CN103980373B - A kind of algal polysaccharide sulfate extracting method - Google Patents
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Abstract
The present invention relates to a kind of new method for extracting of botanical drug substance, i.e. a kind of algal polysaccharide sulfate extracting method.Preparation trade name: Hai Kun Sheng Xi Capsule.Its main extraction step is as follows: (1) dry sea-tangle adds 10 times amount water soaking 8 hours, controls room temperature 8-32 DEG C; Getting soak solution, to be concentrated into original volume 1/5 for subsequent use; Adopt this step, the algal polysaccharide on marine organisms surface is separated.(2) sea-tangle after soaking takes out chopping, with the homogenate of AH high pressure homogenizer.(3) homogenate hydro-oxidation sodium adjust ph 12, stirs 30 minutes, static 12 hours, with salt acid for adjusting pH value 1.5-2, stirs 8 hours, static 12 hours; (4) filter.(5) concentrated solution in filtrate and step (1) merges and adopts special type 500 electrodialytic desalting.(6) concentration of liquid medicine, decolouring.(7) centrifugal, filter cake 95% washing with alcohol.(8) dry, pulverize dry thing.Improve yield, reduce costs.After testing, present method improves more than 40% than original process recovery ratio.
Description
technical field
The present invention relates to a kind of new method for extracting of botanical drug substance, i.e. a kind of algal polysaccharide sulfate extracting method.Preparation trade name: Hai Kun Sheng Xi Capsule.
Background technology
In the prior art, chronic renal failure is that chronic renal disease or the chronic kidney caused by accumulative renal system disease go down, and the syndromes that consequent various clinical symptom and metabolism disorder form.This disease belongs to difficult and complicated illness, and the existing world, domestic doctor trained in Western medicine circle there is no effect method, and Chinese materia medica has certain curative effect in delaying chronic kidney exhaustion course advancement, rare two class Chinese medicines in the medicine of existing treatment by Chinese herbs chronic kidney hypofunction.Algal polysaccharide sulfate bulk drug (preparation trade name; Hai Kun Sheng Xi Capsule) as the two class medicines (national drug standards YBZ00902003-2008) extracted in marine plant sea-tangle, there is material cost low, source is easy, effect outstanding feature.Algal polysaccharide sulfate is the effective constituent extracted from marine algae sea-tangle, is the rare sulfuric ester ionic polysaccharide of occurring in nature.Through the cooperation of pulling together of the Institute of Oceanology of the Chinese Academy of Sciences and Jilin long queue Pharma Inc., algal polysaccharide sulfate bulk drug and Hai Kun Sheng Xi Capsule obtain national New Drug Certificate, realize industrialization, for vast Patients with Chronic Renal Disease opens a new therapy approach, achieving must economic and social benefit.Function with cure mainly: change turbid toxin expelling, for the wet turbid disease of chronic renal failure (compensatory phase, Decompensated stage and uremia are early stage).Disease is seen nauseating, and vomiting, receives difference, abdominal distension, and body is heavy sleepy, oliguria, edema, thick and greasy fur.Wet turbid card is the modal TCM Syndrome Type of chronic kidney hypofunction, wide in clinical application range for the wet medicine of turbid card of chronic kidney hypofunction, be suitable for patient numerous, and Hai Kun Sheng Xi Capsule dose is little, without increasing gi tract burden and the too much sorrow of Water l oad, wet turbid card cardinal symptom and disease integration of chronic kidney hypofunction is also improved significantly simultaneously, the side effect such as large and diarrhoea without common treatment renal failure medicine gastrointestinal reaction, therefore this medicine has its advantage and uniqueness.Algal polysaccharide sulfate bulk drug method for making: the segment of 8000kg sea-tangle is added 140000kg water in dissolving tank, during soaking at room temperature 4, soak solution hydro-oxidation sodium, adjust pH to 12, obtain alkali condensation product, get condensation product sheet frame filter-cloth filtering, filter cake adds acid dissolve, adjust ph 3.5, solution