CN103319546A - Method for separating high-purity stachyose from rehmannia - Google Patents
Method for separating high-purity stachyose from rehmannia Download PDFInfo
- Publication number
- CN103319546A CN103319546A CN2013102413131A CN201310241313A CN103319546A CN 103319546 A CN103319546 A CN 103319546A CN 2013102413131 A CN2013102413131 A CN 2013102413131A CN 201310241313 A CN201310241313 A CN 201310241313A CN 103319546 A CN103319546 A CN 103319546A
- Authority
- CN
- China
- Prior art keywords
- water
- separation
- stachyose
- behind
- rehmannia
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for separating high-purity stachyose from rehmannia, belonging to the technical field of natural product extraction and separation. The method comprises the following steps of: 1) sufficiently and uniformly mixing a fresh rehmannia crude extract with water so as to obtain a loading solution; 2) filling aminopropyl bonded silica gel into a high-pressure preparative liquid chromatographic column, subsequently loading the loading solution on the high-pressure preparative liquid chromatographic column, and eluting by using an acetonitrile-water system as the eluant; and 3) carrying out sectional collection under the detection of a differential detector so as to obtain a stachyose liquid, and concentrating and drying the stachyose liquid under reduced pressure at low temperature so as to obtain the high-purity stachyose. By utilizing the method, stachyose can be obtained through direct and rapid separation, the separation time is short, the separation quantity is large, the yield can be greater than 85%, the purity is as high as greater than 98%, less waste materials are produced, the column efficiency is high, a small size of eluant is needed, a small space is occupied, the cost consumption of the whole process is reduced, the filler and the solvent can be recycled, and the method is environmental-friendly and applicable to industrial production.
Description
Technical field
The invention belongs to the natural product extraction separation technology field, be specifically related to a kind of from glutinous rehmannia the method for separation and Extraction stachyose.
Background technology
Stachyose is a kind of good functional food ingredients as a kind of emerging functional four poly oligosaccharides, has the effect that improves body health, and these functional four poly oligosaccharides have the regulating intestinal canal flora, improve lipid metabolism.Improve the effect of body immunity, this oligosaccharide has hypoglycemic, reducing blood-fat, the effect of increase insulin sensitivity simultaneously.
At present, stachyose is mainly ion-exchange resin purification aspect separation and purification and enzyme process prepares stachyose, but make spent ion exchange resin and enzyme process prepare stachyose, preparation cycle is long and cost is higher, based on above reason development of new separation purifying technique, seek more economically, efficiently, separating and purifying technology efficiently, more and more become the focus that the investigator pays close attention to.
Summary of the invention
The object of the present invention is to provide a kind of from glutinous rehmannia the method for Separation of Water threose, the method is simple to operate, disengaging time is short, cost is low, the product purity that obtains is high, yield is high.
The present invention is achieved through the following technical solutions:
A kind of from glutinous rehmannia the method for Separation of Water threose, may further comprise the steps:
1) Rehmannia Root crude extract and water are pressed the solid-liquid ratio of 1g:3～7ml, fully behind the mixing, obtained sample solution;
2) with behind the aminopropyl bonded silica gel filling high pressure preparative liquid chromatography post, sample solution is splined on high pressure preparative liquid chromatography post, take the acetonitrile-water system as elutriant, with speed isorheic elution 30～40min of 10～200ml/min, the volume ratio of acetonitrile and water is (68～73) in the described elutriant: (27～32);
3) under detecting, the differential detector carries out Fractional Collections according to the chromatogram appearance time, when the corresponding peak of stachyose begins to rise, collect, finish five of whole peak height/a period of time to collect when this peak drops to, obtain the wood liquid glucose, with dry behind the wood liquid glucose concentrating under reduced pressure, obtain high purity stachyose.
Step 2) described loading adopts the gradation loading, each loading 10～20ml.
Drying is after the wood liquid glucose is concentrated into relative density and is 1.10～1.15 behind the described concentrating under reduced pressure of step 3), under 20～40 ℃, and vacuum-drying 20～40h.
