CN108261418A - The preparation and drying means that a kind of pachymaran dissipates - Google Patents

The preparation and drying means that a kind of pachymaran dissipates Download PDF

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CN108261418A
CN108261418A CN201611263391.1A CN201611263391A CN108261418A CN 108261418 A CN108261418 A CN 108261418A CN 201611263391 A CN201611263391 A CN 201611263391A CN 108261418 A CN108261418 A CN 108261418A
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pachymaran
drying
extraction
dissipates
poria cocos
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CN108261418B (en
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张卫元
李硕
张靖
曾勇
朱秀高
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Wuhan Sheng Sheng Biological Polytron Technologies Inc
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
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    • 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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Abstract

The invention belongs to technical field of traditional Chinese medicine pharmacy, specifically disclose preparation and drying means that a kind of pachymaran dissipates, are a kind of using Poria cocos as raw material, prepare and be dried to obtain the method that pachymaran dissipates.The present invention includes extraction step, desalting steps, drying steps; using sodium hydroxide solution or sodium bicarbonate solution stirring extraction; compared to traditional water refluxing extraction ethanol precipitation or ethanol reflux extraction; greatly reduce consuming and the energy consumption of organic reagent; production cycle and cost are saved, and conducive to environmental protection.It in drying steps, after constant pressure and dry, then is dried under reduced pressure to obtain the method for pachymaran extract, solve since spray-drying efficiency is low, product quality is bad caused by poria polysaccharide water soluble is poor, is not easy to form homogeneous system in water the problems such as.The application simple process is easy, conducive to industrialized production.

Description

The preparation and drying means that a kind of pachymaran dissipates
Technical field
The invention belongs to technical field of traditional Chinese medicine pharmacy, and in particular to one kind prepares using Poria cocos as raw material and drying obtains Fu The method that Siberian cocklebur polysaccharide dissipates.
Background technology
In recent years, in animal husbandry in the prevalence of the eruption and prevalence that infectious disease still occurs after vaccine inoculation, Yi Jiyong The phenomenon that dose is gradually increased and ideal therapeutic effect is not achieved.This phenomenon is largely because long-term a large amount of abuses Drug and unreasonable vaccine inoculation, cause livestock and poultry body's immunity decline and caused by adverse consequences.In animal productiong, The immunity of animal how to be improved so as to reduce its incidence, and then improves its economic benefit, it has also become relevant expert and cultivation The problem of family growing interest.It was verified that taking effective means, activating immune system enhances the disease resistance of body, can make poultry The immune response of higher level can be obtained after fowl body vaccine inoculation, enhances the immune effect of vaccine.
Immunopotentiator can enhance animal immune function, improve the immune effect of animal disease resistant ability and vaccine, thus It has broad prospects in prevention and control animal sexually transmitted disease.At present, chemicals para-immunity reinforcing agent research field obtains Larger progress, has played the sound development of animal husbandry positive.But these chemicals immunopotentiators are not With degree, there is reduce breeding performonce fo animals or even have toxic side effect and there are medicament residue problem, and then endanger people The health of class, therefore the research of Chinese medicine immunity enhancer is increasingly subject to the concern of people.
Poria cocos Poriacocos (Schw.) Wolf is the dry sclerotia of On Polyporaceae Poria cocos, and clinical practice history is swung Long, it cures and writes first recorded in China's allusion《Sheng Nong's herbal classic》, record in version over the years《Pharmacopoeia of People's Republic of China》.Traditional Chinese medicine is recognized For, Poria cocos tonifying Qi benefit member, eliminating pathogen to support vital qi.
Pachymaran (Poria Wolf Polysaccharides, PWP) is considered as the main work in tuckahoe extracts Property ingredient, there are the multiple biological activities such as antitumor, antiviral and enhancing is immune.Numerous studies show tuckahoe extracts total starches There is immunoregulation effect to immune system, pachymaran to the specificity and nospecific immunity of body, humoral immunity with it is thin Born of the same parents, which are immunized, wide influence.In humoral immunity, pachymaran can rise content of immunoglobulin IgG;Exempt from cell In terms of epidemic disease, pachymaran can activating macrophage, enhance the phagocytic activity of phagocyte.Many experiments show pachymaran It can enhance cell immune response in vitro in vivo, stimulate the conversion of T cell, experiment in vitro can enhance lymphocyte activity 20-28 times;Can induce bone-marrow-derived lymphocyte secretory antibody, promote antibody level of serum, can raise IL-1, IL-2, IL-6, IL-10, The expression of the cell factors such as IFN-γ, TNF-α, and inhibit the expression of immunosuppressor TGF-B;Pachymaran can also pass through simultaneously P38 kinase activator mouse macrophage NF- к B/Rel, induce the expression of NO.
Present technology is based on the various pharmacological activity of pachymaran, develops and has prepared pachymaran and dissipates.And according to Pharmacology and clinical effectiveness use it for enhancing animal immune function, it is horizontal to improve vaccine antibody.
