CN101085129B - Acorus gramineus total phenylpropanoid extraction preparation method - Google Patents
Acorus gramineus total phenylpropanoid extraction preparation method Download PDFInfo
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Abstract
The invention discloses total phenyl propanoid extract and total phenol extract extracted from grassleaved sweetflag rhizome and its preparation method. Total phenyl propanoid extract mainly comprises beta -asaricin, alpha -asaricin, eudesmin, galgravin, veraguensin and other derivant with veraguensin as mother nuclide. Total phenol extract mainly comprises caffeic acid, protocatechuic acid, ferulic acid, vanillic acid and glucosides with vanillic acid as mother nuclide and other derivants. Total phenyl propanoid extract and total phenol extract of grassleaved sweetflag rhizome can be extracted through one or more of methods of solvent-extraction, solvent extraction, precipitation method, macroporous adsorbent resin, extraction by supercritical fluid, column chromatography, and liquid-liquid countercurrent distribution chromatography. Total percentage content of phenyl propanoids in the obtained total phenyl propanoid extract of Grassleaved sweetflag rhizome is 5-100% (w/w), wherein content of beta -asaricin and alpha -asaricin occupy 5-100% (w/w).Total percentage content of phenols in total phenol extract of grassleaved sweetflag rhizome is 5-100% (w/w), wherein content of caffeic acid and protocatechuic acid occupy 5-100% (w/w).
Description
Technical field
The invention belongs to medical technical field, be specifically related to the total phenylpropanoid extract of Chinese medicine Rhizome of Grass leaf Sweelflag and total phenol extraction thing and preparation method thereof, quality controlling means, and in the application of medicine and field of health care food.
Background technology
Rhizome of Grass leaf Sweelflag is a conventional Chinese medicine, derives from Araeceae Acorus Rhizome of Grass leaf Sweelflag Acorus tatarinowiiSchott. and belongs to the dry rhizome of other plant together.Traditional Chinese medicine theory thinks that Rhizome of Grass leaf Sweelflag has the open-minded phlegm of having one's ideas straightened out, the inducing resuscitation intelligence development, hearing-improing and eyesight improving, the dampness elimination appetizing and the cold effect of removing numbness of loosing, cure mainly stupor, epilepsy, demented, coronary heart disease, stenocardia, irregular pulse, apoplexy, dizzy, tinnitus, deaf, atrophic gastritis, cerebral trauma, retarded, cards such as nasosinusitis, modern pharmacological research shows that Rhizome of Grass leaf Sweelflag has calmness, anti-frightened, spasmolysis is relievingd asthma, antidepressant, promote memory, lipopenicillinase, anticancer, multiple efficacies such as anti-arrhythmia, wide clinical application is in the treatment epilepsy, coma due to blocking of the respiratory system, the pyreticosis coma, forgetful, deafness with qi stagnation, the ambition unhappiness, energy-stagnation stomachache, diseases such as arthritis with fixed pain caused by dampness.Mainly contain compositions such as the plain class of phenylpropyl alcohol, phenols, flavonoid, alkaloids, triterpenes in the Rhizome of Grass leaf Sweelflag.So far, the pharmacologically active of relevant Rhizome of Grass leaf Sweelflag chemical ingredients, application and preparation method, rarely seen have an invention disclosed patent 97106786.4, the preparation method who relates to alkaloids composition in the Rhizome of Grass leaf Sweelflag does not see the patent that relates to Rhizome of Grass leaf Sweelflag total phenylpropanoid extract and total phenol extraction thing and its production and use.
Summary of the invention
The object of the present invention is to provide a kind of Rhizome of Grass leaf Sweelflag total phenylpropanoid extract and preparation method thereof.
Another object of the present invention is to provide total phenol extraction thing of a kind of Rhizome of Grass leaf Sweelflag and preparation method thereof.
A further object of the present invention is to provide the metallic salt derivative of the total phenol extraction thing of a kind of Rhizome of Grass leaf Sweelflag and some alkali or metal-salt formation.
A further object of the present invention is to provide the metal complex of total phenol extraction thing of a kind of Rhizome of Grass leaf Sweelflag and the formation of some metal ion.
The Rhizome of Grass leaf Sweelflag total phenylpropanoid extract that the present invention proposes is the combination that contains the plain active component of multiple phenylpropyl alcohol of therefrom extracting in the remedies calamus, and wherein the main compound structure is as follows:
The total phenol extraction thing of Rhizome of Grass leaf Sweelflag that the present invention proposes is the combination that contains multiple phenolic active components of therefrom extracting in the remedies calamus, and wherein the main compound structure is as follows:
Raw material Rhizome of Grass leaf Sweelflag of the present invention derives from any one plant of Araeceae Acorus.As the starting material that extract Rhizome of Grass leaf Sweelflag total phenylpropanoid and total phenol, it can be commercially available Rhizome of Grass leaf Sweelflag medicine materical crude slice, can be arbitrary position or the whole plant such as stem, leaf, Hua Sui, fruit, underground rhizome and root of these plants, the dry rhizome of scape not be taken out at wherein preferred medicinal material position for these plants yet.Above-mentioned described Rhizome of Grass leaf Sweelflag comprises crude drug and the medicine materical crude slice of handling without any process of preparing Chinese medicine, also comprises various processed products.
