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CN106433962A - Preparation method and use of Xanthoceras sobifoba kernel oil extracted from supercritical fluid and preparation of Xanthoceras sobifoba kernel oil - Google Patents

Preparation method and use of Xanthoceras sobifoba kernel oil extracted from supercritical fluid and preparation of Xanthoceras sobifoba kernel oil Download PDF

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CN106433962A
CN106433962A CN201610909805.7A CN201610909805A CN106433962A CN 106433962 A CN106433962 A CN 106433962A CN 201610909805 A CN201610909805 A CN 201610909805A CN 106433962 A CN106433962 A CN 106433962A
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preparation
kernel oil
extraction
supercritical fluid
lignum xanthoceratiss
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刘欣
孙鹏
刘彦臣
刘君
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Harbin University of Science and Technology
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Harbin University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/104Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/77Sapindaceae (Soapberry family), e.g. lychee or soapberry
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/20Pills, tablets, discs, rods
    • A61K9/2004Excipients; Inactive ingredients
    • A61K9/2022Organic macromolecular compounds
    • A61K9/2031Organic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyethylene glycol, polyethylene oxide, poloxamers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/4816Wall or shell material
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005Wall or coating material
    • A61K9/5021Organic macromolecular compounds
    • A61K9/5052Proteins, e.g. albumin
    • A61K9/5057Gelatin
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/108Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/37Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction

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Abstract

The invention relates to a preparation method and use of Xanthoceras sobifoba kernel oil extracted from supercritical fluid and a preparation of the Xanthoceras sobifoba kernel oil. The preparation method comprises the steps of grinding Xanthoceras sobifoba kernels, sieving by virtue of a 10-100-mesh sieve, and carrying out supercritical fluid extraction in an extraction kettle, so as to obtain the Xanthoceras sobifoba kernel oil and a kernel residue rich in proteins, wherein the kernel residue can be used for extracting total saponins and has an extremely high medical value. Compared with a traditional squeezing process, a CO2 supercritical fluid extraction method has the advantages that the process is simple, the production cycle is short, the extraction efficiency is high, and the serious damage of unsaturated fatty acid in grease and the denaturationof the proteins in medicine residues at the high temperature are avoided. Compared with a method for extracting by virtue of organic solvents such as petroleum ether, the CO2 supercritical fluid extraction method has the advantages that the residual solvent is avoided, operation condition are mild, and the production is safe, toxic free and environmentally friendly. The oil extraction rate of the Xanthoceras sobifoba kernels is not lower than 50%, and GC-MS detection shows that the content of unsaturated fatty acid reaches up to 75% or above. By adding medical auxiliary materials, the dose forms of soft capsules, micro-capsules, cyclodextrin coated preparations, dripping pills and the like can be prepared and can be used for developing health products for preventing and treating hypertension, hyperlipemia and diseases of cardiovascular systems.

Description

A kind of preparation method of supercritical fluid extraction Lignum Xanthoceratiss seed kernel oil and its preparation and Purposes
Technical field
The invention belongs to pharmaceutical technology field, it is related to the preparation of a kind of supercritical fluid extraction Lignum Xanthoceratiss seed kernel oil and its preparation Method and purposes.