Described aminopropyl bonded silica gel passes through activation treatment before use, at first, small-particle ball-type aminopropyl bonded silica gel and ethanol are pressed the solid-liquid ratio of 1g:2～3ml, fully obtained homogenate behind the mixing, after homogenate supersound process 30～40min removed bubble, be packed in the chromatographic column; Secondly, after the water pump pumping liquid is till the Silica Surface absence of liquid, be forced into 45～50bar, use the high flow rate elutriant, with the flow velocity of 200ml/min, rinse out the interior ethanol of post; At last, with the flow velocity of 100ml/min, flushing 1h, the aminopropyl bonded silica gel after obtaining activating.
Described pressurization is to adopt piston to carry out the substep pressurization, and the first step is pressurized to 15～20bar, then with behind the high flow rate elutriant flushing pillar 1h, is pressurized to 45～50bar again.
The described high flow rate elutriant elutriant that to be acetonitrile and water be made into by the volume ratio of 70:30.
The particle diameter of described small-particle ball-type aminopropyl bonded silica gel is 5～20 μ m, and the aperture is
After described high pressure preparative liquid chromatography post post effect reduces, be that 5% ammonia soln carries out wash-out regeneration with mass concentration, regeneration is rear carries out wash-out with pure water, is eluted in the effluent liquid without ammonium ion.
The internal temperature of described differential detector is made as 30 ℃, and outside temperature is made as 35 ℃.
Described Rehmannia Root crude extract is after Rehmannia Root is cleaned, section, add flooding 1～4h after, under 80～100 ℃, heating and refluxing extraction 1～5h behind extracting liquid filtering, gets filtrate; Add in the filtrate after dehydrated alcohol to ethanol content reaches 90%, under 0～4 ℃, leave standstill 10～14h after, under 3000～4000r/min, centrifugal 25～35min gets precipitation; After precipitation was dissolved in water, behind activated carbon decolorizing, behind the destainer concentrating under reduced pressure, under 25～30 ℃, after vacuum tightness reached 0.09～0.15Mpa, vacuum-drying 20～40h obtained the Rehmannia Root crude extract.
Compared with prior art, the present invention has following useful technique effect:
The present invention separates first Application in the extraction of stachyose with the high pressure preparative chromatography, use the aminopropyl bonded silica gel as column packing, the success separation obtains high purity stachyose, only use this a kind of chromatogram system of acetonitrile and water in the sepn process, carry out constant current constant speed Gradient elution, adopt differential detector on-line monitoring method separated product and impurity, accomplish accurate collection, the sepn process simple and fast, flash liberation just can achieve the goal, without any need for chemical treatment method, can not lose stachyose, can be directly, separate fast and obtain stachyose, and disengaging time is short, fractional dose is large, and yield reaches more than 85%, and the stachyose purity that obtains is up to more than 98%.
The waste material that the inventive method produces is few, and the post effect is high, and required effluent volume is little, and floor space is little, has reduced the consuming cost of whole technique, filler and solvent recoverable, and environmental friendliness is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the HPLC color atlas of each composition in the Fractional Collections glutinous rehmannia crude extract of the present invention;
Fig. 2 is the HPLC mensuration chromatic graph spectrum that the present invention separates the stachyose that obtains.
Wherein, 1 is glucose, and 2 is fructose, and 3 is sucrose, and 4 is stachyose, and 5 is raffinose.
Embodiment
The present invention is described in further detail below in conjunction with concrete drawings and Examples, and the explanation of the invention is not limited.
The reagent that the present invention is used and laboratory apparatus
1, reagent: preparation is analytical pure with acetonitrile, ethanol, ammonia, and analyzing with acetonitrile is chromatographically pure, and water is the secondary redistilled water;
2, laboratory apparatus: the present invention has adopted the small-particle ball-type aminopropyl bonded silica gel filler of external import, can under high pressure use, the resolution of this aminopropyl bonded silica gel related impurities is near analysis mode HPLC, has simultaneously good Reusability ability, the major diameter preparative column is that imported from America (VARIAN) can be loaded high-pressure chromatographic column certainly, it is imported from America (VARIAN) that high pressure prepares liquid phase systems, preparation is imported from America (VARIAN) with differential refraction detector, automatically the fraction collection system is imported from America (VARIAN), and product analysis uses high performance liquid chromatograph to produce as the U.S. (Waters).
