CN102274246B - Raw material pretreatment method for improving dissolution rate of active ingredients of medicinal plants - Google Patents
Raw material pretreatment method for improving dissolution rate of active ingredients of medicinal plants Download PDFInfo
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Abstract
The invention discloses a raw material gas explosion pretreatment method for improving the dissolution rate of active ingredients of medicinal plants. The method comprises the following steps of: putting materials preimpregnated in water or aqueous solution into a high-pressure container, sealing, introducing a medium, keeping the temperature between 40 and 250 DEG C for 0.5 to 30 minutes, releasing pressure quickly, and discharging the materials in the high-pressure container to a normal-pressure container to obtain materials which are subjected to gas explosion pretreatment, wherein the medium is one or a combination of two of air, carbon dioxide, ozone, liquid nitrogen, nitrogen, water vapor and supercritical CO2. On the basis of the bioactivity of the active ingredients of the medicinal plants, various medium combination gas explosion modes in the low-temperature and high-pressure state are adopted selectively to ensure the treatment strength of the materials, and the dissolution rate of the active ingredients is improved on the premise that the active ingredients are not damaged to improve the utilization rate of raw materials; and the method is quick, simple, economic, high in adaptation degree and wide in selective range, and pollution is avoided, so the method is a significant path for realizing high-value utilization of the medicinal plants.
Description
Technical field
The invention belongs to medicinal plants application, particularly a kind of preprocessing method of raw materials that improves active components in medicinal plant dissolution rate.
Background technology
Under the world trends impact of aged tendency of population, global medical system reform, health care and " back to nature ", traditional medicine range of application and utilization rate in the world improves constantly, space in international market constantly expands, and has worldwide shown good opportunity to develop and boundless development prospect.According to World Health Organization (WHO), estimate, global eighty per cant population is being used or was once using various traditional medicine disease-treatment and health-care at present, and traditional medicine generally all be take medicinal plants as main material.Medicinal plants is the flora that contains the material with certain physiologically active that can prevent and cure diseases.
The chemical composition of medicinal plants can be divided in short: effective ingredient, auxiliary element, invalid components and component of organization.1. effective ingredient: be the material of main pharmacodynamics, general monomeric compound chemically, can represent with molecular formula and structural formula, and have certain physicochemical property, as certain alkaloid, glycosides, volatile oil, organic acid etc.Chinese crude drug often contains a plurality of active ingredients, and a kind of effective ingredient has many-sided pharmacological action, and its mechanism of action is very complicated.What during Chinese medicine extraction, often obtain is " effective site ".Through purity test, not monomeric compound, but mixture, as the total alkaloids containing in extract, total flavones, total glycosides, total volatile oil etc. all belong to effective site.Application effective site is in pharmacology and can represent clinically or partly represent and the curative effect of crude drug or prescription be conducive to bring into play its comprehensive effectiveness, meets the feature of Chinese medicine.2. auxiliary element: refer to that itself is without special efficacy, but can strengthen or relax the material of effective ingredient effect, or be conducive to the leaching of effective ingredient or the material of enhancing preparation stability.3. invalid components: refer to that inanimate object is active.Do not play the material of drug effect.4. suck tissue: refer to that some form crude drug cell or other insoluble substances.Extract and from medicinal raw material, isolate effective ingredient exactly, be directly connected to the content of product effective ingredient, affect the enforcement of inherent quality, clinical efficacy, economic benefit and GMP.In extraction process, lixiviate goes out effective site or effective ingredient to greatest extent, and bottom line lixiviate goes out invalid even harmful material.
In medicinal plants, the content of effective ingredient is generally lower, be present in the vacuole of plant cell more, along with being dried of plant, effective ingredient can be attached on plant cell wall, and plant cell wall is the compact texture consisting of cellulose, hemicellulose, lignin, pectic substance etc.The extraction of effective ingredient generally adopts solvent extraction, and leaching process carries out according to following flow process:: (I) diffusion of solvent from liquid phase main body to material particles surface; (II) solvent is from particle surface to inner diffusion; (III) dissolving of granule interior effective ingredient in solvent; (IV) dissolve rear effective ingredient from granule interior to its diffusion into the surface; (V) effective ingredient is from particle surface to liquid phase main diffusion.Wherein step (I), (V) belong to external diffusion, and step (II), (IV) belong to internal diffusion, and step (III) belongs to course of dissolution.Leaching process is generally to carry out under the condition of additional stirring, liquid phase main body is in eddy current state, boundary region is very thin, therefore resistance of liquid mass transfer will be far smaller than solid phase resistance to mass tranfer, thereby internal diffusion is the control step of whole leaching process, that is to say that effective ingredient exchanges the rate-limiting step that becomes whole leaching process by cell wall, cell wall is the barrier of extracts active ingredients.Therefore, no matter adopt which kind of extracting method, the destructiveness to plant cell, will directly affect extraction efficiency and following process process.