Rhizome of Grass leaf Sweelflag total phenylpropanoid extract of the present invention, be meant to extract and obtain from any position of above-mentioned arbitrary plant, the composition that comprises the plain active component of multiple phenylpropyl alcohol, wherein preferably do not take out to extract the dry rhizome of scape and prepare, contain the composition of the plain active component of multiple phenylpropyl alcohol from Acorustatarinowii Schott..The plain constituents of these phenylpropyl alcohols mainly comprise beta-Asarone, α-trans-Isoasarone, Eudesmin, galgravin, veraguensin and are other derivative of parent nucleus with it.
As Rhizome of Grass leaf Sweelflag total phenylpropanoid extract, the summation of the plain constituents percentage compositions of wherein various phenylpropyl alcohols is 5～100% (w/w), wherein 50～100% (w/w) preferably.
Among the plain active components of the various phenylpropyl alcohols that Rhizome of Grass leaf Sweelflag total phenylpropanoid extract of the present invention is contained, compositions such as beta-Asarone, α-trans-Isoasarone, Eudesmin, galgravin, veraguensin most importantly.As Rhizome of Grass leaf Sweelflag total phenylpropanoid extract, the content of beta-Asarone, two kinds of compositions of α-trans-Isoasarone accounts for 5～100% (w/w) of whole total phenylpropanoid content.
The total phenol extraction thing of Rhizome of Grass leaf Sweelflag of the present invention, be meant to extract and obtain from any position of above-mentioned arbitrary plant, the composition that comprises multiple phenolic active components, wherein preferably from Acorus tatarinowiiSchott. dry rhizome, extract and to prepare, contain the composition of multiple phenolic active components.These phenols components mainly comprise coffic acid, Protocatechuic Acid, forulic acid, vanillic acid and are glucoside compound and other derivative of parent nucleus with it.
As the total phenol extraction thing of Rhizome of Grass leaf Sweelflag, the summation of wherein various phenols component percentage compositions is 5～100% (w/w), wherein 50～100% (w/w) preferably.
The total phenol extraction thing of Rhizome of Grass leaf Sweelflag of the present invention, can with metal-salts (as yellow soda ash, salt of wormwood, lime carbonate, sodium-acetate, zinc acetate etc.) such as some alkali (as sodium hydroxide, potassium hydroxide etc.) and sodium salt, sylvite, calcium salt, zinc salt, form the metallic salt derivative.These derivatives have and identical or close pharmacologically active and the purposes of the total phenol extraction thing of above-mentioned Rhizome of Grass leaf Sweelflag.
The total phenol extraction thing of Rhizome of Grass leaf Sweelflag of the present invention can also form metal complex with metal ions such as sodium, potassium, calcium, iron, aluminium, zinc, copper, barium, chromium, strontiums.These metal complexs have and identical or close pharmacologically active or the purposes of the total phenol extraction thing of above-mentioned Rhizome of Grass leaf Sweelflag.
Among the various phenolic active components that the total phenol extraction thing of Rhizome of Grass leaf Sweelflag of the present invention is contained, most importantly coffic acid, Protocatechuic Acid, forulic acid, vanillic acid, 4-{[(E)-(4-hydroxylbenzoyl) diazenyl] carbonyl}phenol, 3,5,4 '-trihydroxy--6, compositions such as 7-methylene-dioxy flavones, Schuttgelb.As the total phenol extraction thing of Rhizome of Grass leaf Sweelflag, the content of coffic acid, Protocatechuic Acid composition accounts for 5～100% (w/w) of whole total phenol contents.
The invention allows for the preparation technology of described Rhizome of Grass leaf Sweelflag total phenylpropanoid extract and total phenol extraction thing, it can adopt following any one method, or the arbitrary combination of these methods is prepared: (1) solvent-extraction process; (2) solvent extration; (3) precipitator method; (4) supercritical fluid extraction; (5) column chromatography; (6) liquid-liquid adverse current partition chromatography.Wherein preferable methods is the precipitator method and macroporous adsorbent resin method.
