gastrodia elata has large volume, high water content and long airing time, so that the contained phenylethanoid glycosides are easily hydrolyzed by enzyme, and the content of the phenylethanoid glycosides is reduced. Therefore, the process increases the production cost, and the loss of effective components caused by the decomposition of heat-sensitive components in the gastrodia elata due to improper process temperature control on the heat-sensitive components in the gastrodia elata, such as leonurus glycoside, geniposide, hesperetin A, catalpol, catechin and the like.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a freeze-dried preparation containing a gastrodia elata extract, a preparation method of the freeze-dried preparation, and application of the freeze-dried preparation and the preparation method thereof in the fields of medicines and the like. The freeze-dried preparation containing the gastrodia elata extract prepared by the method has the advantage that the content of active ingredients in the gastrodia elata is obviously improved.
The invention provides a freeze-dried preparation containing a gastrodia elata extract, which comprises the gastrodia elata extract and a binder, wherein the gastrodia elata extract accounts for 0.004wt% -95wt% of the freeze-dried preparation, and the gastrodia elata extract contains at least one of iridoid and glycosides thereof, lignan glycosides, phenethyl alcohol glycosides, flavonoids and alkaloids. Wherein the phenylethanoid glycosides have effects of enhancing immunity, protecting neuron, reducing free radical generation and resisting lipid peroxidation, and the iridoid has effects of antivirus, antibacterial, antioxidant, protecting liver and gallbladder, anti-tumour, antiinflammatory, and enhancing immunity.
According to some preferred embodiments of the lyophilized formulation of the present invention, the mass percentage of the binder in the lyophilized formulation is 0.01wt% to 50wt%.
In the present invention, the content of the parahydroxybenzyl alcohol in the gastrodia elata extract may be 2wt%, 2.5wt%, 3wt%, 3.5wt%, 4wt%, 4.5wt%, 5wt%, 5.5wt%, 6wt%, 6.5wt%, 7wt%, 7.5wt%, 8wt%, 8.5wt%, 9wt%, 9.5wt%, 10wt% and any value therebetween, preferably 5wt% to 8wt%.
In the present invention, the content of the balsamoside a in the gastrodia elata extract may be 2.5wt%, 3wt%, 3.5wt%, 4wt%, 4.5wt% and any value therebetween, and is preferably 3wt% to 4.5wt%.
In the present invention, the content of the balaneboside B in the gastrodia elata extract may be 1.0wt%, 1.2wt%, 1.4wt%, 1.6wt%, 1.8wt%, 2.0wt%, 2.2wt%, 2.4wt%, 2.6wt%, 2.7wt% and any value therebetween, preferably 1.2wt% to 1.5wt%.
In the present invention, the content of the balsamoside E in the gastrodia elata extract may be 0.7wt%, 0.9wt%, 1.1wt%, 1.3wt%, 1.5wt%, 1.7wt%, 1.9wt%, 2.1wt%, 2.3wt%, 2.5wt% and any value therebetween, preferably 1.0wt% to 1.5wt%.
According to some preferred embodiments of the lyophilized preparation of the present invention, the lyophilized preparation is lyophilized from a preformulation comprising gastrodia elata extract and a binder.
According to some preferred embodiments of the lyophilized formulation of the present invention, the weight percentage of the gastrodia elata extract in the pre-solution is 0.004wt% to 50wt%, the weight percentage of the binder in the pre-solution is 0.01wt% to 50wt%, and the weight of the gastrodia elata extract is proportional to the weight of the binder.
According to some preferred embodiments of the lyophilized formulation of the present invention, the weight percentage of the gastrodia elata extract in the pre-formulation solution is 50wt% to 95wt%, the weight percentage of the binder in the pre-formulation solution is 0.01wt% to 20wt%, and the weight of the gastrodia elata extract is inversely proportional to the weight of the binder.
According to some preferred embodiments of the lyophilized formulation of the present invention, the lyophilized formulation is an oral formulation, a solid beverage or a non-wash care skin care product.
