CN104926955A - Method for fractionating polysaccharide from cistanche - Google Patents
Method for fractionating polysaccharide from cistanche Download PDFInfo
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Abstract
The invention relates to a method for fractionating polysaccharide from cistanche. The method includes the following steps of 1), obtaining fleshy stems of the cistanche, smashing the fleshy stems, performing pretreatment with an ethanol solution, adding purified water to obtained filter residues, and performing solid-liquid separation to obtain clear liquid I and the filter residues II; 2), filtering the clear liquid I with a micro-filtration membrane to obtain permeate liquid; 3), sequentially adopting an ultrafiltration membrane capable of intercepting polysaccharide in hundred thousand level of molecular weight, an ultrafiltration membrane capable of intercepting polysaccharide in 10,000 level of molecular weight, an ultrafiltration membrane capable of intercepting polysaccharide in 1,000 level of molecular weight and a nanofiltration membrane capable of intercepting polysaccharide in 100 level of molecular weight to filter the permeate liquid to obtain soluble polysaccharide products different in molecular weight. The polysaccharide different in molecular weight can be rapidly fractionated, the molecular weight of the products is concentrated and identical in activity, and the polysaccharide is non-toxic and harmless; during preparation, less ethanol is used, production energy consumption is low, fewer process is involved, and the period is short.
Description
Technical field
The invention belongs to technical field of biochemical separation, be specifically related to a kind of method of fractional separation polysaccharide from Herba Cistanches.
Background technology
Herba Cistanches is the plant of parasitics for many years of a kind of Orobanchaceae (Orobanchaceae) Cistanche deserticola (Cistanche Hoffmg.et Link), and obligatory parasitism is in the root of sacsaoul class plant, and the whole world has more than 20 to plant.Have 4 kind of 1 mutation within Chinese territory, be mainly distributed in the ground such as the Inner Mongol, Ningxia, Gansu, Qinghai and Xinjiang.Herba Cistanches begins to be loaded in Shennong's Herbal, successive dynasties medicine book all has detailed record to it, be listed in top grade medicinal material for a long time, have another name called rue greatly, sweetly to rue greatly, desert cistanche, Herba Cistanches and ground essence etc., the effect such as have warming and recuperating the kidney-YANG, beneficial smart tonifying Qi and relax bowel, is widely used in that treatment insufficiency of kidney-YANG, impotence are infertile clinically, blood and essence asthenia, muscles and bones is unable, soreness of the waist and knees and the dry constipation of intestines.China's West Inner Mongolia is the Desert Herba Cistanches of main producing region and Cistanche Tubulosa is Herba Cistanches certified products.
The chemical composition of Herba Cistanches is very complicated, and what content was maximum is carbohydrate.Carbohydrate comprises polysaccharide and the oligose of different polymerization degree, and different monose and disaccharide.Wheat-based diet and oligosaccharides have raising immunizing power, relax bowel and treat the effects such as type ii diabetes.
CN 104262414 A discloses a kind of method simultaneously preparing benzyl carbinol glycosides, N.F,USP MANNITOL, oligosaccharide syrup and polysaccharide from Herba Cistanches, comprise the steps: to adopt monose, oligose and the benzyl carbinol glycosides in aqueous ethanolic solution extraction Herba Cistanches, then macroporous adsorptive resins Separation of Benzene ethanol glycoside and carbohydrate, the benzyl carbinol glycosides solution that wash-out obtains becomes product through concentrate drying, carbohydrate is through concentrating under reduced pressure, normal temperature crystallization, separating oligomeric carbohydrate and N.F,USP MANNITOL, N.F,USP MANNITOL recrystallization obtains high purity N.F,USP MANNITOL, and centrifugal clear liquid is oligosaccharide syrup.Residue adopts Aqua pure extract polysaccharide, and alcohol precipitation collects polysaccharide.
CN 101870742 B has invented a kind of separating and purifying method of wheat-based diet, Herba Cistanches is cleaned after drying and pulverize, use sherwood oil and alcohol immersion respectively and supersound process, to remove the compositions such as fat, filter rear residue distilled water immersion and be placed in refrigerator and cooled and freeze, after taking out, microwave treatment makes it rapid thawing, and filtrate is wheat-based diet extracting solution; Allow this extracting solution normal pressure by macroporous adsorptive resins, concentrating under reduced pressure, alcohol precipitation, lyophilize, then use acetone, anhydrous diethyl ether and absolute ethanol washing successively, pure wheat-based diet can be obtained.
Can find out, in the prior art, due to the polysaccharide of macromolecule in Herba Cistanches and the polysaccharide of small-molecular-weight wrap up in take together with precipitate, cause fractional separation thorough, molecular weight product is not concentrated, and physico-chemical property is inconsistent, biologically active labile; In addition, the alcohol precipitation process of wheat-based diet will expend the ethanol of incredible amount, and the storage of ethanol and recovery time consumption and energy consumption, make troubles also to the industrialization of wheat-based diet.
Summary of the invention
The object of the present invention is to provide a kind of method of fractional separation polysaccharide from Herba Cistanches, it can prepare the polysaccharide of the differing molecular polymerization degree quickly and easily.