When these methods of use are prepared, generally comprise following step:
(1) extract: solvent for use can be water or any one alcohols, ketone and esters solvent, or the mixed solvent formed by a certain percentage of these solvents, or the acidity or the basic solvent that are made into by these solvents and acid, alkali, salt.Extracting method can be decoction, reflux, supersound extraction, cold soaking, diacolation, microwave extraction, high pressure extract etc.
Preferred extraction process is: the Rhizome of Grass leaf Sweelflag medicinal material adds 30～90% ethanol, and refluxing extraction 2～3 times was extracted 1～2 hour at every turn, and solvent load is 5～15 times of amounts (L/kg).
(2) filter: comprise methods such as centrifugal, suction filtration, ultrafiltration, press filtration, use or do not use following any one finings or its combination: the alcohol precipitation agent, gelatin, kaolin, various resins, polyoxyethylene glycol, poly-second triol, chitosan and natural clarifying agent finished product are as 101 fruit juice clarifiers, ZTC+1 natural clarifying agent etc.
(3) concentrate: comprise thin film evaporation, rotary evaporation and decocting and concentrating etc. under normal pressure or the reduced pressure.
(4) drying: comprise vacuum-drying, spraying drying, lyophilize etc.
When adopting solvent extration to be prepared, general earlier extract mixture being suspended from the water, then with low polar ester class, alkanes or ether solvent (as sherwood oil, ether, hexane, gasoline, ethyl acetate etc.) chloroform, ethyl acetate or the mixture of these solvents, extraction obtains total phenylpropanoid composition and total phenol composition wherein, obtains total phenylpropanoid extract and total phenol extraction thing.
When adopting the precipitator method to be prepared, preferred Rhizome of Grass leaf Sweelflag phenylpropyl alcohol extract preparation technology is: Rhizome of Grass leaf Sweelflag medicinal material ethanol extraction adds the distilled water of certain volume, makes that the medicinal material amount is 1: 6～1: 10 with disperseing back liquor capacity ratio.Respectively with 3000～5000 rev/mins speed centrifugal 30～60 minutes again, inclining supernatant liquor, will precipitate with 2～5BV (crude drug amount) sherwood oil to reflux 2～3 times, each 1.0～2.0 hours, merge petroleum ether extract, reclaim solvent, residue is the phenylpropyl alcohol extract.
When adopting the macroporous adsorbent resin method to be prepared, used macroporous resin can be any one types such as nonpolar, low-pole, middle polarity, weakly alkaline or slightly acidic, the code name of these resins is different because manufacturer is different, as D101, D4020, HPD400, AB-8, S-8, HZ-806 etc., the resin of low-pole or middle polarity preferably wherein is as AB-8, HPD400, D 101 etc.Used eluent is water and aqueous ethanol, methyl alcohol, acetone etc., wherein 0～100% ethanol preferably.
Preferred Rhizome of Grass leaf Sweelflag phenols extract resin purification technology is: select for use middle polarity such as AB-8, HPD400 or low-pole macroporous adsorbent resin as the purifying resin, Rhizome of Grass leaf Sweelflag ethanol extraction sample solution concentration 2～4mg/mL (in total phenol amount), absorption flow velocity 2～6BV/h, resin column blade diameter length ratio 1: 8～1: 13, applied sample amount is 0.5～2.55mg/mL (in total phenol amount), 1～2 times of resin volume of water elution carries out removal of impurities, the removal of impurities flow velocity is 3～8BV/h, with 3～6 times of resin volumes of 40～90% ethanol elutions, elution flow rate is 4～9BV/h.
The total phenol extraction thing of Rhizome of Grass leaf Sweelflag preparation method, when using the macroporous adsorbent resin method, used macroporous resin can be any types such as nonpolar, low-pole, middle polarity, weakly alkaline or slightly acidic, the code name of these resins is different because manufacturer is different, as D101, D4020, HPD400, AB-8, S-8, HZ-806 etc., the resin of low-pole or middle polarity preferably wherein, as AB-8, HPD400, D 101 etc., used eluent is water and aqueous ethanol, methyl alcohol, acetone etc.The total phenol extraction thing of Rhizome of Grass leaf Sweelflag preparation method, select for use middle polarity such as AB-8, HPD400 or low-pole macroporous adsorbent resin as the purifying resin, the Rhizome of Grass leaf Sweelflag ethanol extraction is in the sample solution concentration 2～4mg/mL of total phenol amount, absorption flow velocity 3～9BV/h, resin column blade diameter length ratio 1: 5～1: 10, applied sample amount in total phenol amount is 0.5～2.55mg/mL, 1～2 times of resin volume of water elution carries out removal of impurities, the removal of impurities flow velocity is 3～8BV/h, with 4～8 times of resin volumes of 40～90% ethanol elutions, elution flow rate is 5～9BV/h.