When the freeze-dried preparation is used as an oral preparation, the weight percentage of the gastrodia elata extract in the pre-preparation liquid is 0.004wt% -50 wt%, and the weight percentage of the binder in the pre-preparation liquid is 0.01wt% -50 wt%. The freeze-dried preparation has the disintegration time of less than 3s under the condition of 0.1-0.3 mL of saliva, the dissolution rate in 1min is more than 90 percent, and the oral disintegration and the rapid dissolution can be realized.
When the freeze-dried preparation is used as a solid beverage, such as granules or instant tablets, the weight percentage of the rhizoma gastrodiae extract in the pre-preparation liquid is 50wt% -95wt%, and the weight percentage of the binder in the pre-preparation liquid is 0.01wt% -20 wt%. The freeze-dried preparation is put into water with the temperature of 20-50 ℃, the disintegration time is still less than 10s, the freeze-dried preparation is dissolved in 15s until no particles are seen, the dissolution amount is more than 90% in 1min, and the quick disintegration, the quick and uniform dissolution and the quick dissolution at low water temperature can be realized.
When the freeze-dried preparation is used as a non-washing and protecting skin care product, such as essence, cream milk or body milk, the weight percentage of the rhizoma gastrodiae extract in the pre-preparation liquid is 0.004-30 wt%, and the weight percentage of the binder in the pre-preparation liquid is 0.01-50 wt%.
According to some preferred embodiments of the lyophilized formulation of the present invention, the binder is a lyophilized binder and/or a low temperature binder.
The freeze-dried binder is preferably at least one selected from artificial or natural high molecular polymers, modified artificial or natural high molecular polymers, inorganic gelling agents, polysaccharides, polysaccharide derivatives and salts thereof, sugar alcohols, cellulose ethers, modified starches, albumin and polyamino acids.
The low temperature binder is preferably selected from C 1 ～C 16 At least one of alcohol, grease, surfactant, artificial or natural high molecular polymer or modified artificial or natural high molecular polymer.
Wherein the artificial or natural high molecular polymer may be at least one selected from the group consisting of collagen, gelatin, hydrolyzed collagen, acacia, xanthan gum, soy protein gum, sclerotium rolfsii gum, biosaccharide gum, carrageenan, guar gum, gellan gum, pectin, konjac gum, carrageenan, locust bean gum, alginic acid, sodium alginate, agar, polyvinyl alcohol methyl acrylate graft copolymer, carbomer resin, polyvinyl pyrrolidone, polyvinyl alcohol and derivatives thereof, polyethylene glycol and derivatives thereof, polyethylene oxide, polyacrylamide, sodium polyacrylate, and polyacrylic acid and derivatives thereof.
The modified artificial or natural high molecular polymer can be at least one selected from modified Arabic gum, modified xanthan gum, modified guar gum, modified pectin, modified sodium polyacrylate, and grafted starch and modified paraffin.
According to some preferred embodiments of the lyophilized preparation of the present invention, the lyophilized preparation further comprises an adjuvant, wherein the adjuvant is 0.01wt% to 50wt% in the pre-formulation. Preferably, the auxiliary material is selected from at least one of a skeleton supporting agent, a disintegrating agent, a skin feeling modifier, an antioxidant, a flavoring agent, an essence, a trans-mucosal or transdermal absorption enhancer and a pH regulator.
Wherein the scaffold support agent may be at least one selected from maltose, trehalose, microcrystalline cellulose, mannitol, sorbitol, xylitol, glycine, alanine, glutamic acid, sodium phosphate, aluminum silicate and maltodextrin.
The disintegrant may be selected from at least one of effervescent agents, anhydrous lactose, a combination of starch and amylase, a combination of cellulose and cellulase, a combination of gum and hemicellulase, a combination of gelatin and protease, salts of alginic acid, carrageenase, a combination of sucrose and invertase.
The skin feeling modifier can be selected from polymethylsilsesquioxane, tapioca starch, modified tapioca starch, corn starch, modified corn starch, pearl powder, silica, titanium dioxide, mica, polydimethylsiloxane, di (C) 12 ～C 13 ) Alcohol malate, dimyristyl tartrate, PPG-15 stearyl alcohol ether, chinlon-12, and Vaccinium myrtillus seed oil.