A kind of from glutinous rehmannia the method for Separation of Water threose, may further comprise the steps:
1) Rehmannia Root crude extract and water are pressed the solid-liquid ratio of 1g:3～7ml, fully behind the mixing, obtained sample;
2) with behind the aminopropyl bonded silica gel filling high pressure preparative liquid chromatography post, the sample gradation is splined on high pressure preparative liquid chromatography post, take the acetonitrile-water system as elutriant, with speed isorheic elution 20～40min of 10～200ml/min, the volume ratio of acetonitrile and water is (68～73) in the described elutriant: (27～32); Described gradation loading is each loading 10～20ml sample;
3) under the differential detector detects, carry out Fractional Collections, obtain the wood liquid glucose, will obtain high purity stachyose after the wood liquid glucose low-temperature reduced-pressure drying.
The Rehmannia Root crude extract that uses is after Rehmannia Root is cleaned, section, after adding flooding 1～4h, under 80～100 ℃, heating and refluxing extraction 1～5h collects extracting solution again, after the extracting solution filtered while hot, add dehydrated alcohol in the filtrate and shake up after contain the alcohol amount and reach 90%, low temperature was placed 10～14 hours, after taking out under 3000～4000r/min, centrifugal 25～35min, abandoning supernatant, throw out uses activated carbon decolorizing with water dissolution, behind the destainer concentrating under reduced pressure, under 20～40 ℃, when vacuum tightness reached 0.09～0.15Mpa, vacuum-drying 20～40h obtained the glutinous rehmannia crude extract.
Before the purified water threose, need to carry out chromatographic column loads, take by weighing an amount of aminopropyl bonded silica gel filler, press the solid-liquid ratio of 1g:2～3ml, adding is made homogenate with the abundant mixing of ethanol, after homogenate supersound process 30～50min removed bubble, pour in the gc column tube,, cover behind the flange and carry out the substep pressurization with piston until Silica Surface does not just have liquid with the vacuum pump pumping liquid, be pressurized to 15～20bar for the first time, then behind the elutriant flushing pillar 1h with high flow rate, be pressurized to again 45～50bar, continue with the activation of elutriant flushing pillar constant speed, stand-by; For obtaining best separating effect, it highly is about 25cm that pillar is loaded.
The Rehmannia Root crude extract is dissolved in the water, and the ratio of dissolving is about 1:3～7, then filters with filtering membrane, and the sample batch sampling high pressure preparative liquid chromatography system that dissolving is good carries out the constant speed Gradient elution, and elution time is 20～40min; Elutriant is comprised of acetonitrile and water two portions, and the Polarity Control of elutriant is between 10～20min at stachyose in the retention time in the high pressure chromatogram, and the flow velocity of whole preparation process remains between 10～200ml/min.
Product carries out Fractional Collections (30 ℃ of internal temperatures, 35 ℃ of outside temperatures) according to the chromatographic peak appearance time under the differential detector detects.In the chromatographic separation of the present invention, glucose, sucrose, fructose are in the leading portion of stachyose, and the peak type is relatively symmetrical, but the peak do not reach in baseline separation so the sepn process when beginning to rise at the peak and collect, and the peak drops to whole high five/for the moment to be finished to collect.
The stachyose elutriant of collecting in the chromatographic separation process, be concentrated into relative density 1.10～1.15(60 ℃ survey by Rotary Evaporators) time use vacuum-drying, under 20～40 ℃, vacuum tightness is under 0.09～0.15Mpa, vacuum-drying 20～40h, the powder that drying obtains, by high performance liquid chromatography quantitative analysis purity more than 98%.
Through chromatographic separation repeatedly, the separator column effect of high pressure preparative liquid chromatography post reduces, this moment, available quality concentration was that 5% ammonia soln carries out the counterflush preparative column, column flow rate is 10～20% of chromatographic separation flow velocity, then use pure water to wash away ammonia unnecessary on the chromatographic column, recover chromatographic column post effect.