When adopting supercritical fluid extraction to be prepared, can directly extract the Rhizome of Grass leaf Sweelflag starting material, also can the product that above-mentioned arbitrary method and step obtained be extracted.Can use or not use following any kind solvent and solvent mixture during extraction: water, alcohols, ketone and esters solvent.
When adopting column chromatography to be prepared, the object of its processing can be the product that the said extracted step is obtained, and also can be the product behind above-mentioned solvent-extraction process, solvent extration, the precipitator method or supercritical fluid extraction preliminary purification.Used stationary phase can be silica gel, polymeric amide, aluminum oxide, dextran (Sephadex series or Sephadex LH-20 series), C-8, C-18, gac, Mierocrystalline cellulose etc., used elutriant is different because of the difference of stationary phase, generally the mixed solvent of being made up of water, methyl alcohol, ethanol, acetone, chloroform, ethyl acetate, sherwood oil etc.
Liquid-when the liquid counter-current extraction was prepared, the object of its processing can be the product of said extracted step when adopting, and also can be the product behind above-mentioned solvent-extraction process, solvent extration, the precipitator method or supercritical fluid extraction preliminary purification.General earlier extract mixture being suspended from the water, then with low polar ester class, alkanes or ether solvent (as sherwood oil, ether, hexane, gasoline, ethyl acetate etc.), chloroform, ethyl acetate, or the mixture of these solvents, extraction obtains total phenylpropanoid composition and total phenol composition wherein, gets total phenylpropanoid extract and total phenol extraction thing.
Rhizome of Grass leaf Sweelflag total phenylpropanoid extract and total phenol extraction thing can be separately, make up or press the arbitrary proportion compatibility with other any Chinese and western drugs or food, be used to prepare medicine or functional foodstuff, prepared medicine or functional foodstuff can be capsule, tablet, pill, granule, oral liquid, syrup, electuary, vina, injection, paste, powder, beverage etc.
Quality controlling means of the present invention can comprise one or both in the following content assaying method:
1. total phenylpropanoid
Precision takes by weighing α-trans-Isoasarone reference substance an amount of (about 3mg), puts in the 50mL measuring bottle, adds dissolve with methanol and is diluted to scale, shakes up, and precision is got 2.0mL to the 25mL volumetric flask, adds anhydrous methanol and it is dissolved fully and is diluted to scale, shakes up, in contrast product solution.Accurate α-trans-Isoasarone reference substance solution 0.0,1.0,2.0,3.0,4.0, the 5.0mL of drawing puts respectively in the 10mL measuring bottle, and each measuring bottle adds the anhydrous methanol constant volume, measures absorbancy in the 260nm place.With α-trans-Isoasarone reference substance sampling amount is X-coordinate, and absorbancy is an ordinate zou, the drawing standard curve.
Precision takes by weighing each 3 parts in Rhizome of Grass leaf Sweelflag total phenylpropanoid extract sample, and every part of 20mg puts in the 100mL measuring bottle, it is an amount of to add chloroform, supersound process 5 minutes with chloroform dissolving and be diluted to scale, shakes up, filter, discard filtrate just, precision is measured subsequent filtrate 10.0mL in the 25mL measuring bottle, adds anhydrous methanol to scale, shake up, as sample solution.The above-mentioned sample solution 1.0mL of accurate respectively absorption puts in the 25mL measuring bottle, and accurate respectively again α-trans-Isoasarone reference substance solution 2.0, the 4.0mL of drawing puts in the 10mL measuring bottle, and each measuring bottle adds the anhydrous methanol constant volume, measures absorbancy in the 260nm place.The external standard two-point method calculates content.
2. beta-Asarone, α-trans-Isoasarone
Chromatographic condition: chromatographic column: kromasil ODS C
18Post (4.6mm * 250mm, 5 μ m); Moving phase: methanol-water (56: 44); Flow velocity: 1.0mL/min; Detect wavelength: 257nm; Column temperature: room temperature.
Typical curve is drawn:
Get beta-Asarone reference substance 5mg, the accurate title, decide, and puts in the 25mL measuring bottle, adds dissolve with methanol and be diluted to scale, shakes up, and promptly gets beta-Asarone reference substance storing solution (every 1mL contains beta-Asarone 0.2mg).
Get α-trans-Isoasarone reference substance 2mg, the accurate title, decide, and puts in the 25mL measuring bottle, adds dissolve with methanol and be diluted to scale, shakes up, and promptly gets α-trans-Isoasarone reference substance storing solution (every 1mL contains α-trans-Isoasarone 0.08mg).