At present, for from Poria cocos extraction prepare pachymaran and there are some open to report, but there are certain deficiency, examples Such as:
Wang Xuequn is in 2016 in publication number CN106046192A, entitled " a kind of technique that polysaccharide is extracted from Poria cocos " Patent application in choose Poria cocos raw material ultra-fine grinding and obtain Poria cocos powder, centrifuged after water ultrasonic wave extraction, using complex enzyme zymohydrolysis point From filtrate is obtained, except pachymaran concentrate is concentrated to give after deproteinized, spray drying obtains pachymaran, and column layer is carried out after ultrafiltration Purifying pachymaran is analysed to obtain, is freeze-dried, obtains pachymaran.But this method uses ultrasonic extraction, is not easy industrialization amplification life Production, and obtained polysaccharide is obtained into micromolecular polysaccharide with complex enzyme for hydrolyzing, but it is more to have no relevant theories integration small molecule Poria cocos Sugar has better bioactivity.
Liu Zhimou in 2015 publication number CN105639617A, it is entitled " comprehensive exploitation of Poria cocos a kind of and application Poria cocos sclerotium crushing and water-adding is impregnated refluxing extraction filtering by application in the patent of method and its new application ", and extracting solution is concentrated and dried Obtain water-soluble pachymaran;The extraction of filter residue sodium hydroxide solution filters, and filter residue is washed to neutrality and is used to prepare dietary fiber, filtrate PH value is adjusted to faintly acid, filtration drying obtains Poria cocos total triterpene and alkali solubility pachymaran mixture, and it is water-soluble to add in ethyl alcohol after dry In liquid, dissolution filter obtains Poria cocos total triterpene alcoholic solution and alkali solubility pachymaran solid;By alkali solubility pachymaran washing and drying To obtain the final product;The alcoholic solution of Poria cocos total triterpene is concentrated and dried, obtains Poria cocos total triterpene.This method is although it is contemplated that each effective in Poria cocos Component, but it is unfavorable for actual production operation, process is cumbersome, high energy consumption.
Wang Anguo is equal to 2015 in publication number CN105132491A, entitled " a kind of extracting method of pachymaran " After Poria cocos is crushed in patent application plus water expansion, addition saccharomycete and lactic acid bacteria ferment, zymotic fluid are uniformly mixed, is added Enter complex enzyme formulation hydrolysis, after alcohol precipitates, sediment is spray-dried to obtain finished product.This method is using the side such as fermentation, enzyme hydrolysis Method hydrolyzes pachymaran, and process is relatively complicated, and since by a large amount of enzyme hydrolysis, polysaccharide component is largely by water It solves as ingredients such as monosaccharide and disaccharides, has lost the pharmacological activity of polysaccharide, therefore pachymaran bioactivity exists obtained by this method Certain query.
Text is inherited in 2015 in publication number CN105061627A, the patent Shen of entitled " extracting method of pachymaran " Please in Poria cocos ethyl alcohol is extracted, filter residue water carries, and collects filtrate, and by filtrate concentrated extract, ethanol precipitation centrifuges to obtain precipitation;It will be heavy Form sediment absolute ethyl alcohol, acetone successively washs respectively, by the distillation water dissolution of the precipitation after washing, crosses molecular cut off as in 60,000 Empty fiber membrane, collect concentrate, then by concentrate cross molecular cut off be 100,000 hollow-fibre membrane, collect permeate from The heart, filtering, takes filtrate spare;Filtrate is taken to be spray-dried, as pachymaran.This method is relatively cumbersome using process, using second Alcohol extracting and the method for membrane filtration, process costs are higher, and since obtained macromolecular polysaccharide water solubility is bad, and spraying is dry Dry process yield is relatively low.
Yuan Juan is equal to 2014 in publication number CN104208107A, a kind of entitled " tuckahoe extracts and preparation method thereof And application " patent application in Poria cocos is pulverized and sieved, with ethyl alcohol mixing in proportion;It is placed in Microwave Extraction Equipment and carries out microwave Extraction;Filtering with microporous membrane, filter residue discard, and merging filtrate is concentrated up to liquid tuckahoe extracts or by filtrate, is drying to obtain admittedly State tuckahoe extracts.The Microwave Extraction that is used in this method is all difficult to amplify production for processes such as air filter membrane filtrations, and process into This and equipment investment are high.
Song Decheng in 2008 publication number CN101757045A, entitled " a kind of preparation method of pachymaran " it is special Profit application in method be:It is crushed after weighing Poria cocos slice, adds water, circumfluence distillation, ethanol precipitation after reduced pressure, it is heavy to collect Shallow lake obtains pachymaran.Although water extraction ethanol precipitation is the conventional method for extracting the macromolecular substances such as polysaccharide, but due to water Dissolubility pachymaran only accounts for about the 4% of polysaccharide weight, and most of is water-insoluble polysaccharide, therefore it is more that this method is used to prepare Poria cocos Sugar, resource utilization are extremely low.
Invention content
For the deficiencies in the prior art, the preparation dissipated the present invention provides a kind of pachymaran and drying means, Solve organic reagent in existing water refluxing extraction ethanol precipitation or ethanol reflux extraction consuming is big and high energy consumption Problem solves the problems, such as that existing ultrasonic extraction, Enzymatic Extraction are not easy to industrialized production.Invent the constant pressure and dry used Afterwards, it then is dried under reduced pressure to obtain the method for pachymaran extract, solves existing spray-drying efficiency is low, product quality is bad etc. Problem, simple process is easy, conducive to industrialized production.