Embodiment 1
A kind of from glutinous rehmannia the method for Separation of Water threose, may further comprise the steps:
1) in the open glass container of 5L, the ball-type aminopropyl bonded silica gel that adds the 10 μ m of 700g, add and analyze ethanol 2100mL, stir into homogenate, behind the ultrasonic 40min, pour ready diameter 5cm into, column length is that extracting liquid covers flange in the stainless steel chromatogram column jecket of 30cm, the elutriant that is made into by the volume ratio of 70:30 with acetonitrile and water, flow velocity with 200ml/min carries out wash-out, rinses out ethanol in the chromatographic column, carries out the substep pressurization with piston in the post, the first step is pressurized to 15bar, then behind the flow velocity flushing 1h with 100ml/min, be forced into again 50bar, activation;
2) after chromatographic column is ready to complete, taking by weighing Rehmannia Root crude extract 100g(stachyose content is 38.9%), be dissolved in the 500ml water, filter, high pressure prepares flow rate pump 50ml/min, sample introduction 10ml, take the volume ratio 68:32 of acetonitrile and water as elutriant, carry out the constant speed wash-out, (30 ℃ of internal temperatures, 35 ℃ of outside temperatures) detects whole elution process under the differential detector, observe chromatographic peak by software, referring to Fig. 1, rise at 15.8min stachyose product peak, collect by automatic fraction collector, collection time is that the stachyose peak began ascent stage 15.87 minutes, the stachyose peak whole peak height 1/5th that descends finishes to collect, and finishes this elution system behind the 30min, and 1 is glucose in the collection of illustrative plates, 2 is fructose, 3 is sucrose, and 4 is stachyose, and 5 is raffinose; Carry out the repetition sample introduction after this wash-out finishes and collect, until that the Rehmannia Root of preparation is slightly extracted sample feeding is complete;
3) collect liquid and in Rotary Evaporators, reclaim solvent, to relative density 1.10(60 ℃ survey), (vacuum tightness is 0.09～0.15Mpa to use vacuum-drying, temperature is not higher than 30 ℃) dry 20～40h, obtain dried powder 32.6g, by the high performance liquid chromatography quantitative analysis, referring to Fig. 2, stachyose content is 98.6%, and yield is 87.4%.
A kind of from glutinous rehmannia the method for Separation of Water threose, may further comprise the steps:
1) in the open glass container of 5L, the ball-type aminopropyl bonded silica gel that adds the 5 μ m of 200g, add and analyze ethanol 600mL, stir into homogenate, behind the ultrasonic 30min, pour ready diameter 1.5cm into, column length is that extracting liquid covers flange in the stainless steel chromatogram column jecket of 20cm, the elutriant that is made into by the volume ratio of 70:30 with acetonitrile and water, flow velocity with 200ml/min carries out wash-out, rinses out ethanol in the chromatographic column, carries out the substep pressurization with piston in the post, the first step is pressurized to 15bar, then behind the flow velocity flushing 1h with 100ml/min, be forced into again 45bar, activation;
2) after chromatographic column is ready to complete, taking by weighing Rehmannia Root crude extract 150g(stachyose content is 38.9%), be dissolved in the 900ml water, filter, high pressure prepares flow rate pump 100ml/min, sample introduction 20ml, take the volume ratio 70:30 of acetonitrile and water as elutriant, carry out the constant speed wash-out, (30 ℃ of internal temperatures under the differential detector, 35 ℃ of outside temperatures) detect whole elution process, observe chromatographic peak by software, rise at 14.6min stachyose product peak, collect by automatic fraction collector, collection time is that the stachyose peak began ascent stage 14.67 minutes, and the peak whole peak height 1/5th that descends finishes to collect.Finish this elution system behind the 40min, carrying out the repetition sample introduction collects, until the Rehmannia Root of preparation slightly to extract sample feeding complete, collect liquid and in Rotary Evaporators, reclaim solvent, to relative density 1.10(60 ℃ survey), (vacuum tightness is 0.09～0.15Mpa) under 25～30 ℃ to use vacuum-drying, dry 20～40h obtains dried powder 52.3g, by the high performance liquid chromatography quantitative analysis, stachyose content is 98.9%, and yield is 88.6%.
