CN104926954A - Method for separating and preparing polysaccharide, oligosaccharide and mannitol from cistanche - Google Patents
Method for separating and preparing polysaccharide, oligosaccharide and mannitol from cistanche Download PDFInfo
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- CN104926954A CN104926954A CN201510346059.0A CN201510346059A CN104926954A CN 104926954 A CN104926954 A CN 104926954A CN 201510346059 A CN201510346059 A CN 201510346059A CN 104926954 A CN104926954 A CN 104926954A
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Abstract
The invention provides a method for separating and preparing polysaccharide, oligosaccharide and mannitol from cistanche. The method includes: obtaining fleshy stems from cistanche and smashing the same, adding purified water for extraction and performing solid-liquid separation to obtain clear liquid I and residues II; filtering the clear liquid I with a micro-filtration membrane to obtain permeable liquid III; filtering the permeable liquid III with an ultrafiltration membrane to obtain permeable liquid V and intercepted liquid VII containing a polysaccharide product; filtering permeable liquid V with nanofiltration membrane to obtain intercepted liquid VI containing an oligosaccharide product and intercepted liquid VII containing a mannitol product. With the method, cistanche polysaccharide, the oligosaccharide and the mannitol high in purity are easily and rapidly separated and prepared, the production process is simple, the period is short, three products of the polysaccharide, the oligosaccharide and the mannitol are developed at one step, and the method is good in industrial production and market development prospect.
Description
Technical field
The invention belongs to technical field of biochemical separation, from Herba Cistanches, the while of relating to a kind of, be separated the method preparing polysaccharide, oligose and N.F,USP MANNITOL.
Background technology
Herba Cistanches is the perennial plant that one belongs to Orobanchaceae (Orobanchaceae) Cistanche deserticola (Cistanche Hoffmg.etLink), and obligatory parasitism is in the root of sacsaoul class plant, and the whole world about has 22 kinds.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 is for a long time as a class rare Chinese medicine, have another name called rue greatly, sweetly to rue greatly, desert cistanche, Herba Cistanches, essence etc., begin to be loaded in Shennong's Herbal, successive dynasties medicine book all has detailed record to it, be listed in top grade medicinal material, there is warming and recuperating the kidney-YANG, benefiting essence-blood, effect of relaxing bowel, be widely used in that insufficiency of kidney-YANG, blood and essence asthenia, impotence are infertile clinically, the unable and dry constipation of intestines of soreness of the waist and knees, muscles and bones.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 has polysaccharide, 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 diabetes B.
N.F,USP MANNITOL is national essential drugs, includes in " Chinese Pharmacopoeia ".The character of N.F,USP MANNITOL is relatively stable, not easily be oxidized by the oxygen in air, to the good stability of diluted acid, diluted alkaline and heat.N.F,USP MANNITOL Regular Insulin in human body metabolism's approach and body is uncorrelated, is not suitable as the nutrition source of oral microorganism, thus unlikely carious tooth, so N.F,USP MANNITOL is widely used in food service industry, pharmaceutical industries.N.F,USP MANNITOL can be used as osmotic diuretic and dehydrant, its injection liquid can be used for reducing intracranial pressure, intraocular pressure, diuresis and prevent and treat early stage acute renal insufficiency, also can make compound with amino acid ligand infuses for chewable tablet and diabetic subject, obese person and anticariogenic sweeting agents such as fresheners in hangover medicine, mouth, also deep processing can synthesize medicinal derivative etc. further simultaneously.Larger gap is also there is between the supply of current domestic N.F,USP MANNITOL and requirement.
Be that raw material is prepared in the process of benzyl carbinol glycosides and polysaccharide with Herba Cistanches, the N.F,USP MANNITOL of rich content often cannot be recycled because being difficult to obtain sterling, and oligose also because being difficult to make dry product, or is difficult to after drying preserve and transport and give up.
Therefore, expect that exploitation is a kind of in the art and can be separated the method obtaining polysaccharide, oligose and N.F,USP MANNITOL product from Herba Cistanches simultaneously.
Summary of the invention
For the deficiencies in the prior art, a kind of separation from Herba Cistanches is the object of the present invention is to provide to prepare the method for polysaccharide, oligose and N.F,USP MANNITOL.Described method production technique is simple, and the cycle is short, achieves the preparation of the sharp separation of Herba Cistanches carbohydrate, high purity N.F,USP MANNITOL, improves the Additional Value of Commodities of Herba Cistanches, has widened the Application Areas of Herba Cistanches.
For reaching this goal of the invention, the present invention by the following technical solutions:
On the one hand, the invention provides a kind of separation from Herba Cistanches and prepare the method for polysaccharide, oligose and N.F,USP MANNITOL, said method comprising the steps of:
(1) get the fleshy stem of Herba Cistanches, pulverize, then add Aqua pure extract and carry out solid-liquid separation, obtaining clear liquid I and residual II;
(2) micro-filtrate membrane filtration clear liquid I, obtains permeate III;
(3) ultrafiltration membrance filter permeate III, obtains permeate V and the trapped fluid IV containing polysaccharide product;
(4) nanofiltration membrane permeate V, obtains the trapped fluid VI containing oligose product and the permeate VII containing N.F,USP MANNITOL product.