The preparation and drying means, step that a kind of pachymaran of the present invention dissipates are as follows:
(1) extraction step:Poria cocos block is taken, 14~80 mesh is crushed and sieves to obtain Poria cocos powder, adds aqueous slkali, after stirring extraction, 800 ~2400rpm centrifuges to obtain supernatant, and supernatant is adjusted with acid pH value, and after standing 30~90min, 800~2400rpm centrifugations obtain Sediment;
(2) desalting steps:The sediment that extraction step (1) is taken to obtain adds water, is stood after stirring, 800~2400rpm from Gains in depth of comprehension repeat above-mentioned desalination processes 2~4 times to polysaccharide desalination product is precipitated as;
(3) drying steps:It takes the polysaccharide desalination product that desalting steps (2) obtain, after constant pressure and dry, then is dried under reduced pressure, obtains To pachymaran extract, gained pachymaran extract be crushed into 40~100 mesh sieve, pachymaran is obtained and dissipate.
Preferably, in the extraction step (1), the aqueous slkali is:0.1~1.5mol/L sodium hydroxide solutions or 0.2 ~2.0mol/L sodium bicarbonate solutions, it is 10~30mL to add in volume with Poria cocos powder mass ratio:1g;The stirring extraction, mistake Cheng Wei:Speed of agitator 40~100rpm stirs 20~60min at 25~70 DEG C;The supernatant is adjusted with acid pH value, process For:One kind in 4~10mol/L hydrochloric acid solutions or 6~12mol/L sulfuric acid solutions is added in supernatant, adjusts pH value to 6.5 ~9.0;
Preferably, in the desalting steps (2), described plus water is:Add in the deposit that volume is obtained with extraction step Amount is than being 3~6L:1kg;It is stood after the stirring, process is:After adding water, 20~40min is stirred at 25~60 DEG C, stirring turns 40~100rpm of speed stands 20~60min after stirring;
Preferably, in the drying steps (3), the constant pressure and dry is:60~90 DEG C of drying temperature, drying time 2~5 Hour;It is described be dried under reduced pressure for:Dry vacuum degree -0.06~-0.1Mpa, 50~80 DEG C of drying temperature, drying time 1.5~3 Hour.
Compared with prior art, the advantages of the present invention are:
The present invention discloses using Poria cocos as raw material and a kind of prepares and dry and to obtain the method that dissipates of pachymaran.The present invention uses Sodium hydroxide solution or sodium bicarbonate solution stirring extraction, compared to traditional water refluxing extraction ethanol precipitation or alcohol reflux Extraction method greatly reduces consuming and the energy consumption of organic reagent, saves production cycle and cost, and conducive to environmental protection, go back Solve the problems, such as that existing ultrasonic extraction, Enzymatic Extraction are not easy to industrialized production.
The common drying means of traditional Chinese medicine extraction concentrate mainly has constant pressure and dry, is dried under reduced pressure, is spray-dried, in early period In research, we are respectively adopted pachymaran extract three kinds of modes and (detailed in Example 7,8,9) are dried, and as a result show Show, spray drying drying time is most short, but yield is minimum, may be sprayed due to the poor dispersion of pachymaran in water It will appear serious wall built-up phenomenon during mist, it is low so as to cause yield;The constant pressure and dry time is relatively short, and product yield is high, But may occur " boiling Poria cocos " situation due to prolonged high temperature, lead to finished color dull gray, hard, crushing is not thorough;Decompression Dry product yield is higher, and quality is good, but may be high due to dry Poria cocos water content at the beginning, even if vacuum pump is persistently evacuated, Drying box wall hanging droplet, humidity is too big in drying box, in " imperfect vacuum situation ", rate of drying is caused to reduce, and due to object Expect the aqueous height in surface, drying is caused to be not thorough.
Based on the above results, it after the constant pressure and dry that the present invention uses, then is dried under reduced pressure to obtain the side of pachymaran extract Method is solved since poria polysaccharide water soluble is poor, is not easy to form homogeneous system in water and leads to that spray-drying efficiency is low, normal pressure The problems such as product quality is bad when dry, drying is not thorough when being dried under reduced pressure.Simple process is easy, conducive to industrialized production.
Specific embodiment
Applicant in conjunction with specific embodiments further elaborates technical scheme of the present invention below.
The preparation and drying means, step that a kind of 1 pachymaran of embodiment dissipates are as follows:
(1) extraction step:Poria cocos block is taken, 80 mesh is crushed and sieves to obtain Poria cocos powder 500g, add 1.5mol/L sodium hydroxide solutions 15L, it is 30mL to add in volume with Poria cocos powder mass ratio:1g stirs 60min, speed of agitator 100rpm at 50 DEG C;Stirring extraction knot Shu Hou, 2400rpm centrifuge to obtain supernatant, and 6mol/L hydrochloric acid solutions are added in supernatant, adjust pH value to 9.0, stand 90min Afterwards, 800rpm is centrifuged, and obtains sediment 3.15kg;
(2) desalting steps:The sediment 3.15kg that extraction step (1) is taken to obtain adds water 18.9L, adds in volume with carrying It is 6L to take the sediment mass ratio that step obtains:1kg stirs 20min at 60 DEG C, and speed of agitator 100rpm is stood after stirring 20min;800rpm, which is centrifuged, to be precipitated;
Precipitation repetition is above-mentioned to add water (each amount of water is 18.9L) desalination processes 2 times, obtains polysaccharide desalination product 2.85kg;
(3) drying steps:The polysaccharide desalination product 2.85kg that desalting steps (2) obtain is taken, constant pressure and dry 5 hours is dry Temperature 60 C;Then it is dried under reduced pressure under vacuum degree -0.085Mpa 3 hours, 50 DEG C of drying temperature, obtains pachymaran extraction Object is crushed and is sieved with 100 mesh sieve, and is obtained pachymaran and is dissipated 225g.