The antioxidant can be at least one selected from vitamin C, vitamin E, 2,6-di-tert-butyl-4-methylphenol, tert-butyl hydroquinone, butyl hydroxy anisole, N-phenylacetyl-L-glutamine, trihydroxy phenyl butanone, citric acid, phosphoric acid derivatives, EDTA, baicalin, astaxanthin, sodium sulfite, sodium metabisulfite, gallate, phytic acid, tea polyphenols, anthocyanins, resveratrol, glutathione, superoxide dismutase, yeast/rice fermentation product filtrate, plant extract, beauveria bassiana extract, gymnosphaera sinensis extract, fruit and vegetable extract, and plant-derived polyphenol compounds.
The flavoring agent and essence can be at least one of essence such as mint, chocolate, fruit and vegetable, flower and grass, plant, vanilla, coffee, tea, corn, lemon, milk, fruit, raspberry, hawthorn, and medlar.
The transmucosal or transdermal absorption enhancer may be selected from at least one of lecithin, tween and span.
The transdermal absorbent can be at least one selected from azone, lecithin and ethoxy diethylene glycol.
The pH regulator may be at least one selected from citric acid, sorbic acid, tartaric acid, lactic acid, malic acid, sodium bicarbonate, sodium carbonate, disodium hydrogen phosphate, calcium phosphate, potassium phosphate, and trimagnesium phosphate.
According to some preferred embodiments of the lyophilized preparation of the present invention, the lyophilized preparation further comprises other active ingredients, and the mass percentage of the active ingredients in the pre-formulation is 0.01wt% to 50wt%; more preferably, the other active ingredients are selected from at least one of steroid saponin, radix astragali extract, ginseng extract, american ginseng extract, gynostemma pentaphyllum extract, flavone, ginseng polysaccharide, sea cucumber polysaccharide, amino acid, dencichine, pilose antler polypeptide, resveratrol, pearl powder, hydrolyzed pearl, rana japonica oil extract, SOD or hawthorn extract.
According to some preferred embodiments of the lyophilized formulation of the present invention, the lyophilized formulation may be, but is not limited to, a tablet shape, a spherical shape, an ellipsoidal shape, or various human, animal, plant, food, graphic logo or cartoon characters.
According to some preferred embodiments of the lyophilized preparation of the present invention, the gastrodia elata extract is prepared by a carbon dioxide supercritical extraction-macroporous resin exchange adsorption process, comprising:
s1, adding pure water into the chopped gastrodia elata, and performing homogenate and juicing to obtain juice A and residue B;
s2, performing carbon dioxide supercritical extraction on the slag B to obtain an extract C;
and S3, subjecting the juice A and/or the extract C to exchange adsorption through a macroporous resin column, eluting, determining a target object by sampling thin-layer chromatography, collecting a target section, concentrating, and freeze-drying to obtain the gastrodia elata extract.
Pure water is usually added to the S1 in an amount of 1 to 10 times the weight of Gastrodia elata Blume, and the temperature of the homogenate and the juice extraction may be 0 ℃, 2 ℃, 4 ℃,6 ℃, 8 ℃, 10 ℃, 12 ℃, 14 ℃, 16 ℃, 18 ℃, 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃,30 ℃, 32 ℃, 34 ℃, 36 ℃, 38 ℃ or any value therebetween, preferably 10 ℃ to 20 ℃.
In the S2, the carbon dioxide supercritical extraction conditions comprise: the entrainer is ethanol or an aqueous solution of ethanol, and limits the extraction temperature and extraction time.
Wherein the extraction temperature may be-40 ℃, -38 ℃, -36 ℃, -34 ℃, -32 ℃, -30 ℃, -28 ℃, -26 ℃, -24 ℃, -22 ℃, -20 ℃, -18 ℃, -16 ℃, -14 ℃, -12 ℃, -10 ℃, -8 ℃, -6 ℃, -4 ℃, -2 ℃,0 ℃, 2 ℃, 4 ℃,6 ℃, 8 ℃, 10 ℃, 12 ℃, 14 ℃, 16 ℃, 18 ℃, 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃,30 ℃, 32 ℃, 34 ℃, 36 ℃, 38 ℃ and any value therebetween, preferably-10 ℃ to 20 ℃.