Containing abundant soluble polysaccharide in Herba Cistanches, oligose and a certain amount of free N.F,USP MANNITOL, all soluble in water, be thus easy to pure water and leach.Aqueous extracts with the membrane filter method of PSPP, can isolate polysaccharide, oligose, the N.F,USP MANNITOL that in permeate, content is more successively, and available crystallization process is separated out and purifying.The disposable separation from Herba Cistanches of the method obtains N.F,USP MANNITOL, oligosaccharide syrup and polysaccharide 3 kinds of products, technique is simple, required equipment is conventional equipment, and organic reagent only relates to ethanol, pollution-free, workable, reduce Herba Cistanches production cost, shorten the production cycle, improve the utilization ratio of main component in Herba Cistanches, add the Additional Value of Commodities of Herba Cistanches, widened Herba Cistanches and utilized field.
Preferably, described Herba Cistanches be Desert Herba Cistanches, the combination of Cistanche Tubulosa, any one or at least two kinds spent in vain in the fleshy stem of Herba Cistanches or Herba Cistanches sinensis.
Preferably, clear liquid for adding Aqua pure extract 1 ~ 3 time, then solid-liquid separation, and merges by step (1), obtains clear liquid I and residual II.
Preferably, in step (1), Herba Cistanches degree of grinding is 10 ~ 60 orders, such as 10 orders, 15 orders, 20 orders, 25 orders, 30 orders, 35 orders, 40 orders, 45 orders, 50 orders, 55 orders or 60 orders, and more preferably, Herba Cistanches degree of grinding is 20 ~ 40 orders;
Preferably, in step (1), the liquid-solid ratio of pure water and Herba Cistanches is 8:1 ~ 40:1, such as 8:1,9:1,10:1,11:1,12:1,13:1,14:1,15:1,16:1,17:1,18:1,19:1,20:1,22:1,24:1,26:1,28:1,30:1,32:1,34:1,36:1,38:1 or 40:1, preferred 10:1 ~ 20:1, further preferred 15:1.
Preferably, the temperature of step (1) described extraction is 20 ~ 100 DEG C, such as 20 DEG C, 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 43 DEG C, 45 DEG C, 48 DEG C, 50 DEG C, 53 DEG C, 55 DEG C, 58 DEG C, 60 DEG C, 63 DEG C, 65 DEG C, 68 DEG C, 70 DEG C, 73 DEG C, 75 DEG C, 78 DEG C, 80 DEG C, 83 DEG C, 85 DEG C, 88 DEG C, 90 DEG C, 93 DEG C, 95 DEG C, 98 DEG C or 100 DEG C, preferably 50 ~ 80 DEG C, preferably 70 DEG C further.
Preferably, the time of step (1) described extraction is 30 ~ 180min, such as 30min, 35min, 40min, 45min, 50min, 55min, 60min, 65min, 70min, 75min, 80min, 85min, 90min, 95min, 100min, 110min, 120min, 130min, 140min, 150min, 160min, 170min or 180min, preferably 60 ~ 120min, further preferred 90min.
Preferably, step (1) described extracting mode is that heated and stirred is extracted or ultrasound-enhanced extraction.
Preferably, the power of described ultrasound-enhanced extraction is 100 ~ 1000W, such as 200W, 300W, 400W, 500W, 600W, 700W, 800W or 900W, preferably 200 ~ 500W, further preferred 300W.
Preferably, step (2) described microfiltration membrane is any one in hollow fiber microfiltration membrane, spiral wound microfiltration membrane or ceramic microfiltration membrane, preferably ceramic microfiltration membrane.
Preferably, the aperture of step (2) described microfiltration membrane is 0.10 μm ~ 1.00 μm, such as 0.20 μm, 0.30 μm, 0.40 μm, 0.50 μm, 0.60 μm, 0.70 μm, 0.80 μm or 0.90 μm, more preferably, the aperture of step (2) described microfiltration membrane is 0.22 μm or 0.45 μm.
Preferably, step (3) described ultra-filtration membrane is hollow fiber ultrafiltration membrane or spiral wound ultra-filtration membrane, preferred spiral wound microfiltration membrane.
Preferably, the molecular weight cut-off of step (3) described ultra-filtration membrane is 1000Da ~ 10000Da, such as 1000Da, 1500Da, 2000Da, 3000Da, 4000Da, 5000Da, 6000Da, 7000Da, 8000Da, 9000Da or 10000Da, preferred 2000Da ~ 5000Da, further preferred 3000Da.
Preferably, the density of the described trapped fluid IV of step (3) is 1.00 ~ 1.10kg/L, such as 1.01kg/L, 1.02kg/L, 1.03kg/L, 1.04kg/L, 1.05kg/L, 1.06kg/L, 1.07kg/L, 1.08kg/L, 1.09kg/L or 1.10kg/L, preferably 1.01 ~ 1.05kg/L, further preferred 1.03kg/L.
Preferably, the trapped fluid IV of step (3) is concentrated, dry, obtain polysaccharide product.
Preferably, by the trapped fluid IV concentrating under reduced pressure of step (3), dry, obtain polysaccharide product.