Polyoses content, yield and its pharmacological activity that pachymaran obtained by the present embodiment dissipates measure:Polyoses content is 85.3%, yield 45.0%.Its activity enhanced immunosuppressed mice immunocompetence is measured, assay method is as follows:SPF grades Healthy kunming mice 40, half male and half female, 18-22g are randomly divided into 4 groups, every group 10, successive administration 14 days.Blank group:It fills The physiological saline of stomach 0.9%, every 0.3ml/d, continuous 14d;Model group (hydrocortisone group):Preceding 4d and the same physiology salts of rear 4d Water group is only given 0.9% physiological saline, and every 0.3ml/d, 5-10d are subcutaneously injected hydrocortisone, every 0.3ml/d, (dosage 50mg/kg), and 0.9% physiological saline is given, every 0.3ml/d;Positive controls (levamisol group):Preceding 4d With rear 4d gavage levamisol (dosage 5mg/kg), hydrocortisone (dosage 50mg/kg) is subcutaneously injected in 5-10d, And gavage levamisol (dosage 5mg/kg), every 0.3ml/d;Trial drug group (pachymaran dissipates group):Preceding 4d and rear 4d Gavage pachymaran dissipates (300mg/kg), and hydrocortisone (dosage 50mg/kg), and gavage Fu is subcutaneously injected in 5-10d Siberian cocklebur polysaccharide dissipates (300mg/kg), every 0.3ml/d.Next day after drug withdrawal takes out abdominal cavity after 5% chicken red blood cell 1ml, 2h is injected intraperitoneally Emigrated cell, acetone-methanol (1:1) fixed poststaining, calculating phagocytic percentage, (phagocytic percentage (%)=100 macrophage is thin The macrophage phagocyte number/100 macrophage * 100% of chicken red blood cell is swallowed in born of the same parents).It is measured to gulp down immunosuppressed mice Phagocyte swallows chicken red blood cell ability;It 12 hours after the last administration, plucks eyeball and takes blood, serum is detached, by kit specification side Method measure interleukin 2 (IL-2) and tumor necrosis factor (TNF-α) content, measure its immunosuppressed mice is immunized because The influence of son;And thymus gland, spleen is taken to measure organ index (organ weights/weight * 100).It is measured to exempt from immunosuppressed mice The influence of epidemic disease organ.Result of the test shows, with hydrocortisone model group (phagocytic rate 30.20%, index and spleen index 0.25, The content that thymus index is 0.16, IL-2 is 7.62pg/mL, and the content of TNF-α is 6.03pg/mL.) compare, it can effectively facilitate The phagocytic activity of phagocyte, phagocytic rate 49.52%;Effectively facilitate the raising of index and spleen index and thymus index, index and spleen index It is 0.28, thymus index 0.19;Effectively promote the secretion of IL-2 and TNF-α, the content in mice serum is respectively IL-2 12.15pg/mL with TNF-α 41.68pg/mL.
The preparation and drying means, step that a kind of 2 pachymaran of embodiment dissipates are as follows:
(1) extraction step:Poria cocos block is taken, 14 mesh is crushed and sieves to obtain Poria cocos powder 1000g, add 0.1mol/L sodium hydroxide solutions 10L, it is 10mL to add in volume with Poria cocos powder mass ratio:1g stirs 40min, speed of agitator 40rpm at 25 DEG C;Stirring extraction knot Shu Hou, 800rpm centrifuge to obtain supernatant, and 10mol/L hydrochloric acid solutions are added in supernatant, adjust pH value to 6.5, stand 30min Afterwards, 2400rpm is centrifuged, and obtains sediment 5.95kg;
(2) desalting steps:The sediment 5.95kg that extraction step (1) is taken to obtain adds water 17.85L, adds in volume with carrying It is 3L to take the sediment mass ratio that step obtains:1kg stirs 40min at 25 DEG C, and speed of agitator 40rpm is stood after stirring 60min;2400rpm, which is centrifuged, to be precipitated;
Precipitation repetition is above-mentioned to add water (each amount of water is 17.85L) desalination processes 4 times, obtains polysaccharide desalination product 5.20kg;
(3) drying steps:The polysaccharide desalination product 5.20kg that desalting steps (2) obtain is taken, constant pressure and dry 2 hours is dry 90 DEG C of temperature;Then it being dried under reduced pressure under vacuum degree -0.1Mpa 2 hours, 70 DEG C of drying temperature obtains pachymaran extract, 40 mesh sieve is crushed, pachymaran is obtained and dissipates 433g.
Polyoses content, yield and its pharmacological activity that pachymaran obtained by the present embodiment dissipates measure:Polyoses content is 83.5%, yield 43.3%.Measure its to immunosuppressed mice phagocyte phagocytosis chicken red blood cell ability, immune factor and The influence of immune organ, animal experiment and test method are the same as embodiment 1.Result of the test is shown, (is gulped down with hydrocortisone model group Rate is bitten as 30.20%, index and spleen index 0.25, thymus index 0.16, the content of IL-2 is 7.62pg/mL, the content of TNF-α For 6.03pg/mL.) compare, the phagocytic activity of phagocyte, phagocytic rate 48.13% can be effectively facilitated;Spleen is effectively facilitated to refer to The raising of number and thymus index, index and spleen index 0.29, thymus index 0.18;Effectively promote the secretion of IL-2 and TNF-α, it is small Content in mouse serum is respectively IL-2 11.59pg/mL and TNF-α 43.21pg/mL.