Embodiment 3
A kind of from glutinous rehmannia the method for Separation of Water threose, may further comprise the steps:
1) in the open glass container of 5L, the ball-type aminopropyl bonded silica gel that adds the 20 μ m of 700g, add and analyze ethanol 1800mL, stir into homogenate, behind the ultrasonic 35min, pour ready diameter 15cm into, column length is that extracting liquid covers flange in the stainless steel chromatogram column jecket of 35cm, the elutriant that is made into by the volume ratio of 70:30 with acetonitrile and water, flow velocity with 200ml/min carries out wash-out, rinses out ethanol in the chromatographic column, carries out the substep pressurization with piston in the post, the first step is pressurized to 15bar, then behind the flow velocity flushing 1h with 100ml/min, be forced into again 45bar, activation;
2) after chromatographic column is ready to complete, taking by weighing Rehmannia Root crude extract 100g(stachyose content is 38.9%), be dissolved in the 700ml water, filter, high pressure prepares flow rate pump 200ml/min, sample introduction 15ml, take the volume ratio 73:27 of acetonitrile and water as elutriant, carry out the constant speed wash-out, (30 ℃ of internal temperatures under the differential detector, 35 ℃ of outside temperatures) detect whole elution process, observe chromatographic peak by software, rise at 14.5min stachyose product peak, collect by automatic fraction collector, collection time is that the stachyose peak began ascent stage 14.56 minutes, and the peak whole peak height 1/5th that descends finishes to collect.Finish this elution system behind the 40min, carrying out the repetition sample introduction collects, until the Rehmannia Root of preparation slightly to extract sample feeding complete, collect liquid and in Rotary Evaporators, reclaim solvent, to relative density 1.15(60 ℃ survey), (vacuum tightness is 0.09～0.15Mpa) under 25～30 ℃ to use vacuum-drying, dry 20～40h obtains dried powder 47.9g, by the high performance liquid chromatography quantitative analysis, stachyose content is 98.3%, and yield is 87.9%.
A kind of from glutinous rehmannia the method for Separation of Water threose, may further comprise the steps:
1) in the open glass container of 5L, the ball-type aminopropyl bonded silica gel that adds the 10 μ m of 700g, add and analyze ethanol 1400mL, stir into homogenate, behind the ultrasonic 35min, pour ready diameter 8cm into, column length is that extracting liquid covers flange in the stainless steel chromatogram column jecket of 40cm, the elutriant that is made into by the volume ratio of 70:30 with acetonitrile and water, flow velocity with 200ml/min carries out wash-out, rinses out ethanol in the chromatographic column, carries out the substep pressurization with piston in the post, the first step is pressurized to 15bar, then behind the flow velocity flushing 1h with 100ml/min, be forced into again 45bar, activation;
2) after chromatographic column is ready to complete, taking by weighing Rehmannia Root crude extract 100g(stachyose content is 38.9%), be dissolved in the 300ml water, filter, high pressure prepares flow rate pump 10ml/min, sample introduction 10ml, take the volume ratio 69:31 of acetonitrile and water as elutriant, carry out the constant speed wash-out, (30 ℃ of internal temperatures under the differential detector, 35 ℃ of outside temperatures) detect whole elution process, observe chromatographic peak by software, rise at 15.3min stachyose product peak, collect by automatic fraction collector, collection time is that the stachyose peak began ascent stage 15.38 minutes, and the peak whole peak height 1/5th that descends finishes to collect.Finish this elution system behind the 40min, carrying out the repetition sample introduction collects, until the Rehmannia Root of preparation slightly to extract sample feeding complete, collect liquid and in Rotary Evaporators, reclaim solvent, to relative density 1.12(60 ℃ survey), (vacuum tightness is 0.09～0.15Mpa) under 25～30 ℃ to use vacuum-drying, dry 20～40h obtains dried powder 44.2g, by the high performance liquid chromatography quantitative analysis, stachyose content is 98.3%, and yield is 87.2%.