Traditional method generally adopts mechanical crushing method to carry out break process to material, but because plant cell has very large resistance for the effect of external force, so mechanical treatment is limited to the destructiveness of plant cell.And if plant medicine is crushed to micron order, energy consumption increase, cost raising.Steam explosion technology is widely used in the industries such as papermaking, feedstuff processing, extract drugs in recent years, it utilizes high-temperature high-pressure steam to infiltrate among the hole and cell of material tissue, then moment high speed pay-out out, the mechanical force producing can produce mechanical tear effect to a certain extent, thereby destroys material.This method has been integrated chemical hydrolysis and physical pulverization effect, can within the short time (a few minutes), effectively destroy the compact texture of wood fibre, improves extraction efficiency.
The simple employing air of the application of existing steam explosion technology in medicinal plants is extracted is coupled and carries out steam explosion processing with water vapour, as Chen Hongzhang etc. first passes into air 5-10kg/cm in the air-vapor coupling vapor exploding wall extracting method (200410090699.1) of patent ephedrine discloses steam-explosion jar
2, then pass into water vapour 10-18kg/cm
2, steam explosion is processed 2-20 minute, can make the extraction ratio of ephedrine obviously improve.But the kind of effective ingredient is different in medicinal plants, preprocessing process should design according to the characteristic of raw material.Studying for many years on the basis of medicinal plants property of raw material and comprehensive utilization thereof, a kind of preprocessing method of raw materials that improves active components in medicinal plant extraction ratio is proposed, under the air blasting associated treatment effect that medicinal plants is combined at multimedium, by half fiber degradation in Medicinal Plant Cell wall, lignin is softening, Partial digestion, fibre structure is loose, form significant loose structure, inner specific surface area enlarges markedly, improve internal diffusion speed in material leaching process, thereby improving medicinal plants active component dissolution efficiency.
Summary of the invention
The utilization of medicinal plants is Chinese conventional industries, and under the world trends impact of aged tendency of population, global medical system reform, health care and " back to nature ", development prospect is increasingly extensive.The stripping utilization of the effective ingredient in medicinal plants, must break through the barrier action of Medicinal Plant Cell wall, improves internal diffusion speed in effective ingredient process in leaching.Traditional method generally adopts mechanical crushing method to carry out break process to material, but because plant cell has very large resistance for the effect of external force, so mechanical treatment is limited to the destructiveness of plant cell.And if plant medicine is crushed to micron order, energy consumption increase, cost raising.For the problems referred to above, a kind of preprocessing method of raw materials that improves active components in medicinal plant dissolution rate is proposed, by medicinal plants under the air blasting associated treatment effect of air blasting or multimedium combination, by half fiber degradation in Medicinal Plant Cell wall, lignin is softening, Partial digestion, fibre structure is loose, form significant loose structure, inner specific surface area enlarges markedly, and improves internal diffusion speed in material process in leaching, thereby is improving medicinal plants active component dissolution efficiency, save the consumption of medical material, improve medicinal plants comprehensive utilization value.
Its concrete technical scheme is:
By medicinal plants raw material water or aqueous solution, at 4-50 ℃, soak in advance 0-48h; Material after preimpregnation is placed in to high-pressure bottle, and sealing, passes into medium, makes temperature of charge maintain 0.5-30min at 40-250 ℃, and then quick pressure releasing, is discharged into the material of processing in high-pressure bottle tank in non-pressure vessel, obtains the material after steam exploded pretreatment.
Described aqueous solution comprises dilution 1-100 vinegar doubly, dilution 1-50 Chinese liquor doubly, the sodium carbonate that yellow wine and mass concentration are 0.1-5% and sodium bicarbonate solution.
Described medium is air, carbon dioxide, ozone, liquid nitrogen, nitrogen, water vapour, supercritical CO
2in a kind of or combination of any two kinds.
In material after air blasting is processed, the extraction of effective ingredient is extracted in a conventional manner.