Background technology
Lignum Xanthoceratiss (Xanthoceras sorbifoBa Bunge) are that Sapindaceae (Sapindaceae) Lignum Xanthoceratiss belong to plant Thing, be check winds and fix drifting sand, the fine tree species of water and soil conservation and afforestation, be distributed mainly on northern China Liaoning, Jilin, Hebei, The provinces and regions such as Shandong, Gansu, Ningxia, the Inner Mongol, Shanxi, Henan.《China National medicine will》Described in Lignum Xanthoceratiss kernel be the Mongols Conventional crude drugs, have functions that QI invigorating, calm the nerves, moistening five ZANG-organss, nourishing blood and promoting granulation, long term usage spry and light, can be used for treat infantile enuresiss, urine Frequently, the disease such as urinary incontinence, mental retardation of children, senile dementia, parkinsonism【Ministry of Public Health pharmaceutical biological product examines and determine institute, China National medicine will, People's Health Publisher, 1984:130-132】.Lignum Xanthoceratiss kernel once listed version in 1977 in《Chinese Pharmacopoeia》 【Chinese Pharmacopoeia Commission, 1977 editions Pharmacopoeias of People's Republic of China. one. Beijing:Chemical Industry Press, 1977】. Lignum Xanthoceratiss kernel oil content average out to 59.86%, wherein contains multiple fatty acids, particularly with substantial amounts of unsaturated fatty acid, Total content is up to 92%, and fatty acid component is respectively:Palmic acid, stearic acid, Oleic acid, linoleic acid plus linolenic acid, wherein especially with sub- oil Acid content is highest, may be up to 52.78%, is the main component for treating hypertension;Oleic acid content reaches 31.8l%【1. the bavin spring Mountain, Qi Jianli, Cai Guojun, etc. the analysis of variance of Lignum Xanthoceratiss seed oil content and its fatty acid component. economic forest is studied, and 2013, 31 (2): 100-103;2. Deng Hong, He Ling, Sun Jun. the cold pressing extraction of shinyleaf yellowhorn oil and physicochemical property research. southwest agricultural College journal:Natural science edition, 2006,28 (6): 1027-1031】.Lignum Xanthoceratiss seed kernel oil is easily absorbed by the human body digestion, tool There are the medical values such as reduction cholesterol, vessel softening, preventing and treating cardiovascular system diseases, can improve and coordinate human endocrine, Promote skeleton, brain and nervous system development, prevent infirmities of age.【Wang Lihua. Lignum Xanthoceratiss eat and medical value. China Medical guide, 2006, (10): 41-43】.Lignum Xanthoceratiss seed kernel oil is alternatively arranged as skin protection cosmeticss raw material, precision instrument lubrication Oil, and can be used in developing biodiesel.In addition, after Lignum Xanthoceratiss kernel sloughs oils and fatss, raw material residue can be used for extracting triterpene Class total saponins, for treating infantile enuresiss, frequent micturition, urinary incontinence, mental retardation of children, senile dementia, parkinsonism etc. Disease, has high practical value and wide market prospect in terms of new drug development.Protein in Lignum Xanthoceratiss kernel contains Amount is abundant and amino acid classes are complete, 17 kinds of amino such as glutamic acid rich in needed by human body, arginine, aspartic acid and serine Acid.The AAS of Lignum Xanthoceratiss protein is higher than Semen arachidis hypogaeae, and protein is better than Semen arachidis hypogaeae protein, has higher nutritive value【Wu Beautiful clear, Zheng Zhanwei, Fu Fengqi. Lignum Xanthoceratiss Analysis of Nutritive Composition and edibility research. processing of farm products, 2010, (11): 93-95】;And Lignum Xanthoceratiss Protein processing characteristic is good, be a kind of excellent protein resource it is adaptable to do food additive, or Exploitation vegetable protein beverage.
At present, the traditional extraction extracting method of Lignum Xanthoceratiss seed kernel oil mainly includes:Conventional press method and organic solvent leach Method.Milling process oil yield is low, and the unsaturated fatty acid in oils and fatss under the conditions of high temperature squeezing is seriously damaged, and is easily caused in medicinal residues Protein denaturation;Conventional organic solvents solvent extraction method, long the production cycle, organic solvent consumption is big, and production cost is high, and solvent is not allowed Easily reclaim, big to operator's physical impairment, increase the pollution to environment.Supercritical CO2Fluid extraction compared with traditional handicraft, There is not dissolvent residual, and solvent, abundance are done using carbon dioxide, using safety, extraction selectivity is good, oil High with the quality of the dregs of rice;There is process is simple, no solvent residue in short production cycle, product, operating condition is gentle, do not destroy insatiable hunger The advantages of with fatty acid and protein active, suitable industrialized production.