For reaching above object, the present invention adopts following technical scheme:
The invention provides a kind of method of fractional separation polysaccharide from Herba Cistanches, comprise the steps:
(1) get Herba Cistanches fleshy stem, pulverize, carry out pre-treatment with ethanolic soln, in the filter residue obtained, add purified water, solid-liquid separation, obtain clear liquid I and filter residue II; Containing solubility wheat-based diet in described clear liquid I;
(2) use micro-filtrate membrane filtration clear liquid I, obtain permeate;
(3) adopt molecular weight cut-off to be ultra-filtration membrane, the molecular weight cut-off of 100,000 grades to be the ultra-filtration membrane of ten thousand grades successively, molecular weight cut-off is the ultra-filtration membrane of thousand grades and molecular weight cut-off is the nanofiltration membrane permeate of hundred grades, obtains the soluble polysaccharide product of different molecular weight.
Preferably, step (3) is:
A () is the ultrafiltration membrance filter permeate of 100,000 grades with molecular weight cut-off, obtain trapped fluid IV and permeate V;
B () is the ultrafiltration membrance filter permeate V of ten thousand grades with molecular weight cut-off, obtain trapped fluid VI and permeate VII;
C () is the ultrafiltration membrance filter permeate VII of thousand grades with molecular weight cut-off, obtain trapped fluid VIII and permeate IX;
D () is the nanofiltration membrane permeate IX of hundred grades with molecular weight cut-off, obtain trapped fluid X and permeate XI;
E () is dry respectively by trapped fluid IV, trapped fluid VI, trapped fluid VIII and trapped fluid X, obtain the soluble polysaccharide product of different molecular weight.
In the present invention, use ultra-filtration membrane and/or the nanofiltration membrane of PSPP, polysaccharide component containing corresponding molecular weight cut-off will be obtained (such as, with the ultrafiltration membrance filter that molecular weight cut-off is 100,000 grades, the soluble polysaccharide molecular weight product in trapped fluid is 100,000 grades).After measured, the molecular-weight average of the soluble polysaccharide that trapped fluid IV drying obtains is more than 150kDa, the molecular-weight average of the soluble polysaccharide that trapped fluid VI drying obtains is about 10kDa, the molecular-weight average of the soluble polysaccharide that trapped fluid VIII drying obtains is about 2kDa, and the molecular-weight average of the soluble polysaccharide that trapped fluid X drying obtains is about 200Da.
Carry out pre-treatment with ethanolic soln, the benzyl carbinol glycosides, micromolecular polysaccharide and other alcohol soluble substances that contain in Herba Cistanches can be removed; And the Aqueous extracts obtained after solid-liquid separation containing enriching soluble polysaccharide, the soluble polysaccharide purified water contained in these Herba Cistanchess leaches.The present invention adopts the membrane filtration of PSPP, successively soluble polysaccharide is carried out fractional separation, thus prepares the soluble polysaccharide product of different molecular weight.
Preferably, described Herba Cistanches is Desert Herba Cistanches, Cistanche Tubulosa, spend the combination of a kind of in the fleshy stem of Herba Cistanches or Herba Cistanches sinensis or at least two kinds in vain, it can be such as Desert Herba Cistanches, Cistanche Tubulosa, spend the combination of Herba Cistanches and Herba Cistanches sinensis fleshy stem in vain, or the combination of Desert Herba Cistanches, Cistanche Tubulosa and Herba Cistanches sinensis fleshy stem.
Preferably, it is 20-60 order that described Herba Cistanches is crushed to granularity, can be such as 20 orders, 22 orders, 24 orders, 26 orders, 28 orders, 30 orders, 32 orders, 34 orders, 36 orders, 38 orders, 40 orders, 42 orders, 44 orders, 46 orders, 48 orders, 50 orders, 52 orders, 54 orders, 56 orders, 58 orders or 60 orders, be preferably 40 orders.
Preferably, in described ethanolic soln, the volume percent of ethanol is 40-100%, such as, can be 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95% or 100%, is preferably 70-90%.
Preferably, described ethanolic soln is in units of L, and Herba Cistanches is in units of kg, and the liquid-solid ratio of the two is (10-30): 1, can be such as 10:1,12:1,14:1,15:1,16:1,18:1,20:1,22:1,24:1,26:1,28:1 or 30:1, be preferably 15:1.
Preferably, the pretreated temperature of described ethanolic soln is 20-80 DEG C, such as, can be 20 DEG C, 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C or 80 DEG C, is preferably 50-70 DEG C, is more preferably 60 DEG C.
Preferably, the described ethanolic soln pretreated time is 30-90min, such as, can be 30min, 35min, 40min, 45min, 50min, 55min, 60min, 65min, 70min, 75min, 80min, 85min or 90min, is preferably 60min.
Preferably, step (1) is heating purified water, then solid-liquid separation, obtains clear liquid I and filter residue II.In the present invention, the purified water containing filter residue can be divided into some parts to be separated, to ensure the effect of filtering, then clear liquid be merged, finally obtain clear liquid I.