Accurate respectively beta-Asarone and α-each 2.0mL of trans-Isoasarone reference substance storing solution, the 0.5mL of drawing puts in the same 10mL volumetric flask, adds the methyl alcohol dilution and is settled to scale, shakes up, and promptly gets beta-Asarone, α-trans-Isoasarone mixing reference substance solution.Above-mentioned mixing reference substance solution 0.0,4.0,8.0,12.0,16.0, the 20.0 μ L of accurate respectively absorption by above-mentioned chromatographic condition, measure peak area.With the chromatographic peak peak area is ordinate zou, and reference substance sample size (μ g) is an X-coordinate, the drawing standard curve,
Assay: precision takes by weighing each 3 parts in 3 batches of Rhizome of Grass leaf Sweelflag phenylpropyl alcohol extract samples, and every part of about 20mg puts in the 100mL measuring bottle, it is an amount of to add chloroform, and supersound process 5 minutes is with chloroform dissolving and be diluted to scale, shake up, filter, discard filtrate just, precision is measured subsequent filtrate 10.0mL in the 25mL measuring bottle, add anhydrous methanol to scale, shake up, filter with 0.45 μ m millipore filtration, as the need testing solution of beta-Asarone and α-trans-Isoasarone assay.The above-mentioned need testing solution 10 μ L of accurate absorption inject liquid chromatograph, measure each chromatogram peak-to-peak area, calculate content.
3. total phenol
Precision takes by weighing coffic acid reference substance an amount of (about 5mg), puts in the 100mL measuring bottle, adds dissolve with methanol and is diluted to scale, shakes up, in contrast product solution.
Accurate coffic acid reference substance solution 0.0,0.5,1.0,1.5,2.0, the 2.5mL of drawing, put respectively in the 25mL measuring bottle, each measuring bottle adds dehydrated alcohol and is diluted to 5.0mL, 0.6% iron trichloride-0.9% Tripotassium iron hexacyanide (1: 0.9) the mixing solutions 1.0mL that adds 0.3% sodium lauryl sulphate 2.0mL and new preparation more respectively, mixing is in the dark placed 5min, adds the 0.1mol/L hydrochloric acid soln to scale, in the dark place 20min, measure absorbancy at 720nm wavelength place.With coffic acid reference substance sampling amount is X-coordinate, and absorbancy is an ordinate zou, the drawing standard curve.
Precision takes by weighing each 3 parts of the total phenol extraction matter samples of Rhizome of Grass leaf Sweelflag, and every part of 10mg puts in the 25mL measuring bottle, it is an amount of to add 50% ethanolic soln, supersound process 5 minutes is diluted to scale with 50% ethanolic soln, shakes up, filter, discard filtrate just, precision is measured subsequent filtrate 5.0mL in the 25mL measuring bottle, adds 50% dissolve with ethanol and is diluted to scale, shake up, as sample solution.The above-mentioned sample solution 1.0mL of accurate respectively absorption, coffic acid reference substance solution 1.5mL, 2.0mL, put in the 25mL measuring bottle, each measuring bottle adds dehydrated alcohol and is diluted to 5.0mL, adds 0.6% iron trichloride-0.9% Tripotassium iron hexacyanide (1: 0.9) the mixing solutions 1.0mL of 0.3% sodium lauryl sulphate 2.0mL and new preparation more respectively, mixing, in the dark place 5min, add the 0.1mol/L hydrochloric acid soln to scale, in the dark place 20min, measure absorbancy at 720nm wavelength place.The external standard two-point method calculates content.
4. coffic acid, Protocatechuic Acid
Chromatographic condition: chromatographic column: kromasil ODS C
18Post (4.6mm * 250mm, 5 μ m); Moving phase: methyl alcohol-1% acetic acid aqueous solution (25: 75); Flow velocity: 1.0mL/min; Detect wavelength: 300nm; Column temperature: room temperature.
Typical curve is drawn:
Get coffic acid reference substance 2.5mg, the accurate title, decide, and puts in the 25mL measuring bottle, adds dissolve with methanol and be diluted to scale, shakes up, and promptly gets coffic acid reference substance storing solution (every 1mL contains coffic acid 0.1mg).
Get Protocatechuic Acid reference substance 5mg, the accurate title, decide, and puts in the 25mL measuring bottle, adds dissolve with methanol and be diluted to scale, shakes up, and promptly gets Protocatechuic Acid reference substance storing solution (every 1mL contains Protocatechuic Acid 0.2mg).
Accurate respectively absorption coffic acid and each 2.0mL of Protocatechuic Acid reference substance storing solution put in the same 10mL volumetric flask, add the methyl alcohol dilution and are settled to scale, shake up, and promptly get reference substance solution (every 1mL contains coffic acid 20 μ g, Protocatechuic Acid 40 μ g).