Content of the invention
It is an object of the invention to provide one kind utilizes supercritical CO2The method that fluid extraction prepares Lignum Xanthoceratiss seed kernel oil, This technical process is simple, and oil yield is high, the quality better of oil and the dregs of rice, low-carbon environment-friendly.The Lignum Xanthoceratiss kernel prepared in this way Oil, can make soft capsule, microcapsule, cyclodextrin bag and the dosage form such as preparation, drop pill by adding pharmaceutic adjuvant, for exploitation preventing and treating Hypertension, hyperlipemia, the health product of cardiovascular system diseases, have high practical value and wide market prospect.
The inventive method is realized by following steps:Lignum Xanthoceratiss seed removes the peel to obtain Lignum Xanthoceratiss kernel, under the conditions of 40~50 DEG C Dry 6~12 h, control water content to be less than 8%, pulverize, cross 10~100 mesh sieves, load in extraction kettle.Extraction temperature 30~60 DEG C, extracting pressure 25~35 Mpa, CO2Flow 10~180 L/h, separating still I temperature is 35~45 DEG C, and separating still I pressure is 5 ~20 Mpa, separating still II temperature is 25~35 DEG C, and separating still II pressure is 2~10 Mpa, and extraction time is 60~200 Min, collects extraction fraction, obtains Lignum Xanthoceratiss seed kernel oil.In extraction kettle, leftover materials are the Lignum Xanthoceratiss kernel medicine containing abundant protein Slag, is available for extracting total triterpene saponinss, and extraction finishes oil content in rear residue and is less than 4%.Prepared Lignum Xanthoceratiss seed kernel oil oil yield is not Less than 50%, through GC-MS detection, unsaturated fatty acid content is up to more than 75%.
After Lignum Xanthoceratiss kernel extracts oils and fatss, residue can be used for extracting triterpeness total saponins, for treating infantile enuresiss, urine Frequently, the disease such as urinary incontinence, mental retardation of children, senile dementia, parkinsonism, has high reality in terms of new drug development With being worth and wide market prospect.
After extracting Lignum Xanthoceratiss seed kernel oil, medicinal residues contain abundant protein, and Lignum Xanthoceratiss protein is better than Semen arachidis hypogaeae protein, has higher Nutritive value, processing characteristics are good, be a kind of excellent protein resource it is adaptable to do food additive, or exploitation plant Protein beverage.
It is an advantage of the invention that:
1. the present invention utilizes supercritical CO2Fluid extraction isolation technics, the Lignum Xanthoceratiss seed kernel oil of preparation high-quality, unsaturated lipid Fat acid content up to more than 75%, and multiple dosage forms can be made by adding various pharmaceutic adjuvants, develop and prevent and treat hypertension, height Lipidemia, the health product of cardiovascular system diseases;
2. the present invention is reasonable in design, process is simple, energy-conserving and environment-protective.Using supercritical CO2Fluid extraction isolation technics, obtain high The Lignum Xanthoceratiss seed kernel oil of quality, non-environmental-pollution, simple and efficient to handle, cost is relatively low, is especially suitable for industrialized production;
The Lignum Xanthoceratiss seed kernel oil of obtained high-quality, can be made into soft capsule, microcapsule, cyclodextrin by adding various pharmaceutic adjuvants Bag and the dosage form such as preparation, drop pill.
Prepared Lignum Xanthoceratiss seed kernel oil microcapsule, can be using fluid bed preparation method, spray drying preparation method, emulsifying molding Method.
Specific embodiment
The invention will be further described with reference to embodiments, but the invention is not limited in these embodiments.
