CN103319546B - A kind of from glutinous rehmannia the method for Separation of Water threose - Google Patents
A kind of from glutinous rehmannia the method for Separation of Water threose Download PDFInfo
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Abstract
The invention discloses a kind of from glutinous rehmannia the method for separating high-purity stachyose, belong to natural product extraction separation technology field, comprise the following steps: after 1) fresh rehmannia root crude extract and water fully being mixed, obtain sample solution; 2) with after aminopropyl bonded silica gel filling high pressure preparative liquid chromatography post, sample solution is splined on to high pressure preparative liquid chromatography post, carries out wash-out taking acetonitrile-water system as eluent; 3) under differential detector detects, carry out Fractional Collections, obtain wood liquid glucose, will after wood liquid glucose low-temperature reduced-pressure concentrate drying, obtain high purity stachyose. The present invention can separate and obtain stachyose directly, fast, and disengaging time is short, and fractional dose is large, yield reaches more than 85%, purity is up to more than 98%, and the waste material producing is few, and post effect is high, required effluent volume is little, floor space is little, has reduced the consuming cost of whole technique, filler and solvent recoverable, environmental friendliness, is applicable to suitability for industrialized production.
Description
Technical field
The invention belongs to natural product extraction separation technology field, be specifically related to one and separate and carry from glutinous rehmanniaThe method of water intaking threose.
Background technology
Stachyose, as a kind of emerging functional four poly oligosaccharides, is a kind of good functional food ingredient,Have the effect that improves body health, these functional four poly oligosaccharides have regulating intestinal canal flora, improve lipidMetabolism. Improve effect of body immunity, this oligosaccharide has hypoglycemic, reducing blood lipid, increase simultaneouslyInsulin sensitivity effect.
At present, stachyose is mainly ion-exchange resin purification and enzyme process is prepared wood aspect separation and purificationSugar, but make spent ion exchange resin and enzyme process prepare stachyose, and manufacturing cycle is long and cost is higher,Based on above reason development of new separation purifying technique, searching separates pure more economically, efficiently, efficientlyChange technology, more and more becomes the focus that researcher 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 operation letterSingle, disengaging time is short, and cost is low, and the product purity obtaining is high, and yield is high.
The present invention is achieved through the following technical solutions:
A method for Separation of Water threose from glutinous rehmannia, comprises the following steps:
1) fresh rehmannia root crude extract and water are pressed to the solid-liquid ratio of 1g:3～7ml, after fully mixing, obtainedSample liquid;
2) with after aminopropyl bonded silica gel filling high pressure preparative liquid chromatography post, sample solution is splined on to high pressurePreparative liquid chromatography post, taking acetonitrile-water system as eluent, washes with the speed constant current of 10～200ml/minDe-30～40min, in described eluent, the volume ratio of acetonitrile and water is (68～73): (27～32);
3) under detecting, differential detector carries out Fractional Collections according to chromatogram appearance time, in stachyose correspondenceWhen peak starts to rise, collect, finish five of whole peak height/a period of time to collect when this peak drops to, obtain waterThreose liquid, by dry after wood liquid glucose reduced pressure concentration, obtains high purity stachyose.
Step 2) described loading employing gradation loading, each loading 10～20ml.
Step 3) dry after described reduced pressure concentration be wood liquid glucose to be concentrated into relative density beAfter 1.10～1.15, at 20～40 DEG C, vacuum drying 20～40h.
Described aminopropyl bonded silica gel passes through activation processing before use, first, and by granule ball-type ammoniaPropyl group bonded silica gel and ethanol are pressed the solid-liquid ratio of 1g:2～3ml, obtain homogenate, by homogenate after fully mixingUltrasonic processing 30～40min removes after bubble, is packed in chromatographic column; Secondly, use water pump pumping liquidAfter till Silica Surface no liquid, be forced into 45～50bar, use high flow rate eluent, with 200ml/minFlow velocity, rinse out the ethanol in post; Finally, with the flow velocity of 100ml/min, rinse 1h, obtain livingAminopropyl bonded silica gel after change.