Accurate above-mentioned reference substance solution 4.0,8.0,12.0,16.0,20.0 μ L, the injection high performance liquid chromatograph drawn.Measuring a chromatographic peak peak area according to above-mentioned chromatographic condition, is X-coordinate with the sample size (μ g) of reference substance, and peak area is an ordinate zou, the drawing standard curve.
Assay: precision takes by weighing each 3 parts of 3 batches of total phenol extraction matter samples of Rhizome of Grass leaf Sweelflag, and every part of about 10mg puts in the 10mL measuring bottle, it is an amount of to add 50% ethanolic soln, supersound process 5 minutes is diluted to scale with 50% ethanolic soln, shakes up, filter, discard filtrate just, precision is measured subsequent filtrate 1.0mL in the 10mL measuring bottle, adds 50% dissolve with ethanol and is diluted to scale, shake up, as need testing solution.The above-mentioned need testing solution 20 μ L of accurate absorption inject liquid chromatograph, measure each chromatogram peak-to-peak area, calculate content.
Embodiment
Embodiment 1: Rhizome of Grass leaf Sweelflag total phenylpropanoid extract and total phenol extraction thing preparation technology
Get Rhizome of Grass leaf Sweelflag medicine materical crude slice 1kg, 50% ethanol 10L refluxing extraction 2 times was extracted 2 hours at every turn, and decompression and solvent recovery gets extract, added the water-dispersion dissolving of certain volume, made that medicinal material amount and dispersion back liquor capacity ratio are 1: 6.With 5000 rev/mins speed centrifugal 40 minutes again, inclining supernatant liquor, will precipitate with the 2500mL sherwood oil to reflux 3 times, and each 1.0 hours, merge petroleum ether extract, low-temperature reduced-pressure reclaims solvent, and the residue drying under reduced pressure promptly gets Rhizome of Grass leaf Sweelflag total phenylpropanoid extract.Supernatant liquor is by 10L AB-8 macroporous adsorbent resin, absorption flow velocity 1.0mL/min, the resin column blade diameter length ratio is 1: 10, applied sample amount is 0.96mg/mL (in total phenol amount), 1.7 times of resin volumes of water elution carry out removal of impurities, the removal of impurities flow velocity is 2.0mL/min, 5 times of resin volumes of 50% ethanol elution, and elution flow rate is 2.0mL/min, collect 50% ethanol eluate, reclaim solvent, drying under reduced pressure is the total phenol extraction thing of Rhizome of Grass leaf Sweelflag.
Total phenylpropanoid content is 72% in the mensuration total phenylpropanoid extract, and wherein the content of beta-Asarone, two kinds of compositions of α-trans-Isoasarone accounts for 70% of whole total phenylpropanoid content.Measure that total phenol content is 52% in total phenol extraction thing, wherein the content of coffic acid, two kinds of compositions of Protocatechuic Acid accounts for 15% of whole total phenol contents.
Embodiment 2: Rhizome of Grass leaf Sweelflag total phenylpropanoid extract and total phenol extraction thing preparation technology
Get Rhizome of Grass leaf Sweelflag medicine materical crude slice 1kg, 50% ethanol 15L refluxing extraction 3 times was extracted 1.5 hours at every turn, and decompression and solvent recovery gets extract, added the water-dispersion dissolving of certain volume, made that medicinal material amount and dispersion back liquor capacity ratio are 1: 7.With 5000 rev/mins speed centrifugal 40 minutes again, inclining supernatant liquor, will precipitate with the 3000mL sherwood oil to reflux 3 times, and each 1.0 hours, merge petroleum ether extract, low-temperature reduced-pressure reclaims solvent, and the residue drying under reduced pressure promptly gets Rhizome of Grass leaf Sweelflag total phenylpropanoid extract.Supernatant liquor is by 12L AB-8 macroporous adsorbent resin, absorption flow velocity 1.0mL/min, the resin column blade diameter length ratio is 1: 12, applied sample amount is 1.02mg/mL (in total phenol amount), 2 times of resin volumes of water elution carry out removal of impurities, the removal of impurities flow velocity is 1.0mL/min, 5 times of resin volumes of 50% ethanol elution, and elution flow rate is 2.0mL/min, collect 50% ethanol eluate, reclaim solvent, drying under reduced pressure is the total phenol extraction thing of Rhizome of Grass leaf Sweelflag.
Total phenylpropanoid content is 73% in the mensuration total phenylpropanoid extract, and wherein the content of beta-Asarone, two kinds of compositions of α-trans-Isoasarone accounts for 71% of whole total phenylpropanoid content.Measure that total phenol content is 54% in total phenol extraction thing, wherein the content of coffic acid, two kinds of compositions of Protocatechuic Acid accounts for 15% of whole total phenol contents.