Preferably, the temperature of described trapped fluid IV concentrating under reduced pressure is 40 ~ 90 DEG C, such as 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 or 90 DEG C, preferably 50 ~ 80 DEG C, preferably 70 DEG C further, concentrated vacuum tightness is 0.6 ~ 1.0MPa, such as 0.6MPa, 0.62MPa, 0.65MPa, 0.68MPa, 0.7MPa, 0.75MPa, 0.78MPa, 0.8MPa, 0.85MPa, 0.88MPa, 0.9MPa, 0.93MPa, 0.95MPa, 0.98MPa or 1.0MPa.
Preferably, step (4) described nanofiltration membrane is spiral wound nanofiltration membrane.
Preferably, the molecular weight cut-off of step (4) described nanofiltration membrane is 200Da.
Preferably, the density of the described trapped fluid VI of step (4) is 1.00 ~ 1.02kg/L, preferred 1.01kg/L.
Preferably, trapped fluid VI step (4) obtained concentrates, dry, obtains oligose product.
Preferably, trapped fluid VI concentrating under reduced pressure step (4) obtained, lyophilize, obtains oligose product.
Preferably, the temperature of described trapped fluid VI concentrating under reduced pressure is 40 ~ 90 DEG C, such as 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 or 90 DEG C, preferably 50 ~ 80 DEG C, preferably 70 DEG C further, concentrated vacuum tightness is 0.6 ~ 1.0MPa, such as 0.6MPa, 0.62MPa, 0.65MPa, 0.68MPa, 0.7MPa, 0.75MPa, 0.78MPa, 0.8MPa, 0.85MPa, 0.88MPa, 0.9MPa, 0.93MPa, 0.95MPa, 0.98MPa or 1.0MPa.
Preferably, the oligose obtained is kept in the middle of liquid.
Preferably, described liquid is dehydrated alcohol, mixture without any one in water glycol or anhydrous glycerol or at least two kinds, preferred dehydrated alcohol.
Extract the oligose obtained in natural product, very easily get damp after drying, therefore oligose can be kept at dehydrated alcohol, without water glycol, or in anhydrous glycerol equal solvent.
Preferably, the method for the invention also comprises the permeate VII that step (4) obtained and concentrates, and leaves standstill crystallization, or ethanolic soln heat of solution, cold analysis are brilliant, and prepare crude product N.F,USP MANNITOL, recrystallization obtains N.F,USP MANNITOL product.
Preferably, by permeate VII concentrating under reduced pressure that step (4) obtains.
Preferably, it is 1.05 ~ 1.30kg/L that the permeate VII that step (4) obtains is evaporated to density, such as 1.07kg/L, 1.09kg/L, 1.11kg/L, 1.13kg/L, 1.15kg/L, 1.17kg/L, 1.19kg/L, 1.20kg/L, 1.22kg/L, 1.23kg/L, 1.24kg/L, 1.25kg/L, 1.27kg/L or 1.29kg/L, preferably 1.15 ~ 1.25kg/L, further preferred 1.20kg/L.
Preferably, the time of described standing crystallization is 1 ~ 7 day, such as 1 day, 1.5 days, 2 days, 2.5 days, 3 days, 3.5 days, 4 days, 4.5 days, 5 days, 5.5 days, 6 days, 6.5 days or 7 days.
Preferably, the temperature of described standing crystallization is-5 DEG C ~ 25 DEG C, such as-5 DEG C ,-4 DEG C ,-2 DEG C, 0 DEG C, 5 DEG C, 10 DEG C, 15 DEG C, 20 DEG C, 22 DEG C, 24 DEG C or 25 DEG C, preferably 0 DEG C ~ 10 DEG C, preferably 5 DEG C further, after crystallization completely, and solid-liquid separation.
Preferably, in described ethanolic soln heat of solution, in cold Crystallization Process, in described heat of solution process, the concentration of ethanolic soln is 65 ~ 95%, such as 65%, 70%, 73%, 75%, 80%, 83%, 85%, 88%, 90% or 95%, the liquid-solid ratio of ethanolic soln and crude product N.F,USP MANNITOL is 10:1 ~ 50:1, such as 10:1, 12:1, 15:1, 18:1, 20:1, 23:1, 25:1, 28:1, 30:1, 35:1, 38:1, 40:1, 45:1, 48:1 or 50:1, heat of solution temperature is 40 ~ 80 DEG C, such as 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, cold recrystallization temperature is-5 DEG C ~ 5 DEG C, such as-5 DEG C,-4 DEG C,-3 DEG C,-2 DEG C,-1 DEG C, 0 DEG C, 1 DEG C, 2 DEG C, 3 DEG C, 4 DEG C or 5 DEG C.
Preferably, the crude product N.F,USP MANNITOL obtained is obtained N.F,USP MANNITOL product by ethyl alcohol recrystallization method purifying.
Described recrystallization method is: be dissolved in ethanolic soln by crude product N.F,USP MANNITOL, after dissolving completely, and decrease temperature crystalline, solid-liquid separation, and the crystal ethanolic soln obtained is washed, dry, namely obtain the N.F,USP MANNITOL of higher degree.The purity of the N.F,USP MANNITOL product obtained through recrystallization can reach more than 95%.
Relative to prior art, the present invention has following beneficial effect:
First, the method for the invention can prepare 3 kinds of Herba Cistanches main productss simultaneously: the polysaccharide that what the method for the invention was simple and quick be separated in Herba Cistanches, and oligose, produces highly purified N.F,USP MANNITOL crystal (purity can reach more than 95%); Oligose store method of the present invention, make use of oligose at dehydrated alcohol, extremely low and three kinds of liquid all have certain absorptive principle without solubleness in water glycol and anhydrous glycerol, solve in natural product and be separated the oligose obtained and very easily get damp the agglomerating problem of caking, be separated in natural product in the oligose storage and transport obtained and have great importance.