Material after air blasting is processed is effective component extracting directly, also can pulverize or micronizing for food, field of medicaments.
Beneficial effect of the present invention is:
1, air blasting of the present invention is to have certain difference with the steam explosion technology that the medicinal plants raw material of report adopts at present, the medium main body that steam explosion technology adopts is water vapour, as the steam explosion of the Herba Ephedrae of the reports such as Chen Hongzhang is processed, what adopt is first to pass into certain air, pass into again water vapour, material maintains the regular hour and carries out steam explosion processing under water vapor acting, and the air blasting medium described in the present invention is air, carbon dioxide, ozone, liquid nitrogen, nitrogen, water vapour, the combination of a kind of in supercritical CO 2 or any two kinds, the low temperature designing according to active components in medicinal plant biological activity, air blasting mode under high pressure conditions, can be by single medium if carbon dioxide or multimedium be as first passed into after air
2, adopt under air blasting or the collaborative Effect of Pretreatment of multimedium combination air blasting, half fiber degradation in Medicinal Plant Cell wall, lignin is softening, Partial digestion, fibre structure is loose, forms significant loose structure, and inner specific surface area enlarges markedly, improve internal diffusion speed in material effective ingredient process in leaching, thereby improve the dissolution rate of medicinal plants active component.
3, adopt the collaborative Effect of Pretreatment of air blasting multimedium combination air blasting, the effective ingredient in raw material is carried out to the protection of the low temperature measures etc. of many combinations, improve the dissolution efficiency of active components in medicinal plant but do not damage the effective ingredient in raw material.
4, air blasting or the collaborative pretreatment medicinal plants of multimedium combination air blasting, be a kind of quick, simple, economic pretreatment mode.
5, preprocess method provided by the invention, is a kind of pretreatment mode that can design air blasting medium according to the physical property feature of medicinal plants raw material mix characteristic, effective ingredient, and adaptedness is high, and the range of choice is wide.
6, the condition in air blasting process is the condition of Maillard reaction in medicinal plants, maillard reaction product be increased in the curative effect that can strengthen to a certain extent Chinese medicine.
7, the medicinal plants after air blasting is processed, can be directly used in effective component extracting, also can be directly used in next step processing of medicinal plants, as being applied to the industry such as food, medicine after direct or pulverization process, prepares the product that is rich in active component.
The specific embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1: air blasting is processed Semen Armeniacae Amarum and extracted amygdaloside
By being rich in the medicinal plants Semen Armeniacae Amarum of oils, according to the quality of over dry medical material and the water ratio of 1: 1, add water, then immersion treatment 30min at normal temperatures; Material after immersion treatment, as in steam-explosion jar, is passed into air, make temperature in tank reach 100 ℃, carry out steam explosion processing after maintaining 5min; Collect the material after steam explosion, extract respectively the Semen Armeniacae Amarum glycosides in the Semen Armeniacae Amarum of steam explosion front and back, adopt silver nitrate titration method to measure Semen Armeniacae Amarum content, more not gas-explosive material raising 15.32% of the Semen Armeniacae Amarum glycosides extraction ratio of material after steam explosion.
Embodiment 2: air blasting is processed Radix Zanthoxyli and extracted nitidine chloride
Radix Zanthoxyli medical material is chopped into the fragment of 3-5cm, according to the quality of over dry Radix Zanthoxyli medical material and the water ratio of 1: 1, adds water, then immersion treatment 60min at normal temperatures; Material after immersion treatment, as in steam-explosion jar, is passed into water vapour, make temperature in tank reach 200 ℃, carry out steam explosion processing after maintaining 5min; After steam explosion is processed, material adds the organic solvent of 6 times of its oven dry weights, extracts each 3.0h, merge extractive liquid, under fluidized state 3 times; By extracting solution reduction vaporization, obtain precipitate, in precipitate, add the HCl solution of pH 2 to mix, be extracted with ethyl acetate and remove non-alkaline components, water is adjusted to pH 10 with NaOH afterwards, produces precipitation simultaneously, removes precipitation and is extracted with ethyl acetate remaining water again and obtains Radix Zanthoxyli alkaloid part, it is 0.52% that the Radix Zanthoxyli alkaloid of weighing extracts yield, and after steam explosion, the specific surface area of Radix Zanthoxyli material is 0.95m
2/ g, and the specific surface area of former beginning and end steam explosion Radix Zanthoxyli raw material is 0.68m
2/ g, the extraction yield of former beginning and end gas-explosive material nitidine is 0.31%.