The preparation and drying means, step that a kind of 3 pachymaran of embodiment dissipates are as follows:
(1) extraction step:Poria cocos block is taken, 60 mesh is crushed and sieves to obtain Poria cocos powder 500g, add 1.0mol/L sodium hydroxide solutions 10L, it is 20mL to add in volume with Poria cocos powder mass ratio:1g stirs 20min, speed of agitator 80rpm at 70 DEG C;Stirring extraction knot Shu Hou, 1200rpm centrifuge to obtain supernatant, and 4mol/L hydrochloric acid solutions are added in supernatant, adjust pH value to 7.5, stand 60min Afterwards, 1200rpm is centrifuged, and obtains sediment 3.00kg;
(2) desalting steps:The sediment 3.00kg that extraction step (1) obtains adds water 15.0L, adds in volume and extraction The sediment mass ratio that step obtains is 5L:1kg stirs 30min at 40 DEG C, and speed of agitator 80rpm stands 40min after stirring; 1200rpm, which is centrifuged, to be precipitated;
Precipitation repetition is above-mentioned to add water (each amount of water is 15.0L) desalination processes 3 times, obtains polysaccharide desalination product 2.80kg;
(3) drying steps:The polysaccharide desalination product 2.80kg that desalting steps (2) obtain is taken, constant pressure and dry 4 hours is dry 80 DEG C of temperature;Then it is dried under reduced pressure under vacuum degree -0.06Mpa 1.5 hours, 80 DEG C of drying temperature, obtains pachymaran extraction Object crushed 80 mesh sieve, obtain pachymaran and dissipate 210g.
Polyoses content, yield and its pharmacological activity that pachymaran obtained by the present embodiment dissipates measure:Polyoses content is 87.1%, yield 42.0%.Measure its to immunosuppressed mice phagocyte phagocytosis chicken red blood cell ability, immune factor and The influence of immune organ, animal experiment and test method are the same as embodiment 1.Result of the test is shown, (is gulped down with hydrocortisone model group Rate is bitten as 30.20%, index and spleen index 0.25, thymus index 0.16, the content of IL-2 is 7.62pg/mL, the content of TNF-α For 6.03pg/mL.) compare, the phagocytic activity of phagocyte, phagocytic rate 48.13% can be effectively facilitated;Spleen is effectively facilitated to refer to The raising of number and thymus index, index and spleen index 0.29, thymus index 0.19;Effectively promote the secretion of IL-2 and TNF-α, it is small Content in mouse serum is respectively IL-2 14.21pg/mL and TNF-α 46.72pg/mL.
The preparation and drying means, step that a kind of 4 pachymaran of embodiment dissipates are as follows:
(1) extraction step:Poria cocos block is taken, 24 mesh is crushed and sieves to obtain Poria cocos powder 1000g, add 2.0mol/L sodium bicarbonate solutions 25L, it is 25mL to add in volume with Poria cocos powder mass ratio:1g stirs 60min, speed of agitator 60rpm at 25 DEG C;Stirring extraction knot Shu Hou, 1200rpm centrifuge to obtain supernatant, and 12mol/L sulfuric acid solutions are added in supernatant, adjust pH value to 9.0, stand After 30min, 1200rpm centrifugations obtain sediment 6.30kg;
(2) desalting steps:The sediment 6.30kg that extraction step (1) is taken to obtain adds water 31.50L, adds in volume with carrying It is 5L to take the sediment mass ratio that step obtains:1kg stirs 20min at 25 DEG C, and speed of agitator 60rpm is stood after stirring 30min;1200rpm, which is centrifuged, to be precipitated;
Precipitation repetition is above-mentioned to add water (each amount of water is 31.50L) desalination processes 3 times, obtains polysaccharide desalination product 5.65kg;
(3) drying steps:The polysaccharide desalination product 5.65kg that desalting steps (2) obtain is taken, constant pressure and dry 5 hours is dry 85 DEG C of temperature;Then it being dried under reduced pressure under vacuum degree -0.09Mpa 3 hours, 70 DEG C of drying temperature obtains pachymaran extract, 60 mesh sieve is crushed, pachymaran is obtained and dissipates 465g.
Polyoses content, yield and its pharmacological activity that pachymaran obtained by the present embodiment dissipates measure:Polyoses content is 84.2%, yield 46.5%.Measure its to immunosuppressed mice phagocyte phagocytosis chicken red blood cell ability, immune factor and The influence of immune organ, animal experiment and test method are the same as embodiment 1.Result of the test is shown, (is gulped down with hydrocortisone model group Rate is bitten as 30.20%, index and spleen index 0.25, thymus index 0.16, the content of IL-2 is 7.62pg/mL, the content of TNF-α For 6.03pg/mL.) compare, the phagocytic activity of phagocyte, phagocytic rate 48.51% can be effectively facilitated;Spleen is effectively facilitated to refer to The raising of number and thymus index, index and spleen index 0.27, thymus index 0.17;Effectively promote the secretion of IL-2 and TNF-α, it is small Content in mouse serum is respectively IL-2 13.25pg/mL and TNF-α 44.33pg/mL.