secondary sheet frame filter-cloth filtering, gets filtrate, discards filter cake residue, solution adjust pH 4-5, three sheet frame filter-cloth filterings, get filtrate and add ethanol and be adjusted to alcohol concn 70%, form precipitation, taking precipitate is dry obtains dry substance, and dry substance is pulverized to obtain Thallus Laminariae (Thallus Eckloniae) extract.With tap water 900kg in enamel reaction still, then drop into this batch of Thallus Laminariae (Thallus Eckloniae) extract, stir 30 minutes, slowly add hydrochloric acid 476kg, regulate pH value 2-3, the complete continuation stirring of acid adding 8 hours, lysate is proceeded to slurry tank and leave standstill 12 hours, get supernatant liquor 49kg diatomite vacuum drum and filter.Filtrate electrodialytic desalting, demineralised liquid enriching ammonia neutralization is to neutral.Feed liquid single-effect evaporator is evaporated to 420L, concentrated solution is transferred to alcohol and analyses tank, adds the Klorvess Liquid of 1.4L10%, adds ethanol and makes alcohol amount reach 70%, stir 30 minutes, leave standstill, 12 hours, throw out was centrifugal, filter cake with 95% washing with alcohol once, filter cake is with vacuum decompression loft drier in 60 DEG C of vacuum-dryings, and dry cream is pulverized, and obtains algal polysaccharide sulfate 17kg.Pulverize, airtight preservation.This product, in dry product, must not be less than 25% containing fucose, must not be less than 22% containing hydrolysis sulfate.Its shortcoming is: adopt conventional kelp soaking alkaline cleaning, 3 sheet frame filter-cloth filterings, and scale production efficiency is low, length consuming time, and to the not easily separated removal of the distinctive algin of marine organisms, product yield is low.
Summary of the invention
The object of the invention is a kind of method that improvement is provided for above-mentioned deficiency, ensure that effective constituent is separated out, the better algal polysaccharide sulfate extracting method of extraction effect.
Technical solution of the present invention is: a kind of algal polysaccharide sulfate extracting method, and its step is as follows:
(1) dry sea-tangle adds 10 times amount water soaking 8 hours, controls room temperature 8-32 DEG C; Getting soak solution, to be concentrated into original volume 1/5 for subsequent use; Adopt this step, the algal polysaccharide on marine organisms surface is separated.
(2) sea-tangle after soaking takes out chopping, with high pressure homogenizer homogenate (homogenate of AH high pressure homogenizer, ATS industrial system company limited commercially product, Shanghai); Output 1000kg/ hour, fineness of materials 80 order.
(3) homogenate hydro-oxidation sodium adjust ph 12, stir 30 minutes, static 12 hours (basic solution can change the space structure of polysaccharide and protein in sea-tangle cell walls, makes hard-packed cell walls originally become loose, then through soaking, cellularstructure is mended and is destroyed, intracellular organic matter is separated out), with salt acid for adjusting pH value 1.5-2, stir 8 hours, static 12 hours (dissolve algal polysaccharide, make it separate in cell); Adopt this step, make the inner distinctive algal polysaccharide of marine organisms easily be separated removal, have good separating effect, produce in enormous quantities consuming time short, efficiency is high, and product treatment amount is large, and yield is high, can the advantage of the large production of continuous industry.
(4) diatomite vacuum drum adsorption filtration; Rotary drum rotating speed is for often to turn 0.1 to 10 minute.The absolute pressure of operation vacuum is (0.25 ~ 0.8) × 10 handkerchiefs.
(5) concentrated solution in filtrate and step (1) merges and adopts special type 500 electrodialytic desalting (light, dense water pressure reaches 0.05-0.1MPa), and demineralised liquid enriching ammonia neutralization is to neutral.Special type 500 refers to: rated output is 5 cubes ms/h.
(6) concentration of liquid medicine, adds activated carbon decolorizing.
(7) concentrated solution adds 10% Repone K, and secondary adds ethanol makes alcohol content reach 70%, static throw out, centrifugal, filter cake 95% washing with alcohol.
(8) dry 4 hours of filter cake vacuum decompression at 60 DEG C.