Embodiment 1 supercritical CO2Fluid extraction isolation technics prepare the Lignum Xanthoceratiss seed kernel oil of high-quality
Lignum Xanthoceratiss seed is removed the peel, obtains Lignum Xanthoceratiss kernel, under the conditions of 50 DEG C, dry 8 h, control water content to be less than 8%, pulverize, mistake 60 mesh sieves, load in extraction kettle.40 DEG C of extraction temperature, extracting pressure 28 Mpa, CO2Flow 80 L/h, separating still I temperature is 35 DEG C, separating still I pressure is 25 Mpa, and separating still II temperature is 25 DEG C, and separating still II pressure is 8 Mpa, and extraction time is 150 Min, collects extraction fraction, obtains Lignum Xanthoceratiss seed kernel oil.In extraction kettle, leftover materials are the Lignum Xanthoceratiss kernel medicine containing abundant protein Slag, is available for extracting total triterpene saponinss, and extraction finishes oil content in rear residue and is less than 4%.Prepared Lignum Xanthoceratiss seed kernel oil oil yield is not Less than 70%, through GC-MS detection, unsaturated fatty acid content is up to more than 84%.
Embodiment 2 one kind adopts supercritical CO2Fluid extraction isolation technics prepare the side of the Lignum Xanthoceratiss seed kernel oil of high-quality Method
Take fresh Lignum Xanthoceratiss seed 5 kg, peel off and separate to obtain Lignum Xanthoceratiss kernel, under the conditions of 45 DEG C, dry 10 h, control water content low In 6%, pulverize, cross 30 mesh sieves, load in extraction kettle.45 DEG C of extraction temperature, extracting pressure 35 Mpa, CO2Flow 160 L/h, point It is 40 DEG C from kettle I temperature, separating still I pressure is 10 Mpa, separating still II temperature is 30 DEG C, separating still II pressure is 6 Mpa, extraction Take the time to be 120 min, collect extraction fraction, obtain Lignum Xanthoceratiss seed kernel oil.In extraction kettle, leftover materials are containing abundant protein Lignum Xanthoceratiss kernel medicinal residues, are available for extracting total triterpene saponinss, and extraction finishes oil content in rear residue and is less than 3.6%.Prepared Lignum Xanthoceratiss Seed kernel oil oil yield is not less than 80%, and through GC-MS detection, unsaturated fatty acid content is up to more than 90%.
Embodiment 3 emulsifying molding method prepares Lignum Xanthoceratiss seed kernel oil microcapsule
Concrete grammar step is as follows:
1. adopt supercritical CO2Fluid extraction isolation technics prepare the Lignum Xanthoceratiss seed kernel oil of high-quality
2. the preparation of organic faciess:Take appropriate Lignum Xanthoceratiss seed kernel oil, under 30~120 rpm are stirred continuously, are slowly added into second In acetoacetic ester, ultrasonic and stir and so that it is uniformly dissolved, then add appropriate capsule material ethyl cellulose in solution, continue stirring straight To dissolving, gained suspension is organic faciess;
3. the preparation of aqueous phase:At room temperature, a certain amount of ethyl acetate is added in distilled water, forms ethyl acetate saturation Aqueous solution, then be added thereto to appropriate tween 80, stir to obtain under 30~120 rpm rotating speeds aqueous phase;
4. emulsion process:
By organic faciess under 30~120 rpm mixing speeds, slowly at the uniform velocity it is added in uniform aqueous phase, make oil-in-water (O/W Type) milky solution, keep this rotating speed to stir 30 min, to forming uniform droplet;
5. microcapsule molding:It is slowly dropped into excessive distilled water in emulsion, keep rotating speed in 30~120 rpm, continuously stirred 1 H, with ethyl acetate volatilization, ethyl cellulose separates out and forms microcapsule, is washed 3 times with 5% Diluted Alcohol solution, is dried, obtains final product Wen Guan Fruit seed kernel oil microcapsule.
The Lignum Xanthoceratiss seed kernel oil microcapsule of above-mentioned emulsifying molding method preparation after testing, envelop rate is not less than 45%(GC method, weight Percentage ratio).