The preparation and drying means, step that a kind of 5 pachymaran of embodiment dissipates are as follows:
(1) extraction step:Poria cocos block is taken, 60 mesh is crushed and sieves to obtain Poria cocos powder 1000g, add 0.2mol/L sodium bicarbonate solutions 20L, it is 20mL to add in volume with Poria cocos powder mass ratio:1g stirs 40min, speed of agitator 100rpm at 60 DEG C;Stirring extraction knot Shu Hou, 2400rpm centrifuge to obtain supernatant, and 6mol/L sulfuric acid solutions are added in supernatant, adjust pH value to 7.0, stand 45min Afterwards, 2400rpm is centrifuged, and obtains sediment 5.80kg;
(2) desalting steps:The sediment 5.80kg that extraction step (1) is taken to obtain adds water 34.80L, adds in volume with carrying It is 6L to take the sediment mass ratio that step obtains:1kg stirs 40min at 25 DEG C, and speed of agitator 100rpm is stood after stirring 60min;800rpm, which is centrifuged, to be precipitated;
Precipitation repetition is above-mentioned to add water (each amount of water is 34.80L) desalination processes 2 times, obtains polysaccharide desalination product 5.50kg;
(3) drying steps:The polysaccharide desalination product 5.50kg that desalting steps (2) obtain is taken, constant pressure and dry 4 hours is dry 80 DEG C of temperature;Then it is dried under reduced pressure under vacuum degree -0.09Mpa 1.5 hours, 80 DEG C of drying temperature, obtains pachymaran extraction Object crushed 80 mesh sieve, obtain pachymaran and dissipate 440g.
Polyoses content, yield and its pharmacological activity that pachymaran obtained by the present embodiment dissipates measure:Polyoses content is 82.5%, yield 44.0%.Measure its to immunosuppressed mice phagocyte phagocytosis chicken red blood cell ability, immune factor and The influence of immune organ, animal experiment and test method are the same as embodiment 1.Result of the test is shown, (is gulped down with hydrocortisone model group Rate is bitten as 30.20%, index and spleen index 0.25, thymus index 0.16, the content of IL-2 is 7.62pg/mL, the content of TNF-α For 6.03pg/mL.) compare, the phagocytic activity of phagocyte, phagocytic rate 47.32% can be effectively facilitated;Spleen is effectively facilitated to refer to The raising of number and thymus index, index and spleen index 0.28, thymus index 0.18;Effectively promote the secretion of IL-2 and TNF-α, it is small Content in mouse serum is respectively IL-2 12.81pg/mL and TNF-α 45.12pg/mL.
The preparation and drying means, step that a kind of 6 pachymaran of embodiment dissipates are as follows:
(1) extraction step:Poria cocos block is taken, 80 mesh is crushed and sieves to obtain Poria cocos powder 500g, add 1.0mol/L sodium bicarbonate solutions 10L, it is 20mL to add in volume with Poria cocos powder mass ratio:1g stirs 60min, speed of agitator 80rpm at 25 DEG C;Stirring extraction knot Shu Hou, 1200rpm centrifuge to obtain supernatant, and 10mol/L sulfuric acid solutions are added in supernatant, adjust pH value to 9.0, stand After 20min, 1200rpm centrifugations obtain sediment 3.20kg;
(2) desalting steps:The sediment 3.20kg that extraction step (1) is taken to obtain adds water 16.0L, adds in volume with carrying It is 5L to take the sediment mass ratio that step obtains:1kg stirs 30min at 25 DEG C, and speed of agitator 80rpm is stood after stirring 30min;1200rpm, which is centrifuged, to be precipitated;
Precipitation repetition is above-mentioned to add water (each amount of water is 16.0L) desalination processes 3 times, obtains polysaccharide desalination product 2.85kg;
(3) drying steps:The polysaccharide desalination product 2.85kg that desalting steps (2) obtain is taken, constant pressure and dry 5 hours is dry 90 DEG C of temperature;Then it being dried under reduced pressure under vacuum degree -0.09Mpa 3 hours, 70 DEG C of drying temperature obtains pachymaran extract, It is crushed and is sieved with 100 mesh sieve, obtained pachymaran and dissipate 232g.
Polyoses content, yield and its pharmacological activity that pachymaran obtained by the present embodiment dissipates measure:Polyoses content is 85.8%, yield 46.4%.Measure its to immunosuppressed mice phagocyte phagocytosis chicken red blood cell ability, immune factor and The influence of immune organ, animal experiment and test method are the same as embodiment 1.Result of the test is shown, (is gulped down with hydrocortisone model group Rate is bitten as 30.20%, index and spleen index 0.25, thymus index 0.16, the content of IL-2 is 7.62pg/mL, the content of TNF-α For 6.03pg/mL.) compare, the phagocytic activity of phagocyte, phagocytic rate 48.02% can be effectively facilitated;Spleen is effectively facilitated to refer to The raising of number and thymus index, index and spleen index 0.28, thymus index 0.19;Effectively promote the secretion of IL-2 and TNF-α, it is small Content in mouse serum is respectively IL-2 13.44pg/mL and TNF-α 46.28pg/mL.