Embodiment 3: Rhizome of Grass leaf Sweelflag total phenylpropanoid extract and total phenol extraction thing preparation technology
Get Rhizome of Grass leaf Sweelflag medicine materical crude slice 1kg, 70% ethanol 12L refluxing extraction 2 times was extracted 2 hours at every turn, and decompression and solvent recovery gets extract, added the water-dispersion dissolving of certain volume, made that medicinal material amount and dispersion back liquor capacity ratio are 1: 8.With 5000 rev/mins speed centrifugal 40 minutes again, inclining supernatant liquor, will precipitate with the 2500mL sherwood oil to reflux 3 times, and each 1.0 hours, merge petroleum ether extract, low-temperature reduced-pressure reclaims solvent, and the residue drying under reduced pressure promptly gets Rhizome of Grass leaf Sweelflag total phenylpropanoid extract.Supernatant liquor is by 12L AB-8 macroporous adsorbent resin, absorption flow velocity 1.0mL/min, the resin column blade diameter length ratio is 1: 10, applied sample amount is 0.96mg/mL (in total phenol amount), 2 times of resin volumes of water elution carry out removal of impurities, the removal of impurities flow velocity is 1.0mL/min, 4 times of resin volumes of 90% ethanol elution, and elution flow rate is 2.0mL/min, collect 90% ethanol eluate, reclaim solvent, drying under reduced pressure is the total phenol extraction thing of Rhizome of Grass leaf Sweelflag.
Total phenylpropanoid content is 69% in the mensuration total phenylpropanoid extract, and wherein the content of beta-Asarone, two kinds of compositions of α-trans-Isoasarone accounts for 66% of whole total phenylpropanoid content.Measure that total phenol content is 68% in total phenol extraction thing, wherein the content of coffic acid, two kinds of compositions of Protocatechuic Acid accounts for 14% of whole total phenol contents.
Embodiment 4: Rhizome of Grass leaf Sweelflag total phenylpropanoid extract and total phenol extraction thing preparation technology
Get Rhizome of Grass leaf Sweelflag medicine materical crude slice 1kg, 70% ethanol 12L refluxing extraction 2 times was extracted 2 hours at every turn, and decompression and solvent recovery gets extract, added the water-dispersion dissolving of certain volume, made that medicinal material amount and dispersion back liquor capacity ratio are 1: 10.With 5000 rev/mins speed centrifugal 60 minutes again, inclining supernatant liquor, will precipitate with the 3000mL sherwood oil to reflux 3 times, and each 1.5 hours, merge petroleum ether extract, low-temperature reduced-pressure reclaims solvent, and the residue drying under reduced pressure promptly gets Rhizome of Grass leaf Sweelflag total phenylpropanoid extract.Supernatant liquor is by 10L AB-8 macroporous adsorbent resin, absorption flow velocity 1.0mL/min, the resin column blade diameter length ratio is 1: 10, applied sample amount is 1.0mg/mL (in total phenol amount), 2 times of resin volumes of water elution carry out removal of impurities, the removal of impurities flow velocity is 1.0mL/min, 4 times of resin volumes of 90% ethanol elution, and elution flow rate is 2.0mL/min, collect 50% ethanol eluate, reclaim solvent, drying under reduced pressure is the total phenol extraction thing of Rhizome of Grass leaf Sweelflag.
Total phenylpropanoid content is 70% in the mensuration total phenylpropanoid extract, and wherein the content of beta-Asarone, two kinds of compositions of α-trans-Isoasarone accounts for 68% of whole total phenylpropanoid content.Measure that total phenol content is 56% in total phenol extraction thing, wherein the content of coffic acid, two kinds of compositions of Protocatechuic Acid accounts for 13% of whole total phenol contents.
Embodiment 5: the preparation of Rhizome of Grass leaf Sweelflag total phenylpropanoid sheet
Rhizome of Grass leaf Sweelflag total phenylpropanoid extract 100g
Starch 100g
Said components mixes, and it is an amount of to add talcum powder, is pressed into 1000.
Embodiment 6: the preparation of the total phenol sheet of Rhizome of Grass leaf Sweelflag
The total phenol extraction thing of Rhizome of Grass leaf Sweelflag 100g
Starch 100g
Said components mixes, and it is an amount of to add talcum powder, is pressed into 1000.
Embodiment 7: the preparation of the total phenol compound preparation of Rhizome of Grass leaf Sweelflag
The total phenol extraction thing of Rhizome of Grass leaf Sweelflag 250g
Radix Polygalae total saponins extract 250g
Said components mixes, in the hard gelatin capsule of packing into, and totally 2000 capsules.