Embodiment 4 spray drying technology prepares Lignum Xanthoceratiss seed kernel oil microcapsule
The Lignum Xanthoceratiss seed kernel oil of microcapsule gross weight 30%~40% will be accounted for, with appropriate monoglyceride and soybean phospholipid blended emulsifier (mass ratio 1:1) mix homogeneously prepares the capsule heart;Gelatin and the chitosan compound of microcapsule gross weight 60%~70%, or gelatin will be accounted for With sucrose mixture, or gelatin and cyclodextrin mixtures(Mass ratio 1:1~1:4)It is dissolved in 60 DEG C~90 DEG C of hot water, stirring Uniformly preparation capsule material phase solution;The capsule heart is mutually slowly poured into stirring mixing while hot in capsule material solution, be passed through high pressure homogenizer, 60 DEG C Emulsifying 3 times under the conditions of~80 DEG C, homogenization pressure is usually 10~50MPa, after obtaining the emulsion of uniform particle diameter, in spraying In drying tower, 60 DEG C~150 DEG C of inlet temperature, 70 DEG C~90 DEG C of leaving air temp, feed rate 500~750 ml/h, atomization pressure Power 0.1~2 MPa, is spray-dried, that is, obtain Lignum Xanthoceratiss seed kernel oil microcapsule product, and envelop rate is not less than 85%(GC method, Percentage by weight).
Embodiment 5 fluidization Lignum Xanthoceratiss seed kernel oil microcapsule
At room temperature, arabic gum and polyvinyl alcohol (PVA) mixture of microcapsule gross weight 60%~70% will be accounted for, gelatin is gathered with shell Sugared mixture, or gelatin and sucrose mixture, or gelatin and cyclodextrin mixtures(Mass ratio 1:1~1:4)It is dissolved in 60 DEG C~90 DEG C hot water in, stir preparation capsule material phase solution;The Lignum Xanthoceratiss seed kernel oil of microcapsule gross weight 30%~40% will be accounted for, and appropriate Monoglyceride and soybean phospholipid blended emulsifier (mass ratio 1:1) mix homogeneously prepares the capsule heart;The capsule heart is mutually slowly poured into capsule In material solution, stirring mixing while hot, shears 30 s~2 min with high-shearing dispersion emulsifying machine 10000 rpm, obtains stable O/W Type white Emulsion;Feed velocity 2.5 ml/min, atomizing pressure 0.1~2 MPa, 60 DEG C~150 DEG C of inlet temperature, go out pathogenic wind-warm 70 DEG C~90 DEG C of degree, that is, obtain Lignum Xanthoceratiss seed kernel oil microcapsule product, envelop rate is not less than 75%(GC method, percentage by weight).
Embodiment 6 pressing prepares Lignum Xanthoceratiss kernel fat capsule
A certain proportion of gelatin, glycerol and distilled water are configured in glue pot, under 60~200 rpm mixing speeds, 80 DEG C~ 110 DEG C make it melt, and between vacuum -0.1 below MPa and 80 DEG C~100 DEG C of temperature, carry out 2 h degassings, by above-mentioned glue Liquid puts into couveuse, machine compacting film between 80 DEG C~90 DEG C;Choose the qualified film of compacting and recipe quantity Lignum Xanthoceratiss kernel Oil is pressed into soft capsule by encapsulating machine.By blowing setting at a temperature of 20 DEG C~30 DEG C in net machine of the soft capsule being pressed into, Carry out shaping after setting 3~4 h;Soft capsule after shaping is deoiled with 75% washing with alcohol, is placed in blowing in net machine and 6 hs are dried, After dried soft capsule selected removing scrap rubber capsule, carry out aluminum-plastic packaged.
The preparation of embodiment 7 Lignum Xanthoceratiss seed kernel oil drop pill
Take high-quality Lignum Xanthoceratiss seed kernel oil 25 g, add melting mixing substrate PEG6000 of 75 g:PEG4000 (1:1), stir It is transferred in reservoir after uniformly, airtight and be incubated at 75 DEG C, with dosing pump pill dripping machine dripping from top to bottom, coolant is diformazan Base silicone oil, water dropper bore(Inside/outside footpath):2.1/2.5 mm, drips speed:30 balls/minute, drip away from:8 cm, every ball 25 mg, collect and drip Ball, sucks surface coolant, is dried, obtains final product.