(9) dry thing is pulverized, the algal polysaccharide sulfate of obtained oyster white or buff powder.
Diabetic nephropathy is relevant with metabolic disturbance (as polyvalent alcohol metabolic disturbance, non-glycosylation), cytokine and vasoactive factors etc.The how asymptomatic blood pressure of getting up early can be normal or higher.By the micro-gram/minute of Urine By Radioimmunoassay microalbumin output >200, this phase is called invisible ephrosis, or early nephropathy.If actively control hypertension and hyperglycemia, pathology is expected to take a turn for the better.
Therefore study toxic side effect little, drug effect is definite, and the diabetic nephropathy new drug that dosage is little is the task of top priority, is also the urgent need of the mankind.In clinical trial, by taking the clinical test results analysis of Hai Kun Sheng Xi Capsule to complicated with diabetes nephrotic while of chronic kidney hypofunction, we find that the proteinuria, edema, hypertension etc. of patient obviously improve simultaneously.For this phenomenon, we have good conditioning blood sugar, blood pressure effect for algal polysaccharide sulfate, algal polysaccharide sulfate is disorderly by multipath Mutiple Targets regulating lipid metabolism, by suppressing exogenous lipid absorption, promoting endogenous lipid metabolic activation lipid metabolism enzyme and increase bile acid excretion three aspect regulating lipid metabolisms, and suppress atherosclerotic development by anti peroxidation of lipid and minimizing lipid deposition in the tissue.Little as polyose natural marine toxic side effect, drug effect is definite, is easily accepted by patient, therefore increases the indication of its diabetic nephropathy effect, can meet the clinical needs of part of diabetes mellitus ephrosis people, is also conducive to the marketing scale expanding algal polysaccharide sulfate.
Advantage of the present invention is: 1, Hai Kun Sheng Xi Capsule bulk drug algal polysaccharide sulfate is a kind of sulfuric ester ionic polysaccharide with unique texture and function.The present invention improves extraction process, and operational path adopts kelp soaking, soda acid to extract route, greatly shortens the production cycle; efficiently solve the difficult problem that in marine plant, algal polysaccharide should not be separated, improve yield, reduce costs; decreasing pollution, is conducive to accomplishing scale production.And carry out pharmacodynamics test research and the clinical trial of Hai Kun Sheng Xi Capsule.2, after testing, the unusual effect that present method is brought is the content that improve fucose, >=27mg/ grain.Improve hydrolysis sulfate content, >=25mg/ grain.More than 40% is improved than original process recovery ratio.
Below in conjunction with embodiment, embodiments of the present invention are described in further detail.
Embodiment
Embodiment 1
2000kg sea-tangle is added 20000kg water in dissolving tank, and during soaking at room temperature 8, it is for subsequent use that soak solution is concentrated into 4000kg.Sea-tangle chopping after immersion, homogenate is carried out with refiner, homogenate hydro-oxidation sodium adjust ph 12, stir 30 minutes, static 12 hours, add hydrochloric acid 960kg adjust ph 1.5-2, the complete continuation stirring of acid adding 8 hours, lysate is proceeded to slurry tank leave standstill be no less than 12 hours, get the concentrated solution merging 60kg diatomite vacuum drum after supernatant liquor and kelp soaking and filter.Filtrate adopts special type 500 electrodialytic desalting, and demineralised liquid enriching ammonia neutralization is to neutral.Feed liquid single-effect evaporator is evaporated to 300L, concentrated solution is transferred to alcohol and analyses tank, adds the Klorvess Liquid of 1L10%, adds ethanol and makes alcohol amount reach 70%, stir 30 minutes, leave standstill be no less than 12 hours, throw out link-suspended basket centrifuge is centrifugal, filter cake with 95% washing with alcohol once, filter cake with vacuum decompression loft drier in 60 DEG C of vacuum-dryings, dry cream is pulverized unit with the automatic control of ZKF-3X type and is pulverized, and screen cloth specification 100 order, obtains algal polysaccharide sulfate 6.1kg.Through assay (concrete grammar meets algal polysaccharide sulfate bulk drug national drug standards YBZ00902003-2008 and specifies), the content of fucose reaches more than 28%, hydrolysis sulfate content reaches more than 26% (see table 1), both conformance with standard requirement, significantly improves again fucose, the content being hydrolyzed sulfate and yield.