To sum up, the method of high performance preparative liquid chromatography Separation of Water threose provided by the present invention, under differential detector on-line monitoring, carry out the accurate collection of separated product and impurity, the sepn process simple and fast, flash liberation just can achieve the goal, without any need for chemical treatment method, guaranteed that effectively stachyose can not lose, the sepn process time spent is short, and fractional dose is large, the yield of stachyose can reach more than 85%, and particularly purity can reach more than 98%.Present method running cost is low, and filler for a long time recirculation uses, and solvent is recyclable to be reused, and disengaging time is short, and fractional dose is large, is fit to suitability for industrialized production.
Claims (10)
1. the method for a Separation of Water threose from glutinous rehmannia is characterized in that, may further comprise the steps:
1) Rehmannia Root crude extract and water are pressed the solid-liquid ratio of 1g:3～7ml, fully behind the mixing, obtained sample solution;
2) with behind the aminopropyl bonded silica gel filling high pressure preparative liquid chromatography post, sample solution is splined on high pressure preparative liquid chromatography post, take the acetonitrile-water system as elutriant, with speed isorheic elution 30～40min of 10～200ml/min, the volume ratio of acetonitrile and water is (68～73) in the described elutriant: (27～32);
3) under detecting, the differential detector carries out Fractional Collections according to the chromatogram appearance time, when the corresponding peak of stachyose begins to rise, collect, finish five of whole peak height/a period of time to collect when this peak drops to, obtain the wood liquid glucose, with dry behind the wood liquid glucose concentrating under reduced pressure, obtain high purity stachyose.
According to claim 1 a kind of from glutinous rehmannia the method for Separation of Water threose, it is characterized in that step 2) described loading adopts the gradation loading, each loading 10～20ml.
According to claim 1 a kind of from glutinous rehmannia the method for Separation of Water threose, it is characterized in that, drying is after the wood liquid glucose is concentrated into relative density and is 1.10～1.15 behind the described concentrating under reduced pressure of step 3), under 20～40 ℃, vacuum-drying 20～40h.
According to claim 1 a kind of from glutinous rehmannia the method for Separation of Water threose, it is characterized in that, described aminopropyl bonded silica gel passes through activation treatment before use, at first, small-particle ball-type aminopropyl bonded silica gel and ethanol are pressed the solid-liquid ratio of 1g:2～3ml, fully obtain homogenate behind the mixing, homogenate supersound process 30～40min is removed bubble after, be packed in the chromatographic column; Secondly, after the water pump pumping liquid is till the Silica Surface absence of liquid, be forced into 45～50bar, use the high flow rate elutriant, with the flow velocity of 200ml/min, rinse out the interior ethanol of post; At last, with the flow velocity of 100ml/min, flushing 1h, the aminopropyl bonded silica gel after obtaining activating.
According to claim 4 a kind of from glutinous rehmannia the method for Separation of Water threose, it is characterized in that, described pressurization is to adopt piston to carry out the substep pressurization, and the first step is pressurized to 15～20bar, then with behind the high flow rate elutriant flushing pillar 1h, be pressurized to again 45～50bar.
According to claim 4 or 5 described a kind of from glutinous rehmannia the method for Separation of Water threose, it is characterized in that the described high flow rate elutriant elutriant that to be acetonitrile and water be made into by the volume ratio of 70:30.
According to claim 4 a kind of from glutinous rehmannia the method for Separation of Water threose, it is characterized in that, it is characterized in that, the particle diameter of described small-particle ball-type aminopropyl bonded silica gel is 5～20 μ m, the aperture is
According to claim 1 a kind of from glutinous rehmannia the method for Separation of Water threose, it is characterized in that, after described high pressure preparative liquid chromatography post post effect reduces, be that 5% ammonia soln carries out wash-out and regenerates with mass concentration, carry out wash-out with pure water after the regeneration, be eluted in the effluent liquid without ammonium ion.
According to claim 1 a kind of from glutinous rehmannia the method for Separation of Water threose, it is characterized in that, the internal temperature of described differential detector is made as 30 ℃, outside temperature is made as 35 ℃.