The preparation of embodiment 8 Lignum Xanthoceratiss seed kernel oil cyclodextrin clathrate
First by beta-schardinger dextrin-(β-CD) or HP-β-CD (HP- β-CD) or sulfobutyl ether-beta-cyclodextrin (SEB- β- CD) with distilled water according to 1:6~10 ratio mixing, under the conditions of 16 DEG C~25 DEG C, constant temperature is stirred to dissolve, and is subsequently adding and ring Dextrin mass ratio is 1:4~6 Lignum Xanthoceratiss seed kernel oil, after three is stirred, mixed material is added to colloid mill or ball milling In machine, grind 10~20 min, the material after grinding stands overnight at room temperature, vacuum filtration, under the conditions of 40 DEG C~60 DEG C often Press dry dry, or be dried in 0.1 MPa vacuum under pressure, obtain final product Lignum Xanthoceratiss seed kernel oil cyclodextrin clathrate..

Claims (8)

1. the Preparation method and use of a kind of supercritical fluid extraction Lignum Xanthoceratiss seed kernel oil and its preparation is it is characterised in that super face The concrete technology flow process of boundary's fluid extraction includes:Lignum Xanthoceratiss seed removes the peel to obtain Lignum Xanthoceratiss kernel, under the conditions of 40~50 DEG C dry 6~ 12 h, control water content to be less than 8%, pulverize, cross 10~100 mesh sieves, load in extraction kettle;30~60 DEG C of extraction temperature, extraction pressure Power 25~35 Mpa, CO2Flow 10~180 L/h, separating still I temperature is 35~45 DEG C, and separating still I pressure is 5~20 Mpa, Separating still II temperature is 25~35 DEG C, and separating still II pressure is 2~10 Mpa, and extraction time is 60~200 min, collects extraction Fraction, obtains Lignum Xanthoceratiss seed kernel oil;In extraction kettle, leftover materials are the Lignum Xanthoceratiss kernel medicinal residues containing abundant protein, are available for extracting three Terpene total saponins, extraction finishes oil content in rear residue and is less than 4%;Prepared Lignum Xanthoceratiss seed kernel oil oil yield is not less than 50%, through GC- MS detects, unsaturated fatty acid content is up to more than 75%.
2. the preparation method of a kind of supercritical fluid extraction Lignum Xanthoceratiss seed kernel oil according to claim 1 and its preparation and use Way it is characterized in that, supercritical fluid extraction equipment includes:Filter, refrigeration unit, CO2Effusion meter, intermediate storage tank, CO2High Press pump, blender, heater, extraction kettle, separating still I, separating still II, carry agent fill, carry agent flux meter.
3. the preparation method of a kind of supercritical fluid extraction Lignum Xanthoceratiss seed kernel oil according to claim 2 and its preparation and use On the way, extractant used is carbon dioxide (CO2), 1,1,1,2- tetrafluoroethane, tetrafluoro butane, dimethyl ether, sulfur hexafluoride, third Alkane, butane, the iso-butane mixture of one or more therein.
4. the preparation method of a kind of supercritical fluid extraction Lignum Xanthoceratiss seed kernel oil according to claim 1 and its preparation and use Way is it is characterised in that make medically acceptable various pharmaceutical preparatioies such as by adding various pharmaceutic adjuvants:Soft capsule, micro- Capsule, cyclodextrin bag and the dosage form such as preparation, drop pill.