Preferably, described solid-liquid separation is three-step approach, the liquid-solid ratio substep of purified water and Herba Cistanches successively decreases, described purified water is in units of L, Herba Cistanches is in units of kg, the purified water of the first step and the liquid-solid ratio of Herba Cistanches are (15-20): 1 (can be such as 15:1, 15.5:1, 16:1, 16.5:1, 17:1, 17.5:1, 18:1, 18.5:1, 19:1, 19.5:1 or 20:1), the purified water of second step and the liquid-solid ratio of Herba Cistanches are (8-10): 1 (can be such as 8:1, 8.2:1, 8.4:1, 8.6:1, 8.8:1, 9:1, 9.2:1, 9.4:1, 9.6:1, 9.8:1 or 10:1), the purified water of the 3rd step and the liquid-solid ratio of Herba Cistanches are 5:1.
Preferably, the temperature of described purified water is 20-100 DEG C, can be such as 20 DEG C, 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C, 95 DEG C or 100 DEG C, be preferably 60-90 DEG C, be more preferably 80 DEG C.
Preferably, after in described three-step approach, the purified water temperature of a step is greater than or equal to the purified water temperature of back.
Preferably, in each step of described three-step approach, the mixing time of purified water and Herba Cistanches is 30-180min, can be such as 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min, 130min, 140min, 150min, 160min, 170min or 180min, be preferably 60-120min, be more preferably 90min.
Preferably, described microfiltration membrane is hollow fiber microfiltration membrane, spiral wound microfiltration membrane or ceramic microfiltration membrane.
Preferably, the aperture of described microfiltration membrane is 0.10 μm-1.00 μm, can be such as 0.10 μm, 0.20 μm, 0.30 μm, 0.40 μm, 0.50 μm, 0.60 μm, 0.70 μm, 0.80 μm, 0.90 μm or 1.00 μm, be preferably 0.22 μm or 0.45 μm.
Preferably, described molecular weight cut-off is the ultra-filtration membrane of 100,000 grades is spiral wound ultra-filtration membrane.
Preferably, described molecular weight cut-off is the molecular weight cut-off of the ultra-filtration membrane of 100,000 grades is 100-500kDa, such as, can be 100kDa, 150kDa, 200kDa, 250kDa, 300kDa, 350kDa, 400kDa, 450kDa or 500kDa.
Preferably, the density of described trapped fluid IV is 1.00-1.10g/cm
3, such as, can be 1.00g/cm
3, 1.01g/cm
3, 1.02g/cm
3, 1.03g/cm
3, 1.04g/cm
3, 1.05g/cm
3, 1.06g/cm
3, 1.07g/cm
3, 1.08g/cm
3, 1.09g/cm
3or 1.10g/cm
3, be preferably 1.01-1.05g/cm
3, be more preferably 1.03g/cm
3.
Preferably, drying is carried out to trapped fluid IV.
Preferably, the mode of described drying is any one in spraying dry, vacuum and heating drying or vacuum lyophilization.
Preferably, described molecular weight cut-off is the ultra-filtration membrane of ten thousand grades is spiral wound ultra-filtration membrane.
Preferably, described molecular weight cut-off is the molecular weight cut-off of the ultra-filtration membrane of ten thousand grades is 10-50kDa, such as, can be 10kDa, 15kDa, 20kDa, 25kDa, 30kDa, 35kDa, 40kDa, 45kDa or 50kDa.
Preferably, the density of described trapped fluid VI is 1.00-1.10g/cm
3, such as, can be 1.00g/cm
3, 1.01g/cm
3, 1.02g/cm
3, 1.03g/cm
3, 1.04g/cm
3, 1.05g/cm
3, 1.06g/cm
3, 1.07g/cm
3, 1.08g/cm
3, 1.09g/cm
3or 1.10g/cm
3, be preferably 1.01-1.05g/cm
3, be more preferably 1.03g/cm
3.
Preferably, drying is carried out to trapped fluid VI.
Preferably, the mode of described drying is vacuum and heating drying or vacuum lyophilization.
Preferably, described molecular weight cut-off is the ultra-filtration membrane of thousand grades is spiral wound ultra-filtration membrane.
Preferably, described molecular weight cut-off is the molecular weight cut-off of the ultra-filtration membrane of thousand grades is 1-5kDa, such as, can be 1kDa, 1.5kDa, 2kDa, 2.5kDa, 3kDa, 3.5kDa, 4kDa, 4.5kDa or 5kDa.
Preferably, the density of described trapped fluid VIII is 1.00-1.10g/cm
3, such as, can be 1.00g/cm
3, 1.01g/cm
3, 1.02g/cm
3, 1.03g/cm
3, 1.04g/cm
3, 1.05g/cm
3, 1.06g/cm
3, 1.07g/cm
3, 1.08g/cm
3, 1.09g/cm
3or 1.10g/cm
3, be preferably 1.01-1.05g/cm
3, be more preferably 1.03g/cm
3.
Preferably, drying is carried out to trapped fluid VIII.
Preferably, the mode of described drying is vacuum lyophilization.