The present invention prepares in the process of 3 kinds of products, and equipment is simple, and less investment, in process of producing product, only uses water, and production cost is extremely low; Products production and storage in, do not use any poisonous and hazardous reagent, therefore product safety.
Accompanying drawing explanation
Fig. 1 is the present invention prepares N.F,USP MANNITOL, oligose and polysaccharide from Herba Cistanches simultaneously process flow sheet with membrane separation process.
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
Get Desert Herba Cistanches 1kg, pulverized 40 mesh sieves, add the purified water of 10L, extract 60min at 70 DEG C, extract 3 times, extracting solution 500 order filter-cloth filtering, merging filtrate obtains 25L clear liquid I.The ceramic micro filter membrane filtration gained clear liquid of 1.00 micron pore size, obtain permeate III, permeate III interception is 3000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.10kg/L filtering, obtain 30L permeate V and 3L trapped fluid IV.Trapped fluid temperature be 70 DEG C, vacuum tightness be 0.6MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 70 DEG C, dry vacuum tightness 0.7MPa, time of drying, 24h, obtained wheat-based diet 120g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.40L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 70 DEG C, vacuum tightness be 0.6MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 30g.Gained Herba Cistanches oligose preserved by dehydrated alcohol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.20kg/L, 5 days are left standstill at 5 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 12g, crude product N.F,USP MANNITOL solid is dissolved in 75% ethanolic soln of 200mL, dissolve at 50 DEG C, 5 DEG C of crystallizatioies, the heat of solution of crude product N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 9g.
Embodiment 2
Get Desert Herba Cistanches 1kg, pulverized 60 mesh sieves, add the purified water of 40L, extract 180min at 20 DEG C, extract 1 time, extracting solution 500 order filter-cloth filtering, merges to obtain 35L clear liquid I.The spiral wound membrane filtration gained clear liquid of 0.45 micron pore size, obtain permeate III, permeate III interception is that 5000Da hollow fiber ultrafiltration membrane is filtered, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.05kg/L filtering, obtain 40L permeate V and 5L trapped fluid IV.Trapped fluid temperature be 50 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 80 DEG C, dry vacuum tightness 1.0MPa, time of drying, 24h, obtained wheat-based diet 110g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.01kg/L.45L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 90 DEG C, vacuum tightness be 0.6MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 25g.Gained Herba Cistanches oligose preserved by dehydrated alcohol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.15kg/L, leaves standstill 5 days at-5 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 10g, crude product N.F,USP MANNITOL solid is dissolved in 95% ethanolic soln of 500mL, dissolve at 80 DEG C, 5 DEG C of crystallizatioies, prepare N.F,USP MANNITOL product 9g.
Embodiment 3
Get Desert Herba Cistanches 1kg, pulverized 40 mesh sieves, add the purified water of 8L, extract 60min at 100 DEG C, extract 3 times, extracting solution 500 order filter-cloth filtering, merges to obtain 20L clear liquid I.The spiral wound micro-filtrate membrane filtration gained clear liquid of 0.22 micron pore size, obtain permeate III, permeate III interception is 10000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.03kg/L filtering, obtain 30L permeate V and 2.5L trapped fluid IV.Trapped fluid temperature be 50 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 70 DEG C, dry vacuum tightness 0.7MPa, time of drying, 24h, obtained wheat-based diet 100g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.35L permeate VII and 4L trapped fluid VI, trapped fluid temperature be 80 DEG C, vacuum tightness be 0.8MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 30g.Gained Herba Cistanches oligose is preserved without water glycol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.05kg/L, leaves standstill 7 days at-5 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 12g, crude product N.F,USP MANNITOL solid is dissolved in 65% ethanolic soln of 120mL, dissolve at 40 DEG C ,-5 DEG C of crystallizatioies, prepare N.F,USP MANNITOL product 10g.
Embodiment 4
Get Desert Herba Cistanches 1kg, pulverized 10 mesh sieves, add the purified water of 20L, extract 120min at 50 DEG C, extract 2 times, extracting solution 500 order filter-cloth filtering, merges to obtain 35L clear liquid I.The spiral wound micro-filtrate membrane filtration gained clear liquid of 0.10 micron pore size, obtain permeate III, permeate III interception is 2000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.01kg/L filtering, obtain 40L permeate V and 5L trapped fluid IV.Trapped fluid temperature be 60 DEG C, vacuum tightness be 0.9MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 70 DEG C, dry vacuum tightness 0.9MPa, time of drying, 24h, obtained wheat-based diet 90g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.00kg/L.45L permeate VII and 6L trapped fluid VI, trapped fluid temperature be 50 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 10g.Gained Herba Cistanches oligose is preserved without water glycol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.25kg/L, leaves standstill 1 day at 0 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 9g, crude product N.F,USP MANNITOL solid is dissolved in 80% ethanolic soln of 300mL, dissolve at 65 DEG C ,-5 DEG C of crystallizatioies, prepare N.F,USP MANNITOL product 6g.