The extraction time can be 30min, 32min, 34min, 36min, 38min, 40min, 42min, 44min, 46min, 48min, 50min, 52min, 54min, 56min, 58min, 60min, 62min, 64min, 66min, 68min, 70min, 72min, 74min, 76min, 78min, 80min, 82min, 84min, 86min, 88min, 90min, 92min, 94min, 96min, 98min, 100min; preferably 40min to 80min.
The conditions of the macroporous resin column exchange adsorption in the S3 comprise: the eluent is ethanol solution with the volume concentration of 30vol% -100 vol%. Preferably, the concentration is reduced pressure concentration, and the concentration temperature is 0-25 ℃.
By using the extraction method, 0.10 g-0.20 g of extract can be obtained per 1g of rhizoma gastrodiae, wherein the extract contains 2 multiplied by 10 -3 g～2×10 -2 g p-hydroxybenzyl alcohol, and/or 2.5X 10 -3 g～1.11×10 -2 g of Balisin A, and/or 1X 10 -3 g～5.4×10 -3 g of Balisin B, and/or 7X 10 -4 g～5×10 -3 g of the balaneboside E.
The gastrodia elata extract is prepared by adopting the carbon dioxide supercritical extraction-macroporous resin exchange adsorption process, so that the properties of heat-sensitive components in the gastrodia elata are kept to the maximum extent.
The second aspect of the present invention provides a method for preparing the above lyophilized preparation, comprising:
a) Mixing a solvent, a gastrodia elata extract, a binder, an optional active ingredient and an optional auxiliary material to form a pre-prepared solution, and performing constant volume and degassing to obtain a side product;
c) Freeze-drying the product obtained in the previous step to obtain a freeze-dried preparation;
optionally, between step a) and step c), further comprising
b) And carrying out side product instillation in the cabin with the internal temperature lower than the eutectic point of the pre-prepared liquid, so that the side product is quickly frozen when being dripped.
According to some preferred embodiments of the preparation method of the present invention, the solvent in step a is pure water.
According to some preferred embodiments of the preparation method of the present invention, the pre-formulation in step a may be in the form of a solution, emulsion or suspension.
In a third aspect, the present invention provides another method for preparing the above lyophilized formulation, comprising:
a) Preparation of a soft ice mixture: mixing the gastrodia elata extract, a binder, an optional active ingredient, an optional auxiliary material and a solvent to obtain a pre-mixed liquid 1, and freezing the pre-mixed liquid 1 to obtain a soft ice mixture 1;
b) Mixing a binder, a solvent, an optional active ingredient and an optional auxiliary material to obtain a pre-prepared liquid 2, and freezing and crushing or spraying the pre-prepared liquid 2 at a low temperature to obtain ice powder 2;
c) Mixing the active ingredient with the auxiliary material to obtain dry powder 3; the active ingredient is taken as a dry powder 4;
d) Mixing one or more of the soft ice mixture 1, the ice powder 2, the dry powder 3 and the dry powder 4 to obtain a soft ice mixture;
e) Shaping the soft ice mixture obtained in step d) to obtain a mixture 5;
f) And (5) freeze-drying the mixture 5 to obtain a freeze-dried preparation containing the gastrodia elata extract.
The fourth aspect of the invention provides the application of the freeze-dried preparation or the preparation method in the fields of food, beverage, medicine, health care product and cosmetics.
The invention has the beneficial effects that:
the freeze-dried preparation containing the gastrodia elata extract has the advantages of high disintegration speed, short dissolution time and high dissolution speed, and the freeze-dried preparation is high in drug loading capacity. The obtained rhizoma Gastrodiae extract has good pharmacological properties, and can be added into lyophilized preparation to retain good pharmacological properties.
Detailed Description
The present invention will be described in detail below with reference to examples, but the scope of the present invention is not limited to the following description.
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available from commercial sources.