The preparation and drying means, step that a kind of 7 pachymaran of embodiment dissipates are as follows:
(1) extraction step:Poria cocos block is taken, 60 mesh is crushed and sieves to obtain Poria cocos powder 500g, add 1.0mol/L sodium hydroxide solutions 10L, it is 20mL to add in volume with Poria cocos powder mass ratio:1g stirs 20min, speed of agitator 80rpm at 70 DEG C;Stirring extraction knot Shu Hou, 1200rpm centrifuge to obtain supernatant, and 4mol/L hydrochloric acid solutions are added in supernatant, adjust pH value to 7.5, stand 60min Afterwards, 1200rpm is centrifuged, and obtains sediment 3.00kg;
(2) desalting steps:The sediment 3.00kg that extraction step (1) is taken to obtain adds water 15.0L, adds in volume with carrying It is 5L to take the sediment mass ratio that step obtains:1kg stirs 30min at 40 DEG C, and speed of agitator 80rpm is stood after stirring 40min;1200rpm, which is centrifuged, to be precipitated;
Precipitation repetition is above-mentioned to add water (each amount of water is 15.0L) desalination processes 3 times, obtains polysaccharide desalination product 2.80kg;
(3) drying steps:The polysaccharide desalination product 2.80kg that desalting steps (2) obtain is taken, constant pressure and dry 8 hours is dry 80 DEG C of temperature, obtains pachymaran extract, crushed 80 mesh sieve, obtains pachymaran and dissipate 95g.
Polyoses content, yield and its pharmacological activity that pachymaran obtained by the present embodiment dissipates measure:Polyoses content is 81.7%, yield 19.0%.Measure its to immunosuppressed mice phagocyte phagocytosis chicken red blood cell ability, immune factor and The influence of immune organ, animal experiment and test method are the same as embodiment 1.Result of the test is shown, (is gulped down with hydrocortisone model group Rate is bitten as 30.20%, index and spleen index 0.25, thymus index 0.16, the content of IL-2 is 7.62pg/mL, the content of TNF-α For 6.03pg/mL.) compare, the phagocytic activity of phagocyte, phagocytic rate 38.32% can be effectively facilitated;Spleen is effectively facilitated to refer to The raising of number and thymus index, index and spleen index 0.26, thymus index 0.17;And it can also effectively promote IL-2 and TNF-α Secretion, the content in mice serum is respectively IL-2 10.59pg/mL and TNF-α 28.72pg/mL.
The preparation and drying means, step that a kind of 8 pachymaran of embodiment dissipates are as follows:
(1) extraction step:Poria cocos block is taken, 60 mesh is crushed and sieves to obtain Poria cocos powder 500g, add 1.0mol/L sodium hydroxide solutions 10L, it is 20mL to add in volume with Poria cocos powder mass ratio:1g stirs 20min, speed of agitator 80rpm at 70 DEG C;Stirring extraction knot Shu Hou, 1200rpm centrifuge to obtain supernatant, and 4mol/L hydrochloric acid solutions are added in supernatant, adjust pH value to 7.5, stand 60min Afterwards, 1200rpm is centrifuged, and obtains sediment 3.00kg;
(2) desalting steps:The sediment 3.00kg that extraction step (1) is taken to obtain adds water 15.0L, adds in volume with carrying It is 5L to take the sediment mass ratio that step obtains:1kg stirs 30min at 40 DEG C, and speed of agitator 80rpm is stood after stirring 40min;1200rpm, which is centrifuged, to be precipitated;
Precipitation repetition is above-mentioned to add water (each amount of water is 15.0L) desalination processes 3 times, obtains polysaccharide desalination product 2.80kg;
(3) drying steps:The polysaccharide desalination product 2.80kg that desalting steps (2) obtain is taken, is dried under reduced pressure 10 hours, it is dry 65 DEG C of temperature, vacuum degree are -0.09Mpa, obtain pachymaran extract, crushed 80 mesh sieve, obtain pachymaran and dissipate 105g。
Polyoses content, yield and its pharmacological activity that pachymaran obtained by the present embodiment dissipates measure:Polyoses content is 82.3%, yield 21.0%.Measure its to immunosuppressed mice phagocyte phagocytosis chicken red blood cell ability, immune factor and The influence of immune organ, animal experiment and test method are the same as embodiment 1.Result of the test is shown, (is gulped down with hydrocortisone model group Rate is bitten as 30.20%, index and spleen index 0.25, thymus index 0.16, the content of IL-2 is 7.62pg/mL, the content of TNF-α For 6.03pg/mL.) compare, the phagocytic activity of phagocyte, phagocytic rate 40.63% can be effectively facilitated;Spleen is effectively facilitated to refer to The raising of number and thymus index, index and spleen index 0.27, thymus index 0.17;And it can also effectively promote IL-2 and TNF-α Secretion, the content in mice serum is respectively IL-2 11.49pg/mL and TNF-α 35.62pg/mL.