Preferably, described molecular weight cut-off is the nanofiltration membrane of hundred grades is spiral wound nanofiltration membrane.
Preferably, described molecular weight cut-off is the molecular weight cut-off of the nanofiltration membrane of hundred grades is 200Da-500Da, can be such as 200Da, 220Da, 240Da, 260Da, 280Da, 300Da, 320Da, 340Da, 360Da, 380Da, 400Da, 420Da, 440Da, 460Da, 480Da or 500Da, be preferably 200Da or 500Da.
Preferably, the density of described trapped fluid X is 1.00-1.10g/cm
3, such as, can be 1.00g/cm
3, 1.01g/cm
3, 1.02g/cm
3, 1.03g/cm
3, 1.04g/cm
3, 1.05g/cm
3, 1.06g/cm
3, 1.07g/cm
3, 1.08g/cm
3, 1.09g/cm
3or 1.10g/cm
3, be preferably 1.01-1.05g/cm
3, be more preferably 1.03g/cm
3.
Preferably, drying is carried out to trapped fluid X.
Preferably, the mode of described drying is vacuum lyophilization.
Compared with prior art, the present invention at least has following beneficial effect:
The method of the invention is first with the small molecules carbohydrate in ethanolic soln removing Herba Cistanches and alcohol soluble substance, with the soluble polysaccharide in purified water extraction Herba Cistanches after filter residue and drying, after solid-liquid separation, clear liquid micro-filtrate membrane filtration removes suspended substance, and micro-filtration gained permeate is respectively with the wheat-based diet of molecular weight cut-off to be the ultra-filtration membrane of 100,000 grades, ten thousand grades and thousand grades and molecular weight cut-off the be nanofiltration membrane of hundred grades retains different polymerization degree.The polysaccharide product molecular weight that method of the present invention prepares is concentrated, physicochemical characteristics and biological activity consistent, achieve the fractional separation of wheat-based diet, improve the utilization ratio of main component in Herba Cistanches, wheat-based diet product is become more meticulous, add the Additional Value of Commodities of Herba Cistanches, widen the Application Areas of Herba Cistanches.
Secondly, method of the present invention only uses ethanol in preprocessing process, compared with the method for the multiplex alcohol precipitation of prior art, greatly can reduce the usage quantity of ethanol, reduces production cost and stores ethanol and reclaim the time and operation that consume; In addition, utilize the process of membrane filtration fractional separation to be namely the concentration process of product, do not need other enrichment step, reduce energy consumption and the operation of production process.
Finally, method equipment used of the present invention is conventional equipment, can realize the operate continuously of production process, with short production cycle, less investment, high efficiency; In the production process of product, do not use any poisonous and harmful reagent, the polysaccharide product security of acquisition has sufficient guarantee.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the inventive method.
Embodiment
Technical scheme of the present invention is further illustrated below by embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get Desert Herba Cistanches 10kg, pulverized 40 mesh sieves, add the ethanolic soln of 150L volume fraction 80%, extract 60min at 60 DEG C, extracting solution 500 order filter-cloth filtering, filter residue is air-dry.The Herba Cistanches filter residue of drying is placed in the purified water of 200L, 60min is extracted at 60 DEG C, extracting solution 500 order filter-cloth filtering, the purified water that first filter residue adds 80L extracts 90min at 80 DEG C, extracting solution 500 order filter-cloth filtering, secondary filter residue extracts 120min at adding 50L purified water 90 DEG C, extracting solution 500 order filter-cloth filtering, extracts the clear liquid filtering gained merge about 270L by three times.The clear liquid of the ceramic micro filter membrane filtration gained of 0.45 micron pore size, obtains permeate, is 300kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.10g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV lyophilize obtains 0.2kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 50kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI lyophilize obtains 0.4kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 5kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize obtains 0.4kg soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 500Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains polysaccharide product 0.8kg soluble polysaccharide product D, molecular-weight average about 200Da.
Embodiment 2
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get Desert Herba Cistanches 10kg, pulverized 60 mesh sieves, add the ethanolic soln of 150L volume fraction 95%, extract 90min at 50 DEG C, extracting solution 300 order filter-cloth filtering, filter residue is air-dry.The Herba Cistanches filter residue of drying is placed in the purified water of 150L, 60min is extracted at 70 DEG C, extracting solution 500 order filter-cloth filtering, the purified water that first filter residue adds 100L extracts 60min at 90 DEG C, extracting solution 300 order filter-cloth filtering, purified water extraction 90min at secondary filter residue adds 50L90 DEG C, extracting solution 500 order filter-cloth filtering, extracts three times the clear liquid filtering gained and merges about 250L.The clear liquid of the spiral wound membrane filtration gained of 0.22 micron pore size, obtains permeate, is 500kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV spraying dry obtains 0.1kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 50kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.10g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI vacuum-drying obtains 0.4kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 5kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize obtains 0.4kg soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 200Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.10g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains 1.2kg soluble polysaccharide product D, molecular-weight average about 200Da.