In the following examples, the specific extraction method of the gastrodia elata extract is as follows:
1. cutting cleaned rhizoma gastrodiae into pieces, and adding pure water with the weight 1-10 times of the weight of the rhizoma gastrodiae; homogenizing and juicing the gastrodia elata fragments at 0-38 ℃ to obtain juice A and residue B;
2. extracting the residue B with supercritical carbon dioxide, extracting with ethanol as entrainer at-40 deg.C-38 deg.C for 30-100min to obtain extract C, and discarding the residue;
3. subjecting the extract C to exchange adsorption by a macroporous resin column, washing with water to remove impurities, eluting the gastrodia elata extract by 30-100 vol% ethanol solution, determining a target object by sampling thin-layer chromatography, collecting a target section, concentrating under reduced pressure at 0-38 ℃ until no alcohol smell exists, and freeze-drying to obtain a gastrodia elata extract 1;
4. subjecting the juice A to exchange adsorption by a macroporous resin column, washing with water to remove impurities, eluting a gastrodia elata extract by 30-100 vol% ethanol solution, determining a target object by sampling thin-layer chromatography, collecting a target section, concentrating under reduced pressure at 0-38 ℃ until no alcohol smell exists, and freeze-drying to obtain a gastrodia elata extract 2;
5. the Gastrodia elata extract 1 and Gastrodia elata extract 2 are used separately or combined to obtain the final Gastrodia elata extract.
In some of the following examples, the process for preparing the lyophilized formulation is as follows:
a) Mixing solvent, rhizoma Gastrodiae extract, binder, optional active ingredient and optional adjuvants to form pre-prepared solution in the form of solution, emulsion or suspension, diluting to desired volume, and degassing;
b) Injecting the pre-prepared liquid obtained in the step a) into a quantitative forming die by using a quantitative filling pump, and degassing;
c) Freeze drying the product obtained in the step b), and removing the solvent to obtain a freeze-dried preparation. Wherein the conditions of freeze-drying include: the temperature is-70 ℃ to-10 ℃, the pressure is-0.02 MPa to-0.1 MPa, and the time is 5h to 24h.
In some other embodiments below, the process for preparing the lyophilized formulation is as follows:
a) Preparation of a soft ice mixture:
mixing the gastrodia elata extract, a binder, an optional active ingredient, an optional auxiliary material and a solvent to obtain a pre-mixed solution 1, and freezing the pre-mixed solution 1 to obtain a soft ice mixture 1. The freezing conditions include: the temperature is-70 ℃ to-10 ℃, the pressure is-0.02 MPa to-0.1 MPa, and the time is 5h to 24h. .
b) Mixing a binder, a solvent, an optional active ingredient and an optional auxiliary material to obtain a pre-prepared liquid 2, and freezing and crushing or spraying the pre-prepared liquid 2 at a low temperature to obtain the ice powder 2.
c) Mixing the active ingredient with the auxiliary material to obtain dry powder 3; the active ingredient is provided as a dry powder 4.
d) And mixing one or more of the soft ice mixture 1, the ice powder 2, the dry powder 3 and the dry powder 4 to obtain the soft ice mixture.
e) Using a mould to shape the soft ice mixture obtained in the step d) to obtain a mixture 5, and demoulding.
f) And (5) freeze-drying the mixture 5 to obtain a freeze-dried preparation containing the gastrodia elata extract. Wherein the freeze-drying conditions include: the temperature is-70 ℃ to-10 ℃, the pressure is-0.02 MPa to-0.1 MPa, and the time is 5h to 24h.
[ example 1 ]
A lyophilized preparation containing rhizoma Gastrodiae extract is used as whitening antioxidant component of skin care product or as effective component of anti-alopecia shampoo. In the freeze-dried preparation, 30wt% of gastrodia elata extract, 30wt% of ethyl cellulose, 5wt% of transdermal absorption enhancer peppermint oil, 5wt% of skin feel modifier polymethyl methacrylate, 2wt% of hydrolyzed pearl and 3wt% of organic silicon resin. The skin care product has disintegration time of 5s, dissolution time of less than 12s, and dissolution rate of more than 95% in 50s.
The lyophilized formulation is prepared by the following steps:
a) Preparation of a soft ice mixture: mixing the gastrodia elata extract, ethyl cellulose and water according to a set proportion to obtain a pre-prepared liquid, and freezing the pre-prepared liquid to obtain a soft ice mixture;
b) Taking peppermint oil, polymethyl methacrylate, organic silicon resin and hydrolyzed pearl as dry powder;
e) Mixing the soft ice mixture and the ice powder to obtain all soft ice mixtures;
f) Shaping by using a tablet-shaped mould to obtain a shaped mixture, and demoulding;
g) Freeze-drying the mixture to obtain the non-washing skin care product.