The new and old process results contrast of table 1 algal polysaccharide sulfate
Experimental example
The pharmacodynamics test research of the Hai Kun Sheng Xi Capsule that novel process obtains
One, test materials
1, medicine
Algal polysaccharide sulfate is provided by Huinan, Jilin Province long queue medicine company limited-liability company; lot number: 20131101; the solution being mixed with different concns is dissolved with distillation, dexamethasone acetate, Shanxi Heng Ruida pharmaceutical Co. Ltd during administration; lot number: 110801; 2,4 dinitrochlorobenzene, reagent one factory of Solution on Chemical Reagents in Shanghai company limited produces, hydrochlorothiazide tablet; Shandong Li Fenghuarui Pharmaceutical Co, lot number: 20130105.
2, animal
Male Wistar rat, body weight 220 ~ 260g, Kunming mouse, male and female half and half, body weight 18-22g, is provided by new drug pharmacological research center, Shandong Province.Hybrid domesticated dog, body weight 12-15kg, purchased from every household village, male and female dual-purpose.
3, instrument
RM-6000 type polygraph, MFV-3200 type Electromagnetism flowmeter, Japanese photoelectricity company produces, rat metabolism cage, and Law Firm Suzhou Jiangsu Wuqiao Long Ju factory manufactures.Electronic analytical balance, Mettler-Toledo, Inc. produces.BackmanICS II type turbidinetry: Backman company of the U.S. produces.
Two, test method
1, to 2, the impact of 4 dinitrochlorobenzene induced mice delayed type hypersensitivities
Select the healthy Kunming mouse of body weight 18-24g, male and female dual-purpose.With 2,4 dinitrochlorobenzene acetone solution dorsal sc injection 0.02ml/ mouse sensitization of 1.25%.One day after, animal is divided into 5 groups to sensitization at random, namely by the basic, normal, high dosage group of medicine, and dexamethasone acetate, model group.Respectively gavage give algal polysaccharide sulfate 75,150,300mg/kg, dexamethasone acetate 0.1mg/kg, model group gives isometric(al) physiological saline not, continuous gavage 9 days, 10th day with 0.25%2,4 dinitrochlorobenzene acetone solution subcutaneous injection mouse right foot pad centres, dosage is 0.02ml/, compares parapodum injection isometric(al) acetone solution, two foots are cut from ankle joint after 38 hours, scales/electronic balance weighing, is calculated as follows swelling and inhibiting rate, and carries out statistical procedures.
Swelling=right lumping weight amount (mg)-left lumping weight amount (mg)
Get angular vein blood before putting to death animal centrifugal, rate nephelometry measures change of serum C
3, C
4, IgG, IgM content.
Separately get 10 Kunming mouses as normal group, same raising is after 10 days, and it is centrifugal that angular vein gets blood, and the same mensuration surveys change of serum C
3, C
4, IgG, IgM content.
2, to intact animal diuretic properties
The male and healthy Wistar rat of body weight 150 ~ 200g, is placed in metabolic cage pre-adaptation 1, accesses 6 hr urine, observe the urine volume under free conditions of water drinking, the selected test of the animal selecting urine volume stable.
By 6 hours voided volume, animal is divided into 5 groups at random, the i.e. high, medium and low dosage group of test medicine, hydrochlorothiazide group, normal group, administration group dosage be respectively algal polysaccharide sulfate 50,10,200mg/kg, hydrochlorothiazide 4mg/kg, administration volume be 1ml 100g, normal group gives isometric(al) solvent.
Animal fasting 18 hours before test.After administration, animal puts into rapidly the metabolic cage giving sufficient drinking-water, and place rat 1 in every metabolic cage, gently press thing lower abdomen before putting into, drain remaining urine, after medicine, chamber pot per hour once, and Continuous Observation 6 hours observes the difference of urine volume in each group of certain hour.