According to claim 1 a kind of from glutinous rehmannia the method for Separation of Water threose, it is characterized in that, described Rehmannia Root crude extract is after Rehmannia Root is cleaned, the section, add flooding 1～4h after, under 80～100 ℃, heating and refluxing extraction 1～5h behind extracting liquid filtering, gets filtrate; Add in the filtrate after dehydrated alcohol to ethanol content reaches 90%, under 0～4 ℃, leave standstill 10～14h after, under 3000～4000r/min, centrifugal 25～35min gets precipitation; After precipitation was dissolved in water, behind activated carbon decolorizing, behind the destainer concentrating under reduced pressure, under 25～30 ℃, after vacuum tightness reached 0.09～0.15Mpa, vacuum-drying 20～40h obtained the Rehmannia Root crude extract.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310241313.1A CN103319546B (en) | 2013-06-18 | 2013-06-18 | A kind of from glutinous rehmannia the method for Separation of Water threose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310241313.1A CN103319546B (en) | 2013-06-18 | 2013-06-18 | A kind of from glutinous rehmannia the method for Separation of Water threose |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103319546A true CN103319546A (en) | 2013-09-25 |
| CN103319546B CN103319546B (en) | 2016-05-04 |
Family
ID=49188632
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310241313.1A Active CN103319546B (en) | 2013-06-18 | 2013-06-18 | A kind of from glutinous rehmannia the method for Separation of Water threose |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103319546B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315314A (en) * | 2014-07-31 | 2016-02-10 | 中国食品发酵工业研究院 | Industrial production method for extracting stachyose from radix rehmanniae |
| CN112587959A (en) * | 2019-12-31 | 2021-04-02 | 杭州九源基因工程有限公司 | Method for regenerating chromatographic stationary phase in step of preparing acylated polypeptide |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0383992A (en) * | 1989-08-29 | 1991-04-09 | Ensuiko Sugar Refining Co Ltd | Production of high purity aldosylfructoside |
| CN1118215A (en) * | 1994-06-20 | 1996-03-13 | 李熙 | Rehmannia glutinosa extract and a safner composition having safner activity to a herbicide paraquat |
| JP3623974B2 (en) * | 1993-09-13 | 2005-02-23 | カルピス株式会社 | Oligosaccharide purification method |
| CN1715287A (en) * | 2004-07-01 | 2006-01-04 | 西安大鹏生物科技股份有限公司 | Method for extracting high purity stachyose from radix rehmanniae recen and producing prepared rehmannia root |
| CN101003551A (en) * | 2007-01-16 | 2007-07-25 | 广东太阳神集团有限公司 | Method for producing stabhyose, and method for producing stabhyose and catalpol by using rehmannia root |
| CN101041675A (en) * | 2006-03-24 | 2007-09-26 | 厦门牡丹香化实业有限公司 | Method for extracting glutinous rehmannia oligose and glutinous rehmannia polysaccharide from glutinous rehmannia |
-
2013
- 2013-06-18 CN CN201310241313.1A patent/CN103319546B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0383992A (en) * | 1989-08-29 | 1991-04-09 | Ensuiko Sugar Refining Co Ltd | Production of high purity aldosylfructoside |
| JP3623974B2 (en) * | 1993-09-13 | 2005-02-23 | カルピス株式会社 | Oligosaccharide purification method |
| CN1118215A (en) * | 1994-06-20 | 1996-03-13 | 李熙 | Rehmannia glutinosa extract and a safner composition having safner activity to a herbicide paraquat |
| CN1715287A (en) * | 2004-07-01 | 2006-01-04 | 西安大鹏生物科技股份有限公司 | Method for extracting high purity stachyose from radix rehmanniae recen and producing prepared rehmannia root |
| CN101041675A (en) * | 2006-03-24 | 2007-09-26 | 厦门牡丹香化实业有限公司 | Method for extracting glutinous rehmannia oligose and glutinous rehmannia polysaccharide from glutinous rehmannia |
| CN101003551A (en) * | 2007-01-16 | 2007-07-25 | 广东太阳神集团有限公司 | Method for producing stabhyose, and method for producing stabhyose and catalpol by using rehmannia root |
Non-Patent Citations (2)
| Title |
|---|