When the non-washing skin care product is used, 1-3mL of water, cosmetic water or essence is used for dissolving to obtain essence, cream milk or body milk, and the essence, cream milk or body milk is smeared on the epidermis of the corresponding position of the body, so that the skin care product has whitening and antioxidant effects. Or the lyophilized preparation can be used as shampoo component, and has alopecia preventing effect.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.

Claims (10)

1. The freeze-dried preparation comprises a gastrodia elata extract and a binder, wherein the gastrodia elata extract accounts for 0.004wt% -95wt% of the freeze-dried preparation in mass percent, and the gastrodia elata extract contains at least one of p-hydroxybenzyl alcohol, gastrodia elata polysaccharide, barban glycoside A, barban glycoside B and barban glycoside E.
2. The lyophilized preparation according to claim 1, wherein the mass percentage of the binder in the lyophilized preparation is 0.01wt% to 50wt%;
preferably, the content of each substance in the gastrodia elata extract is as follows:
2 to 10 weight percent of p-hydroxybenzyl alcohol, preferably 5 to 8 weight percent; and/or
2.5 to 5.55 weight percent of the balamin A, preferably 3 to 4.5 weight percent; and/or
1.0-2.7 wt% of the Balsamine B, preferably 1.2-1.5 wt%; and/or
0.7 to 2.5 weight percent of the Balsamine E, preferably 0.4 to 1 weight percent.
3. The lyophilized formulation according to claim 1 or 2, wherein the lyophilized formulation is lyophilized from a preformulation comprising a Gastrodia elata extract and a binder:
preferably, the weight percentage of the gastrodia elata extract in the pre-preparation liquid is 0.004wt% -50 wt%, the weight percentage of the binder in the pre-preparation liquid is 0.01wt% -50 wt%, and the weight of the gastrodia elata extract is in direct proportion to the weight of the binder;
preferably, the weight percentage of the gastrodia elata extract in the pre-preparation liquid is 50wt% -95wt%, the weight percentage of the binder in the pre-preparation liquid is 0.01wt% -20 wt%, and the weight of the gastrodia elata extract is inversely proportional to the weight of the binder.
4. The lyophilized formulation according to any one of claims 1 to 3, wherein the lyophilized formulation is an oral formulation, a solid beverage or a non-wash care skin care product;
preferably, the freeze-dried preparation is an oral preparation, the weight percentage of the gastrodia elata extract in the pre-preparation liquid is 0.004wt% -50 wt%, and the weight percentage of the binder in the pre-preparation liquid is 0.01wt% -50 wt%;
preferably, the freeze-dried preparation is a solid beverage, the weight percentage of the gastrodia elata extract in the pre-preparation liquid is 50wt% -95wt%, and the weight percentage of the binder in the pre-preparation liquid is 0.01wt% -20 wt%;
preferably, the freeze-dried preparation is a non-washing skin care product, the weight percentage of the gastrodia elata extract in the pre-prepared liquid is 0.004-30 wt%, and the weight percentage of the binder in the pre-prepared liquid is 0.01-50 wt%.
5. The lyophilized formulation according to any one of claims 1 to 4, wherein the binder is a lyophilized binder and/or a low temperature binder; preferably, the freeze-dried binder is selected from at least one of artificial or natural high molecular polymer, modified artificial or natural high molecular polymer, inorganic gelling agent, polysaccharide derivative and salt thereof, sugar alcohol, cellulose ether, modified starch, albumin or polyamino acid; and/or the low-temperature binder is selected from C 1 ～C 16 At least one of alcohol, grease, surfactant, artificial or natural high molecular polymer or modified artificial or natural high molecular polymer.
6. The freeze-dried preparation according to any one of claims 1 to 5, further comprising an auxiliary material, wherein the auxiliary material is 0.01 to 50wt% of the pre-formulation solution; preferably, the auxiliary material is selected from at least one of a skeleton supporting agent, a disintegrating agent, a skin feel modifier, an antioxidant, a flavoring agent, essence, a trans-mucosal membrane, a transdermal absorption enhancer and a pH regulator;
further preferably, the freeze-dried preparation also comprises other active ingredients, and the mass percentage of the active ingredients in the pre-prepared liquid is 0.01-50 wt%; more preferably, the other active ingredients are selected from at least one of steroid saponin, radix astragali extract, ginseng extract, american ginseng extract, gynostemma pentaphyllum extract, flavone, ginseng polysaccharide, sea cucumber polysaccharide, amino acid, dencichine, pilose antler polypeptide, resveratrol, pearl powder, hydrolyzed pearl, rana japonica oil extract, SOD or hawthorn extract.