3, to Water-loaded diuretic properties
The male and healthy Wistar rat of body weight 150 ~ 200g, be placed in metabolic cage pre-adaptation 1, access 6 hr urine, whether the urine volume of observing under free conditions of water drinking is stablized, press 2.5ml/100g gavage physiological saline again, the urine volume of collecting in 2 hours reaches the selected test of animal of the amount of pouring into 40%.
By 6 hours voided volume, animal is divided into 6 groups at random, i.e. the basic, normal, high dosage group of test medicine, hydrochlorothiazide group, model group, normal group.Administration group dosage be respectively algal polysaccharide sulfate 50,100,200mg/kg, hydrochlorothiazide 4mg/kg, model group gives isometric(al) physiological saline, and normal group does not process.
Animal fasting 18 hours before test, during test, administration treated animal medicine is mixed in load water (giving 38 DEG C of physiological saline by 2.5ml/100g gavage) and gives.The isometric physiological saline of model group replaces liquid.After administration, animal puts into rapidly the metabolic cage giving sufficient drinking-water, places rat 1, gently presses thing lower abdomen before putting into, drain remaining urine in every metabolic cage.After medicine, chamber pot per hour once, Continuous Observation 6 hours, observes the difference of urine volume in each group of certain hour.
4, on the impact of anesthetized dog renal blood flow
Domesticated dog 3% vetanarcol (30mg/kg) intravenous anesthesia, neck medisection, trachea cannula, ventral decubitus is fixed on operating table, from left side diaphragm side of body angle longitudinal incision skin, separating muscle, exposes kidney, opens adeps renis after peritonaeum, the careful separation Renal artery, being inserted in diameter is 2 ~ 4 ㎜ magnetic flow meter control heads, measures renal blood flow, and operation terminates latter 30 minutes, Deng renal blood flow recover and stable after, respectively by 20,60mg/kg intravenous injection algal polysaccharide sulfate solution, administration volume is 1ml/kg, and medicine gave in 1 minute.Before record medicine, 0.5,1,3,5,10,20,30 minute renal blood flow after medicine.
Three, test-results
1, on the impact of 2,4 dinitrochlorobenzene induced mice delayed type hypersensitivities
The results are shown in Table 2,3.
Table 2 algal polysaccharide sulfate is on the impact of dinitrochlorobenzene induced mice delayed type hypersensitivity
From table 2, algal polysaccharide sulfate ig administration has restraining effect to 2,4 dinitrochlorobenzene induced mice delayed type hypersensitivities in 9 days, and 100,200mg/kg group swelling compares p < 0.01 with model group.Dexamethasone acetate group also has similar effect.
Table 3 algal polysaccharide sulfate is to change of serum C
3, immunoglobulin (Ig), total complement content impact
Normal group p < 0.05p < 0.01*vs model group * p < 0.05** < 0.01
From table 3, mouse subcutaneous injection 2, after 4 dinitrochlorobenzene, immunological indices all raises.After giving medicine ig9 days, algal polysaccharide sulfate 150mg/kg group has restraining effect to mouse humoral immune part index number; Algal polysaccharide sulfate 300mg/kg group and dexamethasone acetate group all have remarkable restraining effect to mouse humoral immune indices, compare p < 0.05 or p < 0.01 with model group.Algal polysaccharide sulfate 75mg/kg group only has effect trend.
2, to normal rat diuretic properties
The results are shown in Table 4
From table 4, after model group gives Water l oad, animal urine volume obviously increases, and 0 ~ 3 hour period compared with normal group significant difference (p < 0.01 or 0.05).Algal polysaccharide sulfate respectively organize upon administration in 6 hours urine volume more all have increase with model group, wherein 100mg/kg group upon administration 3 ~ 4 hours period urine volume have significant difference (p < 0.05); 200mg/kg group upon administration 1 ~ 6 hour period urine volume have significant difference (p < 0.01 or 0.05).Algal polysaccharide sulfate 50mg/kg group also has effect trend.The effect of each dosage group has dose-dependently.It is the strongest that algal polysaccharide sulfate respectively organizes 2 ~ 4 hours diuretic properties upon administration.Hydrochlorothiazide group upon administration in 6 hours urine volume and model group more all have significant difference (p < 0.01 or 0.05).