Embodiment 3
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get Desert Herba Cistanches 10kg, pulverized 20 mesh sieves, add the ethanolic soln of 100L volume fraction 40%, extract 30min at 20 DEG C, extracting solution 500 order filter-cloth filtering, filter residue is dried.The Herba Cistanches filter residue of drying is placed in the purified water of 200L, 60min is extracted at 100 DEG C, extracting solution 300 order filter-cloth filtering, the purified water that first filter residue adds 100L extracts 60min at 100 DEG C, extracting solution 300 order filter-cloth filtering, secondary filter residue extracts 60min at adding 50L purified water 100 DEG C, extracting solution 500 order filter-cloth filtering, extracts the clear liquid filtering gained merge about 290L by three times.The clear liquid of the ceramic micro filter membrane filtration gained of 1.00 micron pore size, obtains permeate, is 500kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV spraying dry obtains 0.1kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 50kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI vacuum-drying obtains 0.5kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 1kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.10g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize obtains 0.5kg soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 200Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.01g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains 1.0kg soluble polysaccharide product D, molecular-weight average about 200Da.
Embodiment 4
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get Desert Herba Cistanches 10kg, pulverized 20 mesh sieves, add the ethanolic soln of 300L volume fraction 90%, extract 30min at 70 DEG C, extracting solution 500 order filter-cloth filtering, filter residue is air-dry.The Herba Cistanches filter residue of drying is placed in the purified water of 200L, 180min is extracted at 20 DEG C, extracting solution 500 order filter-cloth filtering, the purified water that first filter residue adds 100L extracts 120min at 50 DEG C, extracting solution 500 order filter-cloth filtering, secondary filter residue extracts 90min at adding 50L purified water 80 DEG C, extracting solution 500 order filter-cloth filtering, extracts the clear liquid filtering gained merge about 310L by three times.The clear liquid of the ceramic micro filter membrane filtration gained of 1.00 micron pore size, obtains permeate, is 100kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV vacuum-drying obtains 0.4kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 10kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.01g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI lyophilize obtains 0.2kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 3kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.01g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize obtains 0.8kg soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 200Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains 0.7kg soluble polysaccharide product D, molecular-weight average about 200Da.
Embodiment 5
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get Desert Herba Cistanches 10kg, pulverized 40 mesh sieves, add the ethanolic soln of 150L volume fraction 70%, extract 30min at 80 DEG C, extracting solution 500 order filter-cloth filtering, filter residue is air-dry.The Herba Cistanches filter residue of drying is placed in the purified water of 150L, 120min is extracted at 60 DEG C, extracting solution 500 order filter-cloth filtering, the purified water that first filter residue adds 100L extracts 120min at 70 DEG C, extracting solution 500 order filter-cloth filtering, secondary filter residue extracts 120min at adding 50L purified water 80 DEG C, extracting solution 500 order filter-cloth filtering, extracts the clear liquid filtering gained merge about 250L by three times.The clear liquid of the spiral wound micro-filtrate membrane filtration gained of 0.10 micron pore size, obtains permeate, is 300kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV lyophilize obtains 0.2kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 30kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI lyophilize obtains 0.2kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 2kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize obtains 0.8kg soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 500Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains 0.5kg soluble polysaccharide product D, molecular-weight average about 200Da.
Embodiment 6
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get Desert Herba Cistanches 10kg, pulverized 40 mesh sieves, add the ethanolic soln of 150L volume fraction 80%, extract 60min at 60 DEG C, extracting solution 500 order filter-cloth filtering, filter residue is air-dry.The Herba Cistanches filter residue of drying is placed in the purified water of 180L, 120min is extracted at 50 DEG C, extracting solution 500 order filter-cloth filtering, the purified water that first filter residue adds 80L extracts 90min at 80 DEG C, extracting solution 500 order filter-cloth filtering, secondary filter residue extracts 30min at adding 50L purified water 100 DEG C, extracting solution 500 order filter-cloth filtering, extracts the clear liquid filtering gained merge about 260L by three times.The clear liquid of the spiral wound micro-filtrate membrane filtration gained of 0.45 micron pore size, obtains permeate, is 300kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV lyophilize obtains 0.2kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 30kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI lyophilize obtains 0.4kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 3kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize obtains 0.4kg soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 500Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains 0.5kg soluble polysaccharide product D, molecular-weight average about 200Da.
Embodiment 7
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get Desert Herba Cistanches 10kg, pulverized 20 mesh sieves, add the ethanolic soln of 150L volume fraction 60%, extract 60min at 50 DEG C, extracting solution 500 order filter-cloth filtering, filter residue is air-dry.The Herba Cistanches filter residue of drying is placed in the purified water of 150L, 90min is extracted at 80 DEG C, extracting solution 500 order filter-cloth filtering, the purified water that first filter residue adds 80L extracts 90min at 80 DEG C, extracting solution 500 order filter-cloth filtering, secondary filter residue extracts 60min at adding 50L purified water 90 DEG C, extracting solution 500 order filter-cloth filtering, extracts the clear liquid filtering gained merge about 230L by three times.The clear liquid of the spiral wound micro-filtrate membrane filtration gained of 0.45 micron pore size, obtains permeate, is 100kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV lyophilize obtains 0.4kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 30kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.01g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI lyophilize obtains 0.2kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 3kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.01g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize obtains 0.4kg soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 200Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains 0.5kg soluble polysaccharide product D, molecular-weight average about 200Da.