Embodiment 5
Get Desert Herba Cistanches 1kg, pulverized 40 mesh sieves, add the purified water of 15L, extract 90min at 50 DEG C, extract 3 times, extracting solution 500 order filter-cloth filtering, merges to obtain 40L clear liquid I.The hollow fiber microfiltration membrane of 0.45 micron pore size filters gained clear liquid, obtain permeate III, permeate III interception is 1000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.10kg/L filtering, obtain 45L permeate V and 3L trapped fluid IV.Trapped fluid temperature be 90 DEG C, vacuum tightness be 0.6MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 70 DEG C, dry vacuum tightness 0.9MPa, time of drying, 24h, obtained wheat-based diet 130g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.01kg/L.50L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 60 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 20g.Gained Herba Cistanches oligose preserved by dehydrated alcohol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.05kg/L, 7 days are left standstill at-5 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 8g, crude product N.F,USP MANNITOL solid is dissolved in 95% ethanolic soln of 100mL, dissolve at 80 DEG C, 5 DEG C of crystallizatioies, the heat of solution of crude product N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 5g.
Embodiment 6
Get Desert Herba Cistanches 1kg, pulverized 40 mesh sieves, add the purified water of 20L, extract 30min at 80 DEG C, extract 2 times, extracting solution 500 order filter-cloth filtering, merges to obtain 35L clear liquid I.The ceramic micro filter membrane filtration gained clear liquid of 0.45 micron pore size, obtain permeate III, permeate III interception is 5000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.01kg/L filtering, obtain 35L permeate V and 6L trapped fluid IV.Trapped fluid temperature be 70 DEG C, vacuum tightness be 0.9MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 70 DEG C, dry vacuum tightness 1.0MPa, time of drying, 24h, obtained wheat-based diet 120g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.50L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 80 DEG C, vacuum tightness be 0.9MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 30g.Gained Herba Cistanches oligose preserved by dehydrated alcohol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.25kg/L, 5 days are left standstill at 25 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 14g, crude product N.F,USP MANNITOL solid is dissolved in 75% ethanolic soln of 200mL, dissolve at 70 DEG C, 5 DEG C of crystallizatioies, the heat of solution of crude product N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 9g.
Embodiment 7
Get Desert Herba Cistanches 1kg, pulverized 60 mesh sieves, add the purified water of 15L, extract 30min at 70 DEG C, extract 3 times, extracting solution 500 order filter-cloth filtering, merges to obtain 40L clear liquid I.The ceramic micro filter membrane filtration gained clear liquid of 0.22 micron pore size, obtain permeate III, permeate III interception is 2000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.10kg/L filtering, obtain 50L permeate V and 3L trapped fluid IV.Trapped fluid temperature be 70 DEG C, vacuum tightness be 0.9MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 60 DEG C, dry vacuum tightness 1.0MPa, time of drying, 24h, obtained wheat-based diet 115g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.55L permeate VII and 4L trapped fluid VI, trapped fluid temperature be 70 DEG C, vacuum tightness be 0.9MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 30g.Gained Herba Cistanches oligose preserved by dehydrated alcohol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.30kg/L, 5 days are left standstill at 10 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 11g, crude product N.F,USP MANNITOL solid is dissolved in 80% ethanolic soln of 300mL, dissolve at 70 DEG C, 0 DEG C of crystallization, the heat of solution of crude product N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 8g.
Embodiment 8
Get Desert Herba Cistanches 1kg, pulverized 10 mesh sieves, add the purified water of 10L, ultrasonic at 50 DEG C (ultrasonic power 300W) assisted extraction 30min, extracts 3 times, and extracting solution 500 order filter-cloth filtering, merges to obtain 25L clear liquid I.The spiral wound micro-filtrate membrane filtration gained clear liquid of 0.45 micron pore size, obtain permeate III, permeate III interception is 1000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.00kg/L filtering, obtain 30L permeate V and 10L trapped fluid IV.Trapped fluid temperature be 60 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 70 DEG C, dry vacuum tightness 1.0MPa, time of drying, 24h, obtained wheat-based diet 130g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.40L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 70 DEG C, vacuum tightness be 0.6MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 25g.Anhydrous glycerol preserves gained Herba Cistanches oligose.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.15kg/L, 5 days are left standstill at 0 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 11g, crude product N.F,USP MANNITOL solid is dissolved in 75% ethanolic soln of 200mL, dissolve at 50 DEG C, 5 DEG C of crystallizatioies, the heat of solution of crude product N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 9g
Embodiment 9
Get Desert Herba Cistanches 1kg, pulverized 20 mesh sieves, add the purified water of 10L, ultrasonic at 40 DEG C (ultrasonic power 1000W) assisted extraction 30min, extracts 3 times, and extracting solution 500 order filter-cloth filtering, merges to obtain 25L clear liquid I.The spiral wound micro-filtrate membrane filtration gained clear liquid of 0.45 micron pore size, obtain permeate III, permeate III interception is 3000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.03kg/L filtering, obtain 30L permeate V and 10L trapped fluid IV.Trapped fluid temperature be 40 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 40 DEG C, dry vacuum tightness 1.0MPa, time of drying, 24h, obtained wheat-based diet 120g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.40L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 40 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 25g.Anhydrous glycerol preserves gained Herba Cistanches oligose.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.15kg/L, 5 days are left standstill at-5 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 12g, crude product N.F,USP MANNITOL solid is dissolved in 85% ethanolic soln of 400mL, dissolve at 70 DEG C, 0 DEG C of crystallization, the heat of solution of crude product N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 9g.