3, to Water l oad rat diuretic properties
the results are shown in Table 5
Respectively organize urine volume upon administration by the visible algal polysaccharide sulfate of table 5 and more all have increase with normal group, wherein 200mg/kg group upon administration during 0 ~ 5 hour urine volume compare with normal group and have significant difference (p < 0.01 or 0.05); 50,100mg/kg group upon administration in part-time urine volume also have significant difference (p < 0.01 or 0.05).The effect of each dosage group has dose-dependently.It is the strongest that algal polysaccharide sulfate respectively organizes 2 ~ 4 hours diuretic properties upon administration.Hydrochlorothiazide group upon administration in 6 hours urine volume and normal group more all have significant difference (p < 0.01 or 0.05).
4, on the impact of anesthetized dog renal blood flow
The results are shown in Table 6
Table 6 algal polysaccharide sulfate is on the impact of anesthetized dog renal blood flow
X±SD,n=4,*p＜0.05,**p＜0.01
From table 6, NS control group renal blood flow changes without significance; After algal polysaccharide sulfate high dose group medicine, renal blood flow obviously increases, and within after medicine 3,5 and 20 minutes, has significant difference with comparing before medicine, within after medicine 10 minutes, has pole significant difference with comparing before medicine; After low dose group medicine also there is rising effect in renal blood flow, after medicine 0.5,1 minute with medicine before than there being significant difference.After high dose group medicine, 10 minutes renal blood flows increase effect and reach maximum, to may persist to after medicine 20 minutes.
Six, conclusion (of pressure testing)
1, algal polysaccharide sulfate 150,300mg/kgig administration have obvious restraining effect to 2,4 dinitrochlorobenzene induced mice delayed type hypersensitivities in 9 days, and have dose-dependently.Can obviously suppress allergy mouse humoral immune simultaneously.
2, algal polysaccharide sulfate 50, the administration of 200mg/kg single oral gavage all have diuretic properties to normal and Water l oad rat, and 2 ~ 4 Hours drug diuretic properties are the strongest upon administration, and each dosage group difference between the effects is obvious, has doses dependence.
3, algal polysaccharide sulfate 60mg/kg intravenous administration can increase anesthetized dog renal blood flow, and onset in 3 minutes after medicine, reaches maximum effect (15.52%) for 10 minutes, to may persist to after medicine 20 minutes.
The Hai Kun Sheng Xi Capsule clinical experiment report that novel process obtains
1, curative effect evaluation
This test adopts No. I, Hai Kun Sheng Xi Capsule (treatment group) and No. II, Hai Kun Sheng Xi Capsule (control group) treats chronic renal failure respectively and wets and turbidly demonstrate,prove patient 40 example, test-results display: in the routine patient for the treatment of group 40, effective 9 routine, effective 8 examples, stablize 12 examples, efficient is 42.5%, in the routine patient of control group 40, effective 8 examples, effective 8 examples, stablize 15 examples, efficient is 40.0%, two groups efficient without difference, slightly carries master, P < 0.05; The effective index of stability for the treatment of group is 72.5%; The effective index of stability of control group is 60.0%, treatment group and control group general curative effect no significant difference, P > 0.05.In addition, Hai Kun Sheng Xi Capsule has reduction plasma wrea, creatinine, blood uric acid, raises endogenous creatinine clearance rate, improves renal function, increases the effect such as oxyphorase and plasma albumin level.Hai Kun Sheng Xi Capsule improves significantly to wet turbid card cardinal symptom and disease integration tool of chronic kidney hypofunction, therefore Hai Kun Sheng Xi Capsule is applicable to chronic kidney hypofunction wets turbid card patient.