Described pressurization is to adopt piston to carry out substep pressurization, and the first step is pressurized to 15～20bar, then usesHigh flow rate eluent rinses after pillar 1h, then is pressurized to 45～50bar.
Described high flow rate eluent is the eluent that acetonitrile and water are made into by the volume ratio of 70:30.
The particle diameter of described granule ball-type aminopropyl bonded silica gel is 5～20 μ m, and aperture is
After described high pressure preparative liquid chromatography post post effect reduces, the ammonia spirit that is 5% by mass concentrationCarry out wash-out regeneration, after regeneration, carry out wash-out with pure water, be eluted in efflux without ammonium ion.
The internal temperature of described differential detector is made as 30 DEG C, and external temperature is made as 35 DEG C.
Described fresh rehmannia root crude extract is that after fresh rehmannia root is cleaned, section, adds after flooding 1～4h,At 80～100 DEG C, heating and refluxing extraction 1～5h, by after extracting liquid filtering, obtains filtrate; In filtrate, addAfter absolute ethyl alcohol to ethanol content reaches 90%, at 0～4 DEG C, leave standstill after 10～14h,Under 3000～4000r/min, centrifugal 25～35min, obtains precipitation; After precipitation is dissolved in water, use active carbonAfter decolouring, by after destainer reduced pressure concentration, at 25～30 DEG C, vacuum reaches 0.09～0.15MpaAfter, vacuum drying 20～40h, obtains fresh 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 by high pressure preparative chromatography, uses aminopropyl keyClose silica gel as column packing, successfully separate obtain high purity stachyose, in separation process, only use acetonitrile andThis kind of chromatogram system of water, carries out constant current constant speed Gradient elution, adopts differential detector on-line monitoring methodSeparated product and impurity, accomplish accurate collection, separation process simple and fast, and first separation just can reach order, without any need for chemical treatment method, can not lose stachyose, can be directly, separate and obtain fastStachyose, and disengaging time is short, and fractional dose is large, and yield reaches more than 85%, and the stachyose obtaining is pureDegree is up to more than 98%.
The waste material that the inventive method produces is few, and post effect is high, and required effluent volume is little, and floor space is little,Reduce the consuming cost of whole technique, filler and solvent recoverable, environmental friendliness, is applicable to industryChange and produce.
Brief description of the drawings
Fig. 1 is the HPLC chromatogram of each composition in 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 obtaining.
Wherein, 1 is glucose, and 2 is fructose, and 3 is sucrose, and 4 is stachyose, and 5 is gossypose.
Detailed description of the invention
Below in conjunction with concrete drawings and Examples, the present invention is described in further detail, described in be rightExplanation of the present invention instead of restriction.
The reagent that the present invention is used and laboratory apparatus
1, reagent: it is pure that preparation is analysis with acetonitrile, ethanol, ammonia, and analysis is chromatographically pure with acetonitrile, waterFor secondary redistilled water;
2, laboratory apparatus: the present invention has adopted the granule ball-type aminopropyl bonded silica gel filler of external import,Can under high pressure use, the separating degree of this aminopropyl bonded silica gel related impurities approaches analytic type HPLC,Have good Reusability ability, major diameter preparative column is that imported from America (VARIAN) can be certainly simultaneouslyLoad high-pressure chromatographic column, it is imported from America (VARIAN) that high pressure is prepared liquid phase systems, and preparation is rolled over by differentialPhotodetector is imported from America (VARIAN), and fraction collection system is imported from America (VARIAN) automatically,Product analysis is used high performance liquid chromatograph for the U.S. (Waters) production.