5. a kind of supercritical fluid extraction Lignum Xanthoceratiss seed kernel oil and its preparation according to claim 4, involved soft capsule, It is characterized in that, softgel shell substrate used includes natural material such as:Gelatin, tragacanth, carrageenan, arabic gum, guar gum, sea Sodium alginate, modified gelatin, agar, pectin, dextrin etc.;Or semi-synthetic high molecular polymer, such as:Hetastarch, hydroxypropyl form sediment Powder, hypo-methoxy pectin, starch succinate, hydroxypropyl methylcellulose, carboxymethyl cellulose, hydroxyethyl cellulose, ethyl hydroxyl Methylcellulose, carboxymethyl locust bean gum etc.;Or synthesising macromolecule copolymer, such as:Polyvinyl alcohol (PVA), Polyvinylpyrrolidone (PVP) series, poloxamer (Poloxamer), Carbomer, polyoxyethylene type compounds, polymethylacrylic acid, carboxy vinyl gather The mixture of one or more of compound;The antioxidant being added in softgel shell, main inclusion:Lysine, glycine, paddy ammonia One of hydrochlorate, oxammonium hydrochloride, benzoic acid, fumaric acid, p- amino benzoic Acid, maleic acid, citric acid, sodium pyrosulfite or several The mixture planted;Other additives being added in softgel shell, mainly include plasticizer, such as:Propylene glycol, Sorbitol;Coloring agent:Oxygen Change ferrum;Opacifier:Titanium dioxide etc..
6. a kind of supercritical fluid extraction Lignum Xanthoceratiss seed kernel oil and its preparation according to claim 4, involved microcapsule, its It is characterised by, capsule material substrate used includes natural material such as:Shitosan, gelatin, arabic gum, osseocolla, natural gum, agar, Sargassum Hydrochlorate, albumin, starch;Semi-synthetic macromolecular material is such as:Methylcellulose, ethyl cellulose, polyvinyl alcohol (PVA), carboxylic first Base cellulose, cellulose acetate, cellulose acetate-phthalate;Synthesis macromolecular material:1. poly- 'alpha '-hydroxy acids, such as polylactic acid (PLA), polyglycolic acid, PLGA (PLGA), poly butyric etc.;2. cross-linked polyester, such as lactide, Poly- (6-caprolactone), Polyalkylcyanoacrylanano etc.;3. poe and polyanhydrides, such as polyamino acid, poly- carbon ester, polypropylene Acid resin, polyamide, the mixture of one or more of polymethyl methacrylate.
7. a kind of supercritical fluid extraction Lignum Xanthoceratiss seed kernel oil according to claim 4 and its preparation, involved ring is pasted Spermatophore and preparation are it is characterised in that the species of cyclodextrin used includes:Alpha-cyclodextrin (α-CD), beta-schardinger dextrin-(β-CD), hydroxypropyl Group-beta-cyclodextrin (HP- β-CD), hydropropyl-y-cyclodextrin (HP- γ-CD), carboxymethyl-beta-cyclodextrin (CM- β-CD), sulphur fourth Base ether-beta-schardinger dextrin-(SEB- β-CD), the mixture of one or more of methyl-β-cyclodextrin (RM- β-CD).
8. a kind of supercritical fluid extraction Lignum Xanthoceratiss seed kernel oil according to claim 4 and its preparation, involved drop pill Agent is it is characterised in that the substrate of described drop pill is poloxamer-188 (Poloxamer-188), PEG-4000 (PEG-4000), PEG-4000 (PEG-6000), xylitol, medical starch, sodium stearate, polyoxyethylene monostearate The mixture of one or more of fat;Instillation coolant is one or more of dimethicone, liquid paraffin, vegetable oil Mixture;Drop pill preparation condition:Medicine and substrate composition are 1:4~1:2,70 DEG C~90 DEG C of fluid temperature, take insulation to drip System, water dropper bore(Inside/outside footpath):2.1/2.5 mm~3.0/5.0 mm, drips speed:20 d/min~30 d/min, drip away from:4~ 10 cm.
CN201610909805.7A 2016-10-19 2016-10-19 Preparation method and use of Xanthoceras sobifoba kernel oil extracted from supercritical fluid and preparation of Xanthoceras sobifoba kernel oil Pending CN106433962A (en)

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Publication number Priority date Publication date Assignee Title
CN107348284A (en) * 2017-08-22 2017-11-17 中国科学院沈阳应用生态研究所 A kind of anti anoxia protein beverage and its preparation and application
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