Embodiment 8
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get Cistanche Tubulosa 10kg, pulverized 40 mesh sieves, add the ethanolic soln of 150L volume fraction 60%, extract 60min at 50 DEG C, extracting solution 300 order filter-cloth filtering, filter residue is air-dry.The Herba Cistanches filter residue of drying is placed in the purified water of 150L, 90min is extracted at 70 DEG C, extracting solution 500 order filter-cloth filtering, the purified water that first filter residue adds 80L extracts 90min at 80 DEG C, extracting solution 500 order filter-cloth filtering, secondary filter residue extracts 60min at adding 50L purified water 90 DEG C, extracting solution 500 order filter-cloth filtering, extracts the clear liquid filtering gained merge about 230L by three times.The clear liquid of the spiral wound micro-filtrate membrane filtration gained of 0.22 micron pore size, obtains permeate, is 500kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.01g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV lyophilize obtains 0.1kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 10kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.10g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI lyophilize obtains 0.4kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 3kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.01g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize obtains 0.3kg soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 500Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains 0.6kg soluble polysaccharide product D, molecular-weight average about 200Da.
Embodiment 9
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get and spend Herba Cistanches 10kg in vain, pulverized 20 mesh sieves, add the ethanolic soln of 150L volume fraction 80%, extract 60min at 60 DEG C, extracting solution 300 order filter-cloth filtering, filter residue is air-dry.The Herba Cistanches filter residue of drying is placed in the purified water of 160L, 90min is extracted at 60 DEG C, extracting solution 500 order filter-cloth filtering, the purified water that first filter residue adds 90L extracts 90min at 80 DEG C, extracting solution 500 order filter-cloth filtering, secondary filter residue extracts 60min at adding 50L purified water 90 DEG C, extracting solution 500 order filter-cloth filtering, extracts the clear liquid filtering gained merge about 240L by three times.The clear liquid of the spiral wound micro-filtrate membrane filtration gained of 0.22 micron pore size, obtains permeate, is 500kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.01g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV lyophilize obtains 0.1kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 50kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI lyophilize obtains 0.3kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 5kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize obtains 0.5kg soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 200Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains 1.2kg soluble polysaccharide product D, molecular-weight average about 200Da.
Embodiment 10
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get Herba Cistanches sinensis 10kg, pulverized 40 mesh sieves, add the ethanolic soln of 200L volume fraction 80%, extract 60min at 60 DEG C, extracting solution 300 order filter-cloth filtering, filter residue is air-dry.The Herba Cistanches filter residue of drying is placed in the purified water of 180L, 90min is extracted at 70 DEG C, extracting solution 500 order filter-cloth filtering, the purified water that first filter residue adds 90L extracts 90min at 80 DEG C, extracting solution 500 order filter-cloth filtering, secondary filter residue extracts 30min at adding 50L purified water 90 DEG C, extracting solution 500 order filter-cloth filtering, extracts the clear liquid filtering gained merge about 270L by three times.The clear liquid of the spiral wound micro-filtrate membrane filtration gained of 0.45 micron pore size, obtains permeate, is 500kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV lyophilize obtains 0.1kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 50kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI lyophilize obtains 0.2kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 5kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize obtains 0.5kg soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 500Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains 0.9kg soluble polysaccharide product D, molecular-weight average about 200Da.
Embodiment 11
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get Desert Herba Cistanches and Cistanche Tubulosa mixture 10kg, pulverized 40 mesh sieves, and added the ethanolic soln of 150L volume fraction 60%, and extracted 60min at 50 DEG C, extracting solution 300 order filter-cloth filtering, filter residue is air-dry.The Herba Cistanches filter residue of drying is placed in the purified water of 150L, 90min is extracted at 70 DEG C, extracting solution 500 order filter-cloth filtering, the purified water that first filter residue adds 80L extracts 90min at 80 DEG C, extracting solution 500 order filter-cloth filtering, secondary filter residue extracts 60min at adding 50L purified water 90 DEG C, extracting solution 500 order filter-cloth filtering, extracts the clear liquid filtering gained merge about 230L by three times.The clear liquid of the spiral wound micro-filtrate membrane filtration gained of 0.22 micron pore size, obtains permeate, is 300kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV lyophilize obtains 0.2kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 30kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.05g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI lyophilize obtains 0.4kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 3kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize obtains 0.4kg soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 200Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains 1.0kg soluble polysaccharide product D, molecular-weight average about 200Da.