7. The lyophilized preparation according to any one of claims 1 to 6, wherein the Gastrodia elata extract is prepared by a carbon dioxide supercritical extraction-macroporous resin exchange adsorption process comprising:
s1, adding pure water into the chopped gastrodia elata, and performing homogenate and juicing to obtain juice A and residue B;
s2, performing carbon dioxide supercritical extraction on the slag B to obtain an extract C;
s3, subjecting the juice A and/or the extract C to exchange adsorption through a macroporous resin column, eluting, determining a target object by sampling thin-layer chromatography, collecting a target section, concentrating, and freeze-drying to obtain a gastrodia elata extract;
preferably, the conditions for the homogenate squeezing in S1 include: the temperature is 0-38 ℃;
preferably, the conditions of the supercritical carbon dioxide extraction in S2 include: the extraction temperature is-40 ℃ to 38 ℃; the extraction time is 30min to 100min; the entrainer is ethanol or ethanol water solution;
preferably, the conditions of the macroporous resin column exchange adsorption in S3 comprise: the eluent is ethanol solution with the volume concentration of 30vol% -100 vol%; more preferably, the concentration is a concentration under reduced pressure, and the concentration temperature is 0 ℃ to 38 ℃.
8. A method of preparing the lyophilized formulation of any one of claims 1-7, comprising:
a) Mixing a solvent, a gastrodia elata extract, a binder, an optional active ingredient and an optional auxiliary material to form a pre-prepared solution, and performing constant volume and degassing to obtain a side product;
c) Freeze-drying the product obtained in the previous step to obtain a freeze-dried preparation;
optionally, between step a) and step c), further comprising
b) And carrying out side product instillation in the cabin with the internal temperature lower than the eutectic point of the pre-prepared liquid, so that the side product is quickly frozen when being dripped.
9. A method of preparing the lyophilized formulation of any one of claims 1-7, comprising:
a) Preparation of a soft ice mixture: mixing the gastrodia elata extract, a binder, an optional active ingredient, an optional auxiliary material and a solvent to obtain a pre-mixed liquid 1, and freezing the pre-mixed liquid 1 to obtain a soft ice mixture 1;
b) Mixing a binder, a solvent, an optional active ingredient and an optional auxiliary material to obtain a pre-prepared liquid 2, and freezing and crushing or spraying the pre-prepared liquid 2 at a low temperature to obtain ice powder 2;
c) Mixing the active ingredient with the auxiliary material to obtain dry powder 3; the active ingredient is taken as a dry powder 4;
d) Mixing one or more of the soft ice mixture 1, the ice powder 2, the dry powder 3 and the dry powder 4 to obtain a soft ice mixture;
e) Shaping the soft ice mixture obtained in step d) to obtain a mixture 5;
f) And (5) freeze-drying the mixture 5 to obtain a freeze-dried preparation containing the gastrodia elata extract.
10. Use of the lyophilized formulation according to any one of claims 1 to 6 or the method of preparation according to claim 9 in the fields of medicine, food, beverages, health products and cosmetics.
CN202110753111.XA 2021-07-02 2021-07-02 Freeze-dried preparation containing gastrodia elata extract and preparation method and application thereof Pending CN115554365A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116735514A (en) * 2023-08-11 2023-09-12 昆明理工大学 Method for rapidly detecting gastrodia elata sulfuration markers by nano-enzyme combined liquid-liquid microextraction

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116735514A (en) * 2023-08-11 2023-09-12 昆明理工大学 Method for rapidly detecting gastrodia elata sulfuration markers by nano-enzyme combined liquid-liquid microextraction
CN116735514B (en) * 2023-08-11 2023-11-03 昆明理工大学 Method for rapidly detecting gastrodia elata sulfuration markers by nano-enzyme combined liquid-liquid microextraction

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