Embodiment 10
Get Desert Herba Cistanches 1kg, pulverized 40 mesh sieves, add the purified water of 15L, ultrasonic at 40 DEG C (ultrasonic power 100W) assisted extraction 30min, extracts 3 times, and extracting solution 500 order filter-cloth filtering, merges to obtain 40L clear liquid I.The spiral wound micro-filtrate membrane filtration gained clear liquid of 0.45 micron pore size, obtain permeate III, permeate III interception is 2000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.01kg/L filtering, obtain 50L permeate V and 10L trapped fluid IV.Trapped fluid temperature be 70 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 70 DEG C, dry vacuum tightness 1.0MPa, time of drying, 24h, obtained wheat-based diet 100g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.55L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 70 DEG C, vacuum tightness be 0.9MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 20g.Gained Herba Cistanches oligose preserved by dehydrated alcohol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.15kg/L, 6 days are left standstill at 0 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 12g, crude product N.F,USP MANNITOL solid is dissolved in 85% ethanolic soln of 400mL, dissolve at 70 DEG C, 0 DEG C of crystallization, the heat of solution of crude product N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 10g.
Embodiment 11
Get Desert Herba Cistanches 1kg, pulverized 40 mesh sieves, add the purified water of 20L, ultrasonic at 40 DEG C (ultrasonic power 200W) assisted extraction 30min, extracts 2 times, and extracting solution 500 order filter-cloth filtering, merges to obtain 35L clear liquid I.The spiral wound micro-filtrate membrane filtration gained clear liquid of 0.45 micron pore size, obtain permeate III, permeate III interception is 3000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.01kg/L filtering, obtain 40L permeate V and 10L trapped fluid IV.Trapped fluid temperature be 60 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 60 DEG C, dry vacuum tightness 1.0MPa, time of drying, 24h, obtained wheat-based diet 120g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.45L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 70 DEG C, vacuum tightness be 0.9MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 15g.Gained Herba Cistanches oligose preserved by dehydrated alcohol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.05kg/L, 6 days are left standstill at-5 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 13g, crude product N.F,USP MANNITOL solid is dissolved in 75% ethanolic soln of 300mL, dissolve at 70 DEG C, 0 DEG C of crystallization, the heat of solution of crude product N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 9g.
Embodiment 12
Get Desert Herba Cistanches 1kg, pulverized 60 mesh sieves, add the purified water of 40L, ultrasonic at 40 DEG C (ultrasonic power 500W) assisted extraction 60min, extracts 1 time, and extracting solution 500 order filter-cloth filtering, merges to obtain 35L clear liquid I.The spiral wound micro-filtrate membrane filtration gained clear liquid of 0.45 micron pore size, obtain permeate III, permeate III interception is 3000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.02kg/L filtering, obtain 45L permeate V and 5L trapped fluid IV.Trapped fluid temperature be 60 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 60 DEG C, dry vacuum tightness 1.0MPa, time of drying, 24h, obtained wheat-based diet 110g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.50L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 60 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 25g.Gained Herba Cistanches oligose preserved by dehydrated alcohol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.10kg/L, 7 days are left standstill at 0 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 13g, crude product N.F,USP MANNITOL solid is dissolved in 75% ethanolic soln of 300mL, dissolve at 70 DEG C, 0 DEG C of crystallization, the heat of solution of low-purity N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 8g.
Embodiment 13
Get Cistanche Tubulosa 1kg, pulverized 20 mesh sieves, add the purified water of 15L, extract 60min at 70 DEG C, extract 3 times, extracting solution 500 order filter-cloth filtering, merges to obtain 40L clear liquid I.The ceramic micro filter membrane filtration gained clear liquid of 0.45 micron pore size, obtain permeate III, permeate III interception is 5000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.10kg/L filtering, obtain 45L permeate V and 3L trapped fluid IV.Trapped fluid temperature be 60 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 60 DEG C, dry vacuum tightness 1.0MPa, time of drying, 24h, obtained wheat-based diet 120g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.50L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 70 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 30g.Gained Herba Cistanches oligose preserved by dehydrated alcohol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.20kg/L, 7 days are left standstill at 10 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 10g, crude product N.F,USP MANNITOL solid is dissolved in 75% ethanolic soln of 200mL, dissolve at 50 DEG C, 5 DEG C of crystallizatioies, the heat of solution of crude product N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 6g.
Embodiment 14
Get and spend Herba Cistanches 1kg in vain, pulverized 40 mesh sieves, add the purified water of 20L, extract 90min at 60 DEG C, extract 2 times, extracting solution 500 order filter-cloth filtering, merges to obtain 35L clear liquid I.The ceramic micro filter membrane filtration gained clear liquid of 0.45 micron pore size, obtain permeate III, permeate III interception is 3000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.10kg/L filtering, obtain 45L permeate V and 3L trapped fluid IV.Trapped fluid temperature be 60 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 60 DEG C, dry vacuum tightness 1.0MPa, time of drying, 24h, obtained wheat-based diet 100g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.50L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 70 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 25g.Gained Herba Cistanches oligose preserved by dehydrated alcohol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.20kg/L, 7 days are left standstill at 10 DEG C, centrifugal, get solid, for the N.F,USP MANNITOL of crude product is about 10g, crude product N.F,USP MANNITOL solid is dissolved in 65% ethanolic soln of 100mL, dissolve at 50 DEG C ,-5 DEG C of crystallizatioies, the heat of solution of crude product N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 6g.