Embodiment 12
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get Desert Herba Cistanches 1kg, pulverized 40 mesh sieves, add the ethanolic soln of 30L volume fraction 100%, extract 60min at 60 DEG C, extracting solution 500 order filter-cloth filtering, filter residue is air-dry.The Herba Cistanches filter residue of drying is placed in the purified water of 20L, 60min is extracted at 60 DEG C, extracting solution 500 order filter-cloth filtering, the purified water that first filter residue adds 8L extracts 90min at 80 DEG C, extracting solution 500 order filter-cloth filtering, secondary filter residue extracts 120min at adding 5L purified water 90 DEG C, extracting solution 500 order filter-cloth filtering, extracts the clear liquid filtering gained merge about 29L by three times.The hollow fiber microfiltration membrane of 0.22 micron pore size filters the clear liquid of gained, and obtaining permeate, is 500kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.00g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV lyophilize obtains 0.01kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 50kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.00g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI lyophilize obtains 0.04kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 5kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.00g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize 0.04kg obtains soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 500Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.00g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains 0.11kg soluble polysaccharide product D, molecular-weight average about 200Da.
Embodiment 13
The present embodiment adopts the fractional separation of carrying out polysaccharide in Herba Cistanches with the following method:
Get Desert Herba Cistanches and the mixture 1kg spending Herba Cistanches in vain, pulverized 60 mesh sieves, and added the ethanolic soln of 15L volume fraction 100%, and extracted 90min at 50 DEG C, extracting solution 500 order filter-cloth filtering, filter residue is air-dry.The Herba Cistanches filter residue of drying is placed in the purified water of 15L, 90min is extracted at 80 DEG C, extracting solution 500 order filter-cloth filtering, the purified water that first filter residue adds 10L extracts 90min at 80 DEG C, extracting solution 500 order filter-cloth filtering, secondary filter residue extracts 90min at adding 5L purified water 90 DEG C, extracting solution 500 order filter-cloth filtering, extracts the clear liquid filtering gained merge about 25L by three times.The hollow fiber microfiltration membrane of 0.45 micron pore size filters the clear liquid of gained, and obtaining permeate, is 300kDa spiral wound ultrafiltration membrance filter by permeate interception, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.03g/cm
3in time, stops filtering, and obtain trapped fluid IV and permeate V, trapped fluid IV lyophilize obtains 0.02kg soluble polysaccharide product A, more than molecular-weight average 150kDa.
Permeate V interception is 50kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.00g/cm
3in time, stops filtering, and obtain trapped fluid VI and permeate VII, trapped fluid VI lyophilize obtains 0.02kg soluble polysaccharide product B, molecular-weight average about 10kDa.
Permeate VII interception is 5kDa spiral wound ultrafiltration membrance filter, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.00g/cm
3in time, stops filtering, and obtain trapped fluid VIII and permeate IX, trapped fluid VIII lyophilize obtains 0.04kg soluble polysaccharide products C, molecular-weight average about 2kDa.
Permeate IX interception is 500Da spiral wound nanofiltration membrane, and filtration terminates front trapped fluid purified water and constantly washs, and trapped fluid density is 1.00g/cm
3in time, stops filtering, and obtain trapped fluid X and permeate XI, trapped fluid X lyophilize obtains 0.09kg soluble polysaccharide product D, molecular-weight average about 200Da.
Applicant states, the present invention illustrates processing method of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned processing step, does not namely mean that the present invention must rely on above-mentioned processing step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of raw material selected by the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. the method for fractional separation polysaccharide from Herba Cistanches, is characterized in that, comprise the steps:
(1) get Herba Cistanches fleshy stem, pulverize, carry out pre-treatment with ethanolic soln, in the filter residue obtained, add purified water, solid-liquid separation, obtain clear liquid I and filter residue II;
(2) use micro-filtrate membrane filtration clear liquid I, obtain permeate;
(3) adopt molecular weight cut-off to be ultra-filtration membrane, the molecular weight cut-off of 100,000 grades to be the ultra-filtration membrane of ten thousand grades successively, molecular weight cut-off is the ultra-filtration membrane of thousand grades and molecular weight cut-off is the nanofiltration membrane permeate of hundred grades, obtains the soluble polysaccharide product of different molecular weight.
2. method according to claim 1, is characterized in that, step (3) is:
A () is the ultrafiltration membrance filter permeate of 100,000 grades with molecular weight cut-off, obtain trapped fluid IV and permeate V;
B () is the ultrafiltration membrance filter permeate V of ten thousand grades with molecular weight cut-off, obtain trapped fluid VI and permeate VII;
C () is the ultrafiltration membrance filter permeate VII of thousand grades with molecular weight cut-off, obtain trapped fluid VIII and permeate IX;
D () is the nanofiltration membrane permeate IX of hundred grades with molecular weight cut-off, obtain trapped fluid X and permeate XI;
E () is dry respectively by trapped fluid IV, trapped fluid VI, trapped fluid VIII and trapped fluid X, obtain the soluble polysaccharide product of different molecular weight.
3. method according to claim 1 and 2, is characterized in that, described Herba Cistanches is Desert Herba Cistanches, Cistanche Tubulosa, spend the combination of a kind of in the fleshy stem of Herba Cistanches or Herba Cistanches sinensis or at least two kinds in vain;
Preferably, it is 20-60 order that described Herba Cistanches is crushed to granularity, is preferably 40 orders.