A method for Separation of Water threose from glutinous rehmannia, comprises the following steps:
1) fresh rehmannia root crude extract and water are pressed to the solid-liquid ratio of 1g:3～7ml, after fully mixing, obtained sampleProduct;
2) with after aminopropyl bonded silica gel filling high pressure preparative liquid chromatography post, sample gradation is splined on to heightThe standby liquid-phase chromatographic column of compacting, taking acetonitrile-water system as eluent, with the speed constant current of 10～200ml/minWash-out 20～40min, in described eluent, the volume ratio of acetonitrile and water is (68～73): (27～32); InstituteThe gradation loading of stating is each loading 10～20ml sample;
3) under differential detector detects, carry out Fractional Collections, obtain wood liquid glucose, by wood liquid glucose low temperatureAfter drying under reduced pressure, obtain high purity stachyose.
The fresh rehmannia root crude extract using is that after fresh rehmannia root is cleaned, section, adds after flooding 1～4h, thenAt 80～100 DEG C, heating and refluxing extraction 1～5h, collects extract, after extract is filtered while hot,To adding in filtrate absolute ethyl alcohol to shake up to after reaching 90% containing alcohol amount, low temperature is placed 10～14 hours, takes outAfter under 3000～4000r/min, centrifugal 25～35min, abandoning supernatant, sediment water dissolve makeWith activated carbon decolorizing, by after destainer reduced pressure concentration, at 20～40 DEG C, vacuum reaches 0.09～When 0.15Mpa, vacuum drying 20～40h, obtains glutinous rehmannia crude extract.
Before purified water threose, need to carry out chromatographic column filling, take appropriate aminopropyl bonded silica gelFiller, by the solid-liquid ratio of 1g:2～3ml, adds with ethanol and fully mixes and make homogenate, and homogenate is ultrasonicProcess 30～50min and remove after bubble, pour in gc column tube, use vacuum pump pumping liquid until siliconTill glue surface does not just have liquid, cover after flange and carry out substep pressurization with piston, be pressurized to for the first time15～20bar, then rinses after pillar 1h with the eluent of high flow rate, then is pressurized to 45～50bar, continuesRinse pillar constant speed with eluent and activate, stand-by; For obtaining best separating effect, pillar is loaded heightFor 25cm left and right.
Fresh rehmannia root crude extract is dissolved in water, and the ratio of dissolving is about 1:3～7, then enters with filter membraneRow filters, and the sample batch sampling high pressure preparative liquid chromatography system of having dissolved is carried out constant speed Gradient elution,Elution time is 20～40min; Eluent is made up of acetonitrile and water two parts, and the Polarity Control of eluent existsThe retention time of stachyose in high pressure chromatogram is between 10～20min, and the flow velocity of whole preparation process is protectedBe held between 10～200ml/min.
Product carries out Fractional Collections (internal temperature according to chromatographic peak appearance time under differential detector detects30 DEG C, 35 DEG C of external temperatures). In chromatographic isolation of the present invention, glucose, sucrose, fructose are in waterThe leading portion of threose, peak type is more symmetrical, therefore in separation process, opens at peak but peak does not reach baseline separationWhile beginning to rise, collect, peak drops to and finishes to collect whole five high/a period of time.
The stachyose eluent of collecting in chromatographic separation process, is concentrated into relatively close by Rotary EvaporatorsDegree uses vacuum drying when 1.10～1.15 (60 DEG C of surveys), and at 20～40 DEG C, vacuum is 0.09～Under 0.15Mpa, vacuum drying 20～40h, the dry powder obtaining, quantitative by high performance liquid chromatographyPurity assay is more than 98%.
Through chromatographic isolation repeatedly, the splitter effect of high pressure preparative liquid chromatography post reduces, and now can use matterAmount concentration is 5% ammonia spirit carries out back flush preparative column, and column flow rate is chromatographic isolation flow velocity10～20%, then use pure water to wash away ammonia unnecessary in chromatographic column, recover chromatographic column post effect.