Embodiment 3: Folium Eucommiae chlorogenic acid extracting is processed in air blasting
Get Folium Eucommiae medical material 500g, Folium Eucommiae medical material is added to acetic acid water (ratio of acetic acid and water is 1: 100) according to the quality ratio of 1: 2 of over dry medical material and acetic acid water, then immersion treatment 60min at normal temperatures, material after immersion treatment is placed in to steam-explosion jar, passes into carbon dioxide, make temperature in tank reach 80 ℃, carry out steam explosion processing after maintaining 15min, after steam explosion is processed, material or routine are crushed to the water that 40 object materials add 5 times of its oven dry weights, extract 3 times each 50min, merge extractive liquid, at 40 ℃, by extracting solution concentrating under reduced pressure, the ethyl acetate extracting twice that adds 3 times of concentrated solutions, obtain ethyl acetate layer, wherein add the neutralization of 3%NaOH liquid to make the chlorogenic acid in ethyl acetate enter water, after aqueous phase separation, with concentrated hydrochloric acid acid, separate out chlorogenic acid precipitation again, after precipitate and separate with the incomplete dissolving-recrystallization of a small amount of ethyl acetate, be drying to obtain chlorogenic acid crude product chlorogenic acid crude product and deionized water with the solid-liquid ratio of 1: 3, at the high pure nitrogen that passes into continuously 99.99%, keep malleation, under the condition of pressure reduction > 5Pa, dissolve and add 8% activated carbon to be heated to 60 ℃ and reflux 0.5 hour, filter, crystallisation by cooling, crystallization is cleaned with the analytical pure acetone of 5 times, vacuum drying obtains high-purity chlorogenic acid.Weigh and can obtain chlorogenic acid 14.05g, and material after conventional pulverization process can extract to obtain chlorogenic acid 10.25g, extracts yield and has improved 33.17%.
Embodiment 4: air blasting Processing Ag Folium Pruni extracts ginkgetin
According to the quality of over dry Folium Ginkgo and the sodium bicarbonate aqueous solution ratio of 1: 2, add sodium bicarbonate aqueous solution (2%), then immersion treatment 60min at normal temperatures; Material after immersion treatment, as in steam-explosion jar, is passed into ozone, make temperature in tank reach 150 ℃, carry out steam explosion processing after maintaining 30min; Then quick pressure releasing, is discharged into the material of processing in steam-explosion jar in non-pressure vessel, obtains the material after steam exploded pretreatment.Steam explosion Folium Ginkgo and original untreated Folium Ginkgo are crushed to 60 orders with plant pulverizer, by 20: 1 (mL/: g) add 70% alcoholic solution of liquid-solid ratio, in 85 ℃ of heating in water bath reflux, extract, 2h, filter, reclaim filtrate, filtering residue repeats to extract 3 times as stated above, merging filtrate, the extraction ratio of measuring Ginkgo total flavones in filtrate is: 2.18g total flavones/100g raw material, and original for the extraction ratio of gas-explosive material total flavones be 112g total flavones/100g raw material; The specific surface area of gas-explosive material is 0.5139m
2/ g, and the specific surface area of initial material is 0.4524m
2/ g.
Embodiment 5: air blasting Dioscorea zingiberensis is extracted diosgenin
Get Dioscorea zingiberensis 500g, be cut into 5-10cm section; Just broken raw material is dropped in steam-explosion jar, at 115 ℃ of steam pressures, process 4min; In material after steam explosion is processed, add saccharifying enzyme (80U/g steam explosion siccative), cellulase (10U/g steam explosion siccative), after 55 ℃ of water bath heat preservation saccharifying 30min, be cooled to 35 ℃, add 0.1% (NH
4)
2sO
4, 0.1%KH
2pO
4and 0.15% yeast after activation, under 35 ℃ of conditions, carrying out anaerobic fermentation 60h afterwards, ethanol is collected in distillation; Solid state fermentation slag is dropped into steam-explosion jar for the second time, at 230 ℃, process 15min, collect the material of steam explosion for the second time, 80 ℃ of dried; The ratio that is 1/12 according to dried material quality/petroleum ether volume adds petroleum ether, at 85 ℃, reflux, extract, 6h, filtered while hot, collect filtrate, concentrated, crystallizing and drying, obtain diosgenin 6.43g, the Dioscorea zingiberensis material of processing without air blasting adopts the extraction ratio of traditional method diosgenin to improve 25%; And the Dioscorea zingiberensis material that said process is processed has fully utilized the starch in Dioscorea zingiberensis, fiber and diosgenin composition, realizes the comprehensive utilization of Dioscorea zingiberensis resource.