The preparation and drying means, step that a kind of 9 pachymaran of embodiment dissipates are as follows:
(1) extraction step:Poria cocos block is taken, 60 mesh is crushed and sieves to obtain Poria cocos powder 500g, add 1.0mol/L sodium hydroxide solutions 10L, it is 20mL to add in volume with Poria cocos powder mass ratio:1g stirs 20min, speed of agitator 80rpm at 70 DEG C;Stirring extraction knot Shu Hou, 1200rpm centrifuge to obtain supernatant, and 4mol/L hydrochloric acid solutions are added in supernatant, adjust pH value to 7.5, stand 60min Afterwards, 1200rpm is centrifuged, and obtains sediment 3.00kg;
(2) desalting steps:The sediment 3.00kg that extraction step (1) is taken to obtain adds water 15.0L, adds in volume with carrying It is 5L to take the sediment mass ratio that step obtains:1kg stirs 30min at 40 DEG C, and speed of agitator 80rpm is stood after stirring 40min;1200rpm, which is centrifuged, to be precipitated;
Precipitation repetition is above-mentioned to add water (each amount of water is 15.0L) desalination processes 3 times, obtains polysaccharide desalination product 2.80kg;
(3) drying steps:The polysaccharide desalination product 2.80kg that desalting steps (2) obtain is taken, converts the water for adding 1 times of quality, with 60 DEG C of water-baths simultaneously stir evenly, and are spray-dried 4 hours, 170 DEG C of inlet air temperature, 90 DEG C, charging rate 1.3kg/h of leaving air temp, Disk rotating speed 29000rpm is centrifuged, pachymaran is obtained and dissipates 20g.
Polyoses content, yield and its pharmacological activity that pachymaran obtained by the present embodiment dissipates measure:Polyoses content is 83.2%, yield 4.0%.Measure its to immunosuppressed mice phagocyte phagocytosis chicken red blood cell ability, immune factor and The influence of immune organ, animal experiment and test method are the same as embodiment 1.Result of the test is shown, (is gulped down with hydrocortisone model group Rate is bitten as 30.20%, index and spleen index 0.25, thymus index 0.16, the content of IL-2 is 7.62pg/mL, the content of TNF-α For 6.03pg/mL.) compare, the phagocytic activity of phagocyte, phagocytic rate 42.45% can be effectively facilitated;Spleen is effectively facilitated to refer to The raising of number and thymus index, index and spleen index 0.26, thymus index 0.17;And it can also effectively promote IL-2 and TNF-α Secretion, the content in mice serum is respectively IL-2 10.35pg/mL and TNF-α 37.54pg/mL.

Claims (4)

1. a kind of pachymaran dissipates preparation and drying means, including:
(1)Extraction step;Poria cocos block is taken, 14 ~ 80 mesh is crushed and sieves to obtain Poria cocos powder, adds in aqueous slkali, after stirring extraction, 800 ~ 2400rpm centrifuges to obtain supernatant, is adjusted with acid the pH value of supernatant, and after standing 30 ~ 90min, 800 ~ 2400rpm centrifugations, it is heavy to obtain Starch;
(2)Desalting steps;To step(1)Add water in obtained sediment, stood after stirring, 800 ~ 2400rpm, which is centrifuged, to be sunk It forms sediment, is polysaccharide desalination product, this is a desalination processes;Desalination processes repeat 2 ~ 4 times;
(3)Drying steps;By step(2)It after obtained polysaccharide desalination product constant pressure and dry, then is dried under reduced pressure, obtains pachymaran Extract;
(4)By step(3)Obtained pachymaran extract smashes it through 40 ~ 100 mesh sieve, obtains pachymaran and dissipates.
2. a kind of pachymaran as described in claim 1 dissipates preparation and drying means, it is characterised in that:The extraction step (1)In, the aqueous slkali of addition is:In 0.1 ~ 1.5 mol/L sodium hydroxide solutions or 0.2 ~ 2.0mol/L sodium bicarbonate solutions, add It is 10 ~ 30mL to enter volume with Poria cocos powder mass ratio:1g;It is described stirring extraction process be:At 25 ~ 70 DEG C with rotating speed 40 ~ 100rpm stirs 20 ~ 60min;The process for being adjusted with acid supernatant pH value is:4 ~ 10mol/L hydrochloric acid solutions are added in supernatant Or 6 ~ 12mol/L sulfuric acid solutions, pH value is adjusted to 6.5 ~ 9.0.
3. a kind of pachymaran as described in claim 1 dissipates preparation and drying means, it is characterised in that:The desalting steps (2)In each desalination processes, the sediment mass ratio that addition volume and the extraction step of water obtain is 3 ~ 6L:1kg, the stirring The process stood afterwards is:After adding water, at 25 ~ 60 DEG C with 40 ~ 100 rpm of rotating speed stir 20 ~ 40min, after stirring stand 20 ~ 60min。
4. a kind of pachymaran as described in claim 1 dissipates preparation and drying means, it is characterised in that:The drying steps (3)In, the process of constant pressure and dry is:60 ~ 90 DEG C of drying temperature, 2 ~ 5 hours drying times;The process being dried under reduced pressure is:It is dry Vacuum degree -0.06 ~ -0.1Mpa, 50 ~ 80 DEG C of drying temperature, 1.5 ~ 3 hours drying times.
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CN115777948A (en) * 2022-11-25 2023-03-14 中国药科大学 Dietary fiber supplement suitable for IBS patients

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Publication number Priority date Publication date Assignee Title
CN113861449A (en) * 2021-09-16 2021-12-31 湖北中医药大学 Pachyman hydrogel and preparation method and application thereof
CN113861449B (en) * 2021-09-16 2023-11-28 湖北中医药大学 Pachyman hydrogel and preparation method and application thereof
CN115777948A (en) * 2022-11-25 2023-03-14 中国药科大学 Dietary fiber supplement suitable for IBS patients
CN115777948B (en) * 2022-11-25 2024-03-15 中国药科大学 Dietary fiber supplement suitable for IBS patients

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