2, safety evaluation
Obvious adverse reaction is not found in the clinical trial of this group, to Indexs measure such as clinical symptom, white corpuscle, liver function, blood sugar, stool blood, the heart, lungs before and after treatment, all no abnormal, point out this medicine safety, non-evident effect.
Experiment case
Mr. Li, man, 58 years old, workman, was in hospital.
Patient main suit is weak 3 months, edema, feels sick 14 days.Patient occurred weak before 3 months, have a blood test pressure for 200/120mmHg to local hospital, urine protein +++, BUN19.8mmol/L, examine as " chronic nephritis ", give " BAOSHENKANG ", " nifedipine ", " dipyridamole " treatment, without being clearly better, occurs eyelid and edema of pair of lower extremities in nearly 7 days, feel sick, poor appetite.Have a medical check-up: blood pressure 200/120mmHg, nutrition is slightly poor, chronic renal sickly look, and eyelid is edema slightly, edema that two lower limb are slight.Diagnosis: the traditional Chinese medical science: consumptive disease; Doctor trained in Western medicine: 1. chronic renal insufficiency (Delayed graft function phase) 2. chronic glomerulonephritis.Plasma wrea 22.5mmol/L, creatinine 612.4umol/L, Ccr14.8ml/min is checked before treatment, twenty-four-hour urine protein quantification 3.56g, wet turbid card integrated value 24 points, there is Nausea and vomiting in patient, it is poor to receive, abdominal distension, body heavy sleepy, edema, thick fur are greasy, after the treatment of No. I, Hai Kun Sheng Xi Capsule, the turbid card symptom integral value that wets when 4 weeks is 12 points, serum creatinine is down to 389.1umol/L, when 8 weeks, integration is 8 points, serum creatinine is 389.7umol/L, weakly obviously alleviates, and feels sick and disappears, eyelid and edema of pair of lower extremities disappear, and result for the treatment of is obvious.
Describe above, just the specific embodiment of the present invention, various illustrating is not construed as limiting flesh and blood of the present invention.
Claims (1)
1. an algal polysaccharide sulfate extracting method, is characterized in that step is as follows:
(1) dry sea-tangle adds 10 times amount water soaking 8 hours, controls room temperature 8-32 DEG C; Getting soak solution, to be concentrated into original volume 1/5 for subsequent use;
(2) sea-tangle after soaking takes out chopping, uses high pressure homogenizer homogenate;
(3) homogenate hydro-oxidation sodium adjust ph 12, stirs 30 minutes, static 12 hours, with salt acid for adjusting pH value 1.5-2, stirs 8 hours, static 12 hours;
(4) diatomite vacuum drum adsorption filtration; Rotary drum rotating speed is for often to turn 0.1 to 10 minute; The absolute pressure of operation vacuum is 0.25 × 10 handkerchief ~ 0.8 × 10 handkerchief;
(5) concentrated solution in filtrate and step (1) merges and adopts special type 500 electrodialytic desalting, and light, dense water pressure reaches 0.05-0.1MPa; Demineralised liquid enriching ammonia neutralization is to neutral; Special type 500 refers to: rated output is 5 cubes ms/h;
(6) concentration of liquid medicine, adds activated carbon decolorizing;
(7) concentrated solution adds 10% Repone K, adds ethanol and makes alcohol content reach 70%, static throw out, centrifugal, filter cake 95% washing with alcohol;
(8) dry 4 hours of filter cake vacuum decompression at 60 DEG C;
(9) dry thing is pulverized, the algal polysaccharide sulfate of obtained oyster white or buff powder.
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| CN106496352A (en) * | 2016-11-27 | 2017-03-15 | 威海蓝印海洋生物科技有限公司 | A kind of sulfated fucan extracting method |
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| CN107674130A (en) * | 2017-11-19 | 2018-02-09 | 荣成海锐芯生物科技有限公司 | A kind of method that algal polysaccharides are extracted from sea-tangle |
| CN107881207A (en) * | 2017-11-19 | 2018-04-06 | 荣成海锐芯生物科技有限公司 | A kind of preparation method of the laminarin of low content of iodine |
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