Embodiment 6: Fructus Lycii is processed in air blasting
Fructus Lycii raw material is added to yellow wine soak at room temperature 24h, be placed in steam-explosion jar, pass into supercritical CO 2, holding temperature is at 95 ℃ of lasting 5min, then quick pressure releasing, is discharged into material in non-pressure vessel, obtains the Fructus Lycii material after air blasting, this material directly can be used for to infusion beverage, the efficiency that in Fructus Lycii, effective ingredient discharges doubles than gas-explosive material not.
Embodiment 7: air blasting is processed Herba Apocyni veneti and extracted flavone
According to the quality of over dry Herba Apocyni veneti and the distilled water ratio of 1: 1, add distilled water, then immersion treatment 60min at 30 ℃; Material after immersion treatment, as in steam-explosion jar, is passed into water vapour, make temperature in tank reach 180 ℃, carry out steam explosion processing after maintaining 10min; Then quick pressure releasing, is discharged into the material of processing in steam-explosion jar in non-pressure vessel, obtains the material after steam exploded pretreatment.Herba Apocyni veneti raw material after steam explosion is processed carries out the combing classification of fiber, and the long fibre obtaining is for the preparation of textile fiber material, and fiber fines is partly for extracting flavone, the material that more steam explosion is not processed, and flavone extraction ratio has improved 15.4%.
Claims (1)
1. a raw material air blasting preprocess method that improves active components in medicinal plant dissolution rate, is characterized in that comprising the following steps: by medicinal plants raw material water or aqueous solution, at 4-50 ℃, soak in advance 0-48h; Material after preimpregnation is placed in to high-pressure bottle, and sealing, passes into medium, makes temperature of charge maintain 0.5-30min at 40-250 ℃, and then quick pressure releasing, is discharged into the material of processing in high-pressure bottle tank in non-pressure vessel, obtains the material after steam exploded pretreatment;
Described aqueous solution comprises dilution 1-100 vinegar doubly, dilution 1-50 Chinese liquor doubly, the sodium carbonate that yellow wine and mass concentration are 0.1-5% and sodium bicarbonate solution;
Described medium is air, carbon dioxide, ozone, liquid nitrogen, nitrogen, water vapour, supercritical CO
2in a kind of or combination of any two kinds.
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| CN105079467B (en) * | 2014-05-16 | 2018-11-16 | 华中科技大学 | A kind of extracting method of roxburgh anoectochilus terminal bud and its application of extract |
| CN104152262A (en) * | 2014-07-31 | 2014-11-19 | 北京中科百瑞能工程技术有限责任公司 | Method for co-producing eucommia seed oil, eucommia rubber and eucommia extract by refining eucommia fruits through steam explosion |
| CN105907736A (en) * | 2016-05-05 | 2016-08-31 | 王美岭 | Supercritical CO2 ginger oil extraction method and special composite catalyst thereof |
| CN106071552A (en) * | 2016-06-23 | 2016-11-09 | 曾凡跃 | A kind of Pitaya Flower, Flos Rosae Rugosae composite beverage and preparation method thereof |
| CN106269143A (en) * | 2016-08-31 | 2017-01-04 | 华南农业大学 | A kind of Chinese crude drug preprocess method |
| CN106309228A (en) * | 2016-09-07 | 2017-01-11 | 文山金七药业有限公司 | Toothpaste for night use and preparation method thereof |
| CN109453414A (en) * | 2018-09-26 | 2019-03-12 | 南阳市中心医院 | A kind of postoperative anti-infectious dressing of liver and gall surgical department |
| CN109432361A (en) * | 2018-12-21 | 2019-03-08 | 安徽东盛友邦制药有限公司 | A kind of preparation method improving antiviral oral liquor effective component |
| CN111285722A (en) * | 2020-02-25 | 2020-06-16 | 珠海十亿人社区农业科技有限公司 | Preparation method of fruit and vegetable organic fertilizer and fruit and vegetable organic fertilizer |
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| CN101797288B (en) * | 2009-02-11 | 2011-09-07 | 中国科学院过程工程研究所 | Method for preparing granular herbal pieces prepared for decoction through steam explosion of monkshood |
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