Embodiment 1
A method for Separation of Water threose from glutinous rehmannia, comprises the following steps:
1) in the open glass container of 5L, add the ball-type aminopropyl bonded silica gel of the 10 μ m of 700g,Add and analyze ethanol 2100mL, stir into homogenate, after ultrasonic 40min, pour ready diameter 5cm into,Column length is that in the stainless steel chromatogram column jecket of 30cm, extracting liquid covers flange, uses acetonitrile and water to press 70:30The eluent that is made into of volume ratio, carry out wash-out with the flow velocity of 200ml/min, rinse out second in chromatographic columnAlcohol, carries out substep pressurization with piston in post, and the first step is pressurized to 15bar, then uses the stream of 100ml/minSpeed is rinsed after 1h, then is forced into 50bar, activation;
2), after chromatographic column is ready to complete, take fresh rehmannia root crude extract 100g (content of stachyose is 38.9%),Be dissolved in 500ml water, filter, high pressure is prepared flow rate pump 50ml/min, sample introduction 10ml, with acetonitrile withThe volume ratio 68:32 of water is eluent, carries out constant speed wash-out, under differential detector (30 DEG C of internal temperatures,35 DEG C of external temperatures) detect whole elution process, observe chromatographic peak by software, referring to Fig. 1,15.8min stachyose product rises on peak, collects by automatic fraction collector, and acquisition time is waterThreose peak starts ascent stage 15.87 minutes, and the stachyose peak whole peak height 1/5th that declines finishes to collect,After 30min, finish this elution system, in collection of illustrative plates, 1 is glucose, and 2 is fructose, and 3 is sucrose, and 4 areStachyose, 5 is gossypose; After finishing, this wash-out carries out the collection of repetition sample introduction, until the fresh ground of preparationYellow thick extraction sample feeding is complete;
3) collect liquid and in Rotary Evaporators, reclaim solvent, to relative density 1.10 (60 DEG C of surveys), useVacuum drying (vacuum is 0.09～0.15Mpa, and temperature is not higher than 30 DEG C) is dried 20～40h,To dried powder 32.6g, by high performance liquid chromatography quantitative analysis, referring to Fig. 2, content of stachyose is98.6%, yield is 87.4%.
Embodiment 2
A method for Separation of Water threose from glutinous rehmannia, comprises the following steps:
1) in the open glass container of 5L, add the ball-type aminopropyl bonded silica gel of the 5 μ m of 200g,Add and analyze ethanol 600mL, stir into homogenate, after ultrasonic 30min, pour ready diameter 1.5cm into,Column length is that in the stainless steel chromatogram column jecket of 20cm, extracting liquid covers flange, uses acetonitrile and water to press 70:30The eluent that is made into of volume ratio, carry out wash-out with the flow velocity of 200ml/min, rinse out second in chromatographic columnAlcohol, carries out substep pressurization with piston in post, and the first step is pressurized to 15bar, then uses the stream of 100ml/minSpeed is rinsed after 1h, then is forced into 45bar, activation;
2), after chromatographic column is ready to complete, take fresh rehmannia root crude extract 150g (content of stachyose is 38.9%),Be dissolved in 900ml water, filter, high pressure is prepared flow rate pump 100ml/min, and sample introduction 20ml, with acetonitrileWith the volume ratio 70:30 of water be eluent, carry out constant speed wash-out, (internal temperature under differential detector30 DEG C, 35 DEG C of external temperatures) detect whole elution process, observe chromatographic peak by software, at 14.6minStachyose product rises on peak, collects by automatic fraction collector, and acquisition time is that stachyose peak is openedBeginning ascent stage 14.67 minutes, the peak whole peak height 1/5th that declines finishes to collect. After 40min, finish thisInferior elution system, carries out the collection of repetition sample introduction, until the fresh rehmannia root of preparation slightly to extract sample feeding complete,Collect liquid and in Rotary Evaporators, reclaim solvent, to relative density 1.10 (60 DEG C of surveys), use vacuum drying(vacuum is 0.09～0.15Mpa), at 25～30 DEG C, dry 20～40h, obtains dried powder52.3g, by high performance liquid chromatography quantitative analysis, content of stachyose is 98.9%, yield is 88.6%.