Embodiment 15
Get Herba Cistanches sinensis 1kg, pulverized 60 mesh sieves, add the purified water of 15L, extract 30min at 80 DEG C, extract 3 times, extracting solution 500 order filter-cloth filtering, merges to obtain 40L clear liquid I.The ceramic micro filter membrane filtration gained clear liquid of 0.45 micron pore size, obtain permeate III, permeate III interception is 5000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.05kg/L filtering, obtain 45L permeate V and 5L trapped fluid IV.Trapped fluid temperature be 60 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 60 DEG C, dry vacuum tightness 1.0MPa, time of drying, 24h, obtained wheat-based diet 90g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.50L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 70 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 20g.Gained Herba Cistanches oligose preserved by dehydrated alcohol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.15kg/L, 5 days are left standstill at 0 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 10g, crude product N.F,USP MANNITOL solid is dissolved in 95% ethanolic soln of 500mL, dissolve at 80 DEG C, 5 DEG C of crystallizatioies, the heat of solution of crude product N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 9g.
Embodiment 16
Get Desert Herba Cistanches and Cistanche Tubulosa mixture 1kg, pulverized 40 mesh sieves, and added the purified water of 15L, and extracted 40min at 80 DEG C, extract 3 times, extracting solution 500 order filter-cloth filtering, merges to obtain 40L clear liquid I.The ceramic micro filter membrane filtration gained clear liquid of 0.45 micron pore size, obtain permeate III, permeate III interception is 5000Da spiral wound ultrafiltration membrance filter, filtration terminates front trapped fluid pure water and constantly cleans, stop when trapped fluid density is 1.10kg/L filtering, obtain 45L permeate V and 2L trapped fluid IV.Trapped fluid temperature be 60 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum-drying at 60 DEG C, dry vacuum tightness 1.0MPa, time of drying, 24h, obtained wheat-based diet 90g.
Permeate V molecular weight cut-off is the spiral wound nanofiltration membrane of 200Da, and filtration terminates front trapped fluid pure water and constantly cleans, and stops filtering when trapped fluid density is 1.02kg/L.50L permeate VII and 5L trapped fluid VI, trapped fluid temperature be 70 DEG C, vacuum tightness be 1.0MPa condition under concentrating under reduced pressure, concentrated solution vacuum lyophilization, obtains Herba Cistanches oligosaccharides 30g.Gained Herba Cistanches oligose preserved by dehydrated alcohol.
Permeate VII concentrating under reduced pressure, being concentrated into density is 1.15kg/L, 5 days are left standstill at 0 DEG C, centrifugal, get solid, for crude product N.F,USP MANNITOL is about 9g, crude product N.F,USP MANNITOL solid is dissolved in 80% ethanolic soln of 300mL, dissolve at 70 DEG C, 0 DEG C of crystallization, the heat of solution of crude product N.F,USP MANNITOL ethanol, cold analysis crystal method recrystallization prepare N.F,USP MANNITOL product 7g.
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. from Herba Cistanches, be separated the method preparing polysaccharide, oligose and N.F,USP MANNITOL, it is characterized in that, said method comprising the steps of:
(1) get the fleshy stem of Herba Cistanches, pulverize, then add Aqua pure extract and carry out solid-liquid separation, obtaining clear liquid I and residual II;
(2) micro-filtrate membrane filtration clear liquid I, obtains permeate III;
(3) ultrafiltration membrance filter permeate III, obtains permeate V and the trapped fluid IV containing polysaccharide product;
(4) nanofiltration membrane permeate V, obtains the trapped fluid VI containing oligose product and the permeate VII containing N.F,USP MANNITOL product.
2. method according to claim 1, is characterized in that, described Herba Cistanches is Desert Herba Cistanches, the combination of Cistanche Tubulosa, any one or at least two kinds spent in vain in the fleshy stem of Herba Cistanches or Herba Cistanches sinensis.
3. method according to claim 1 and 2, is characterized in that, clear liquid for adding Aqua pure extract 1 ~ 3 time, then solid-liquid separation, and merges by step (1), obtains clear liquid I and residual II;
Preferably, in step (1), Herba Cistanches degree of grinding is 10 ~ 60 orders, and more preferably, Herba Cistanches degree of grinding is 20 ~ 40 orders;
Preferably, in step (1), the liquid-solid ratio of pure water and Herba Cistanches is 8:1 ~ 40:1, preferred 10:1 ~ 20:1, further preferred 15:1.
4. the method according to any one of claim 1-3, is characterized in that, the temperature of step (1) described extraction is 20 ~ 100 DEG C, preferably 50 ~ 80 DEG C, preferably 70 DEG C further;
Preferably, the time of step (1) described extraction is 30 ~ 180min, preferably 60 ~ 120min, further preferred 90min;
Preferably, step (1) described extracting mode is that heated and stirred is extracted or ultrasound-enhanced extraction;
Preferably, the power of described ultrasound-enhanced extraction is 100 ~ 1000W, preferably 200 ~ 500W, further preferred 300W.