| 樊海燕: ""地黄中梓醇和水苏糖的提取、分离和纯化"", 《厦门大学硕士学位论文》, 15 August 2009 (2009-08-15), pages 10 * |
| 武卫红: ""地黄寡糖的制备工艺及其药理活性研究"", 《山东大学硕士学位论文》, 15 December 2006 (2006-12-15), pages 16 - 17 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315314A (en) * | 2014-07-31 | 2016-02-10 | 中国食品发酵工业研究院 | Industrial production method for extracting stachyose from radix rehmanniae |
| CN112587959A (en) * | 2019-12-31 | 2021-04-02 | 杭州九源基因工程有限公司 | Method for regenerating chromatographic stationary phase in step of preparing acylated polypeptide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103319546B (en) | 2016-05-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101712669B (en) | Method for separating and purifying luteolin | |
| CN101343297B (en) | Method for extracting and purifying gardenoside with absorbent charcoal | |
| CN108864217B (en) | Purification method of pomegranate peel punicalagin | |
| CN101721979B (en) | Method for preparing macroporous adsorbent resin special for separating valine | |
| CN102631414B (en) | SepHaniadelavayi Diels total alkaloid extraction and purification technology | |
| CN102617669B (en) | Method for separating and purifying mangiferin from mango pericarp | |
| CN102321135B (en) | Method for separating and purifying cordycepin by utilizing high-speed counter-current chromatography | |
| CN103059094A (en) | Method for extracting tripterine | |
| CN108033993A (en) | A kind of method for preparing triptonide | |
| CN103319546A (en) | Method for separating high-purity stachyose from rehmannia | |
| CN104876843B (en) | A kind of method that high-purity raphanin is prepared in the seed from rouge radish | |
| CN106967136A (en) | A kind of method of separating high-purity oleuropein | |
| CN104513218A (en) | Method for separating petunidin in lycium ruthenicum murray through high-speed counter-current chromatography | |
| CN104370895B (en) | A kind of preparation method of orientin and Lutonaretin | |
| CN104829656A (en) | Method for preparing gentiopicroside chemical reference substances from gentiana straminea maxim | |
| CN102532077B (en) | Method for preparing salvianolic acid B through separation by means of flash chromatography | |
| CN102908371A (en) | Method for preparing high-purity ferulic acid from angelica sinensis | |
| CN104910216A (en) | Separation method for obtaining a plurality of epimeddium flavones by preparative liquid chromatography | |
| CN108299298B (en) | Efficient extraction method of norisoboldine | |
| CN115385901A (en) | Method for simultaneously separating schaftoside and trigonelline from pinellia ternata | |
| CN101544575B (en) | Method for preparing natural 4-hydroxy-isoleucine | |
| CN104059117A (en) | Method for extracting pleocidin from saccharopolyspora spinosa fermentation liquor | |
| CN109810014A (en) | A kind of two caffeoyl spermidine class compound selective enrichment methods in fructus lycii | |
| CN107556275B (en) | Preparation method of atractylenolide II | |
| CN113105421A (en) | Method for separating and purifying fraxins and aesculetin in ash bark by high-speed countercurrent chromatography |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 710075 No. two, No. 69, hi tech Zone, Shaanxi, Xi'an Patentee after: Shaanxi pharmaceutical holding group new drug technology development Co.,Ltd. Address before: 710075 No. two, No. 69, hi tech Zone, Shaanxi, Xi'an Patentee before: SHAANXI PHARMACEUTICAL DEVELOPMENT CENTER |
|
| CP01 | Change in the name or title of a patent holder | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200928 Address after: Room 10101, unit 1, building 3, No. 69, Keji 2nd Road, hi tech Zone, Xi'an City, Shaanxi Province Patentee after: MEDICINE Research Institute OF SHAANXI PHARMACEUTICAL HOLDING COOPERATION Address before: 710075 No. two, No. 69, hi tech Zone, Shaanxi, Xi'an Patentee before: Shaanxi pharmaceutical holding group new drug technology development Co.,Ltd. |
|
| TR01 | Transfer of patent right |