Embodiment 3
A method for Separation of Water threose from glutinous rehmannia, comprises the following steps:
1) in the open glass container of 5L, add the ball-type aminopropyl bonded silica gel of the 20 μ m of 700g,Add and analyze ethanol 1800mL, stir into homogenate, after ultrasonic 35min, pour ready diameter 15cm into,Column length is that in the stainless steel chromatogram column jecket of 35cm, extracting liquid covers flange, uses acetonitrile and water to press 70:30The eluent that is made into of volume ratio, carry out wash-out with the flow velocity of 200ml/min, rinse out second in chromatographic columnAlcohol, carries out substep pressurization with piston in post, and the first step is pressurized to 15bar, then uses the stream of 100ml/minSpeed is rinsed after 1h, then is forced into 45bar, activation;
2), after chromatographic column is ready to complete, take fresh rehmannia root crude extract 100g (content of stachyose is 38.9%),Be dissolved in 700ml water, filter, high pressure is prepared flow rate pump 200ml/min, and sample introduction 15ml, with acetonitrileWith the volume ratio 73:27 of water be eluent, carry out constant speed wash-out, (internal temperature under differential detector30 DEG C, 35 DEG C of external temperatures) detect whole elution process, observe chromatographic peak by software, at 14.5minStachyose product rises on peak, collects by automatic fraction collector, and acquisition time is that stachyose peak is openedBeginning ascent stage 14.56 minutes, the peak whole peak height 1/5th that declines finishes to collect. After 40min, finish thisInferior elution system, carries out the collection of repetition sample introduction, until the fresh rehmannia root of preparation slightly to extract sample feeding complete,Collect liquid and in Rotary Evaporators, reclaim solvent, to relative density 1.15 (60 DEG C of surveys), use vacuum drying(vacuum is 0.09～0.15Mpa), at 25～30 DEG C, dry 20～40h, obtains dried powder47.9g, by high performance liquid chromatography quantitative analysis, content of stachyose is 98.3%, yield is 87.9%.
Embodiment 4
A method for Separation of Water threose from glutinous rehmannia, comprises the following steps:
1) in the open glass container of 5L, add the ball-type aminopropyl bonded silica gel of the 10 μ m of 700g,Add and analyze ethanol 1400mL, stir into homogenate, after ultrasonic 35min, pour ready diameter 8cm into,Column length is that in the stainless steel chromatogram column jecket of 40cm, extracting liquid covers flange, uses acetonitrile and water to press 70:30The eluent that is made into of volume ratio, carry out wash-out with the flow velocity of 200ml/min, rinse out second in chromatographic columnAlcohol, carries out substep pressurization with piston in post, and the first step is pressurized to 15bar, then uses the stream of 100ml/minSpeed is rinsed after 1h, then is forced into 45bar, activation;
2), after chromatographic column is ready to complete, take fresh rehmannia root crude extract 100g (content of stachyose is 38.9%),Be dissolved in 300ml water, filter, high pressure is prepared flow rate pump 10ml/min, sample introduction 10ml, with acetonitrile withThe volume ratio 69:31 of water is eluent, carries out constant speed wash-out, under differential detector (30 DEG C of internal temperatures,35 DEG C of external temperatures) detect whole elution process, observe chromatographic peak by software, at 15.3min woodSugar product rises on peak, collects by automatic fraction collector, and acquisition time is on stachyose peak startsRise 15.38 minutes stages, the peak whole peak height 1/5th that declines finishes to collect. After 40min, finishing this washesDe-system, carries out the collection of repetition sample introduction, until that the fresh rehmannia root of preparation is slightly extracted sample feeding is complete, collectsLiquid reclaims solvent in Rotary Evaporators, to relative density 1.12 (60 DEG C of surveys), uses vacuum drying (trueReciprocal of duty cycle is 0.09～0.15Mpa) at 25～30 DEG C, dry 20～40h, obtains dried powder 44.2g,By high performance liquid chromatography quantitative analysis, content of stachyose is 98.3%, and yield is 87.2%.