5. the method according to any one of claim 1-4, is characterized in that, step (2) described microfiltration membrane is any one in hollow fiber microfiltration membrane, spiral wound microfiltration membrane or ceramic microfiltration membrane, preferably ceramic microfiltration membrane;
Preferably, the aperture of step (2) described microfiltration membrane is 0.10 μm ~ 1.00 μm, and more preferably, the aperture of step (2) described microfiltration membrane is 0.22 μm or 0.45 μm.
6. the method according to any one of claim 1-5, is characterized in that, step (3) described ultra-filtration membrane is hollow fiber ultrafiltration membrane or spiral wound ultra-filtration membrane, preferred spiral wound microfiltration membrane;
Preferably, the molecular weight cut-off of step (3) described ultra-filtration membrane is 1000Da ~ 10000Da, preferred 2000Da ~ 5000Da, further preferred 3000Da;
Preferably, the density of the described trapped fluid IV of step (3) is 1.00 ~ 1.10kg/L, preferably 1.01 ~ 1.05kg/L, further preferred 1.03kg/L;
Preferably, the trapped fluid IV of step (3) is concentrated, dry, obtain polysaccharide product;
Preferably, by the trapped fluid IV concentrating under reduced pressure of step (3), dry, obtain polysaccharide product;
Preferably, the temperature of described trapped fluid IV concentrating under reduced pressure is 40 ~ 90 DEG C, preferably 50 ~ 80 DEG C, and preferably 70 DEG C further, concentrated vacuum tightness is 0.6 ~ 1.0MPa.
7. the method according to any one of claim 1-6, is characterized in that, step (4) described nanofiltration membrane is spiral wound nanofiltration membrane;
Preferably, the molecular weight cut-off of step (4) described nanofiltration membrane is 200Da;
Preferably, the density of the described trapped fluid VI of step (4) is 1.00 ~ 1.02kg/L, preferred 1.01kg/L;
Preferably, trapped fluid VI step (4) obtained concentrates, dry, obtains oligose product;
Preferably, the trapped fluid VI concentrating under reduced pressure that step (4) is obtained, lyophilize, obtains oligose product;
Preferably, the temperature of described trapped fluid VI concentrating under reduced pressure is 40 ~ 90 DEG C, preferably 50 ~ 80 DEG C, and preferably 70 DEG C further, concentrated vacuum tightness is 0.6 ~ 1.0MPa.
Preferably, the oligose product obtained is kept in the middle of liquid;
Preferably, described liquid is dehydrated alcohol, mixture without any one in water glycol or anhydrous glycerol or at least two kinds, preferred dehydrated alcohol.
8. the method according to any one of claim 1-7, is characterized in that, described method also comprises permeate VII step (4) obtained and concentrates, leave standstill crystallization, or ethanolic soln heat of solution, cold analysis crystalline substance, prepare crude product N.F,USP MANNITOL, recrystallization obtains N.F,USP MANNITOL product;
Preferably, by permeate VII concentrating under reduced pressure that step (4) obtains;
Preferably, it is 1.05 ~ 1.30kg/L, preferably 1.15 ~ 1.25kg/L that the permeate VII that step (4) obtains is evaporated to density, further preferred 1.20kg/L.
9. the method according to any one of claim 1-8, is characterized in that, the time of described standing crystallization is 1 ~ 7 day;
Preferably, the temperature of described standing crystallization is-5 DEG C ~ 25 DEG C, preferably 0 DEG C ~ 10 DEG C, preferably 5 DEG C further, after crystallization completely, and solid-liquid separation.
10. the method according to any one of claim 1-9, it is characterized in that, described ethanolic soln heat of solution, in cold Crystallization Process, in described heat of solution process, the concentration of ethanolic soln is 65 ~ 95%, the liquid-solid ratio of ethanolic soln and crude product N.F,USP MANNITOL is 10:1 ~ 50:1, and heat of solution temperature is 40 ~ 80 DEG C, and cold recrystallization temperature is-5 DEG C ~ 5 DEG C;
Preferably, the crude product N.F,USP MANNITOL obtained is obtained N.F,USP MANNITOL product by ethyl alcohol recrystallization method purifying.
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| CN105294398A (en) * | 2015-09-29 | 2016-02-03 | 上海市农业科学院 | Method for preparing high-purity mannitol |
| CN105385653A (en) * | 2015-10-29 | 2016-03-09 | 甘肃中医药大学 | Application of cistanche extract in mesenchymal stem cells |
| CN106963818A (en) * | 2017-03-17 | 2017-07-21 | 广州康琪莱生物科技有限公司 | A kind of Desert Herba Cistanches extract and its quick preparation technology |
| CN107281015A (en) * | 2016-04-09 | 2017-10-24 | 和田帝辰医药生物科技有限公司 | The anti-aging whitening topical agent and preparation method of a kind of Cistanche tubulosa extract |
| CN109043321A (en) * | 2018-08-18 | 2018-12-21 | 安徽国科生物科技有限公司 | A kind of dietary composition of relax bowel and defecation and preparation method thereof |
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| CN109320400A (en) * | 2018-09-30 | 2019-02-12 | 湖南华诚生物资源股份有限公司 | A method of natural mannitol is extracted from mogroside production waste liquid |
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