4. according to the method one of claim 1-3 Suo Shu, it is characterized in that, in described ethanolic soln, the volume percent of ethanol is 40-100%, is preferably 70-90%;
Preferably, described ethanolic soln is in units of L, and Herba Cistanches is in units of kg, and the liquid-solid ratio of the two is (10-30): 1, is preferably 15:1;
Preferably, the pretreated temperature of described ethanolic soln is 20-80 DEG C, is preferably 50-70 DEG C, is more preferably 60 DEG C;
Preferably, the described ethanolic soln pretreated time is 30-90min, is preferably 60min.
5. according to the method one of claim 1-4 Suo Shu, it is characterized in that, step (1) is heating purified water, then solid-liquid separation, obtains clear liquid I and filter residue II;
Preferably, described solid-liquid separation is three-step approach, the liquid-solid ratio substep of purified water and Herba Cistanches successively decreases, described purified water is in units of L, Herba Cistanches is in units of kg, the purified water of the first step and the liquid-solid ratio of Herba Cistanches are (15-20): 1, and the purified water of second step and the liquid-solid ratio of Herba Cistanches are (8-10): the purified water of the 1, three step and the liquid-solid ratio of Herba Cistanches are 5:1;
Preferably, the temperature of described purified water is 20-100 DEG C, is preferably 60-90 DEG C, is more preferably 80 DEG C;
Preferably, after in described three-step approach, the purified water temperature of a step is greater than or equal to the purified water temperature of back;
Preferably, in each step of described three-step approach, the mixing time of purified water and Herba Cistanches is 30-180min, is preferably 60-120min, is more preferably 90min.
6. according to the method one of claim 1-5 Suo Shu, it is characterized in that, described microfiltration membrane is hollow fiber microfiltration membrane, spiral wound microfiltration membrane or ceramic microfiltration membrane;
Preferably, the aperture of described microfiltration membrane is 0.10 μm-1.00 μm, is preferably 0.22 μm or 0.45 μm.
7. according to the method one of claim 1-6 Suo Shu, it is characterized in that, described molecular weight cut-off is the ultra-filtration membrane of 100,000 grades is spiral wound ultra-filtration membrane;
Preferably, described molecular weight cut-off is the molecular weight cut-off of the ultra-filtration membrane of 100,000 grades is 100-500kDa;
Preferably, the density of described trapped fluid IV is 1.00-1.10g/cm
3, be preferably 1.01-1.05g/cm
3, be more preferably 1.03g/cm
3;
Preferably, drying is carried out to trapped fluid IV;
Preferably, the mode of described drying is any one in spraying dry, vacuum and heating drying or vacuum lyophilization.
8. according to the method one of claim 1-7 Suo Shu, it is characterized in that, described molecular weight cut-off is the ultra-filtration membrane of ten thousand grades is spiral wound ultra-filtration membrane;
Preferably, described molecular weight cut-off is the molecular weight cut-off of the ultra-filtration membrane of ten thousand grades is 10-50kDa;
Preferably, the density of described trapped fluid VI is 1.00-1.10g/cm
3, be preferably 1.01-1.05g/cm
3, be more preferably 1.03g/cm
3;
Preferably, drying is carried out to trapped fluid VI;
Preferably, the mode of described drying is vacuum and heating drying or vacuum lyophilization.
9. according to the method one of claim 1-8 Suo Shu, it is characterized in that, described molecular weight cut-off is the ultra-filtration membrane of thousand grades is spiral wound ultra-filtration membrane;
Preferably, described molecular weight cut-off is the molecular weight cut-off of the ultra-filtration membrane of thousand grades is 1-5kDa;
Preferably, the density of described trapped fluid VIII is 1.00-1.10g/cm
3, be preferably 1.01-1.05g/cm
3, be more preferably 1.03g/cm
3;
Preferably, drying is carried out to trapped fluid VIII;
Preferably, the mode of described drying is vacuum lyophilization.
10. according to the method one of claim 1-9 Suo Shu, it is characterized in that, described molecular weight cut-off is the nanofiltration membrane of hundred grades is spiral wound nanofiltration membrane;
Preferably, described molecular weight cut-off is the molecular weight cut-off of the nanofiltration membrane of hundred grades is 200Da-500Da, is preferably 200Da or 500Da;
Preferably, the density of described trapped fluid X is 1.00-1.10g/cm
3, be preferably 1.01-1.05g/cm
3, be more preferably 1.03g/cm
3;
Preferably, drying is carried out to trapped fluid X;
Preferably, the mode of described drying is vacuum lyophilization.
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| CN113121717A (en) * | 2021-05-13 | 2021-07-16 | 中国科学院西北高原生物研究所 | Extraction and optimization method of polysaccharide of cistanche deserticola Ma |
| CN114621363A (en) * | 2022-03-28 | 2022-06-14 | 内蒙古大漠魂生物科技有限公司 | Cistanche polysaccharide with anti-fatigue effect |
| CN115227741A (en) * | 2022-06-09 | 2022-10-25 | 新疆汇峰农业科技有限公司 | Cistanche deserticola extract purification method and equipment |
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