To sum up, the method for high performance preparative liquid chromatography Separation of Water threose provided by the present invention, examines in differentialSurvey the accurate collection of carrying out separated product and impurity under device on-line monitoring, separation process simple and fast, onceSeparate and just can achieve the goal, without any need for chemical treatment method, effectively ensured that stachyose can not lose,The separation process used time is short, and fractional dose is large, and the yield of stachyose can reach more than 85%, particularly purityCan reach more than 98%. This method operating cost is low, and filler for a long time repetitive cycling uses, solventRecyclable reusing, disengaging time is short, and fractional dose is large, is applicable to suitability for industrialized production.
Claims (4)
1. a method for Separation of Water threose from glutinous rehmannia, is characterized in that, comprises the following steps:
1) fresh rehmannia root crude extract and water are pressed to the solid-liquid ratio of 1g:3～7ml, after fully mixing, obtainedSample liquid;
Described fresh rehmannia root crude extract is that after fresh rehmannia root is cleaned, section, adds after flooding 1～4h,At 80～100 DEG C, heating and refluxing extraction 1～5h, by after extracting liquid filtering, obtains filtrate; In filtrate, addAfter absolute ethyl alcohol to ethanol content reaches 90%, at 0～4 DEG C, leave standstill after 10～14h,Under 3000～4000r/min, centrifugal 25～35min, obtains precipitation; After precipitation is dissolved in water, use active carbonAfter decolouring, by after destainer reduced pressure concentration, at 25～30 DEG C, vacuum reaches 0.09～0.15MpaAfter, vacuum drying 20～40h, obtains fresh rehmannia root crude extract;
2) with after aminopropyl bonded silica gel filling high pressure preparative liquid chromatography post, sample solution is splined on to high pressurePreparative liquid chromatography post, taking acetonitrile-water system as eluent, washes with the speed constant current of 50～200ml/minDe-30～40min, in described eluent, the volume ratio of acetonitrile and water is (68～73): (27～32);
Described loading adopts gradation loading, each loading 10～20ml;
Described aminopropyl bonded silica gel passes through activation processing before use, first, is 5～20 μ m by particle diameter,Aperture isBall-type aminopropyl bonded silica gel and ethanol press the solid-liquid ratio of 1g:2～3ml, fullyAfter mixing, obtain homogenate, ultrasonic homogenate processing 30～40min is removed after bubble, be packed in chromatographic column;Secondly, to after till Silica Surface no liquid, be forced into 45～50bar with water pump pumping liquid, use acetonitrileEluent with water is made into by the volume ratio of 70:30, with the flow velocity of 200ml/min, rinses out in postEthanol; Finally, with the flow velocity of 100ml/min, rinse 1h, obtain the aminopropyl bonded silica gel after activation;
3) under detecting, differential detector carries out Fractional Collections according to chromatogram appearance time, in stachyose correspondenceWhen peak starts to rise, collect, finish five of whole peak height/a period of time to collect when this peak drops to, obtain waterThreose liquid, by dry after wood liquid glucose reduced pressure concentration, obtains stachyose;
Dry after described reduced pressure concentration is after wood liquid glucose is concentrated into relative density and is 1.10～1.15,At 20～40 DEG C, 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 pressurization is to adopt piston to carry out substep pressurization, and the first step is pressurized to 15～20bar, then uses acetonitrileThe eluent being made into by the volume ratio of 70:30 with water rinses after pillar 1h, then is pressurized to 45～50bar.
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, the ammonia spirit that is 5% by mass concentration carries outWash-out regeneration, carries out wash-out with pure water after regeneration, is eluted in efflux 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 DEG C, and external temperature is made as 35 DEG C.
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| CN111111264A (en) * | 2019-12-31 | 2020-05-08 | 杭州九源基因工程有限公司 | Regeneration method of chromatographic stationary phase in step of preparing polypeptide |
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