Claims (5)
1. the total phenol extraction thing of Rhizome of Grass leaf Sweelflag preparation method, it is characterized in that: select for use the AB-8 macroporous adsorbent resin as the purifying resin, the Rhizome of Grass leaf Sweelflag ethanol extraction is in the sample solution concentration 2～4mg/mL of total phenol amount, absorption flow velocity 3～9BV/h, resin column blade diameter length ratio 1: 5～1: 10, applied sample amount in total phenol amount is 0.5～2.55mg/mL, 1～2 times of resin volume of water elution carries out removal of impurities, the removal of impurities flow velocity is 3～8BV/h, with 4～8 times of resin volumes of 40～90% ethanol elutions, elution flow rate is 5～9BV/h.
2. the total phenol extraction thing of a Rhizome of Grass leaf Sweelflag preparation method is characterized in that: get Rhizome of Grass leaf Sweelflag medicine materical crude slice 1kg, 50% ethanol 10L refluxing extraction 2 times, the each extraction 2 hours, decompression and solvent recovery gets extract, add the water-dispersion dissolving of certain volume, make that the medicinal material amount is 1: 6 with disperseing back liquor capacity ratio; With 5000 rev/mins speed centrifugal 40 minutes again, inclining supernatant liquor; Supernatant liquor is by 10L AB-8 macroporous adsorbent resin, absorption flow velocity 1.0mL/min, the resin column blade diameter length ratio is 1: 10, is 0.96mg/mL in total phenol amount applied sample amount, 1.7 times of resin volumes of water elution carry out removal of impurities, the removal of impurities flow velocity is 2.0mL/min, 5 times of resin volumes of 50% ethanol elution, and elution flow rate is 2.0mL/min, collect 50% ethanol eluate, reclaim solvent, drying under reduced pressure is the total phenol extraction thing of Rhizome of Grass leaf Sweelflag.
3. the total phenol extraction thing of a Rhizome of Grass leaf Sweelflag preparation method is characterized in that: get Rhizome of Grass leaf Sweelflag medicine materical crude slice 1kg, 50% ethanol 15L refluxing extraction 3 times, the each extraction 1.5 hours, decompression and solvent recovery gets extract, add the water-dispersion dissolving of certain volume, make that the medicinal material amount is 1: 7 with disperseing back liquor capacity ratio; With 5000 rev/mins speed centrifugal 40 minutes again, inclining supernatant liquor; Supernatant liquor is by 12L AB-8 macroporous adsorbent resin, absorption flow velocity 1.0mL/min, the resin column blade diameter length ratio is 1: 12, is 1.02mg/mL in total phenol amount applied sample amount, 2 times of resin volumes of water elution carry out removal of impurities, the removal of impurities flow velocity is 1.0mL/min, 5 times of resin volumes of 50% ethanol elution, and elution flow rate is 2.0mL/min, collect 50% ethanol eluate, reclaim solvent, drying under reduced pressure is the total phenol extraction thing of Rhizome of Grass leaf Sweelflag.
4. the total phenol extraction thing of a Rhizome of Grass leaf Sweelflag preparation method is characterized in that: get Rhizome of Grass leaf Sweelflag medicine materical crude slice 1kg, 70% ethanol 12L refluxing extraction 2 times, the each extraction 2 hours, decompression and solvent recovery gets extract, add the water-dispersion dissolving of certain volume, make that the medicinal material amount is 1: 8 with disperseing back liquor capacity ratio; With 5000 rev/mins speed centrifugal 40 minutes again, inclining supernatant liquor; Supernatant liquor is by 12L AB-8 macroporous adsorbent resin, absorption flow velocity 1.0mL/min, the resin column blade diameter length ratio is 1: 10, is 0.96mg/mL in total phenol amount applied sample amount, 2 times of resin volumes of water elution carry out removal of impurities, the removal of impurities flow velocity is 1.0mL/min, 4 times of resin volumes of 90% ethanol elution, and elution flow rate is 2.0mL/min, collect 90% ethanol eluate, reclaim solvent, drying under reduced pressure is the total phenol extraction thing of Rhizome of Grass leaf Sweelflag.
5. the total phenol extraction thing of a Rhizome of Grass leaf Sweelflag preparation method is characterized in that: get Rhizome of Grass leaf Sweelflag medicine materical crude slice 1kg, 70% ethanol 12L refluxing extraction 2 times, the each extraction 2 hours, decompression and solvent recovery gets extract, add the water-dispersion dissolving of certain volume, make that the medicinal material amount is 1: 10 with disperseing back liquor capacity ratio; With 5000 rev/mins speed centrifugal 60 minutes again, inclining supernatant liquor; Supernatant liquor is by 10L AB-8 macroporous adsorbent resin, absorption flow velocity 1.0mL/min, the resin column blade diameter length ratio is 1: 10, is 1.0mg/mL in total phenol amount applied sample amount, 2 times of resin volumes of water elution carry out removal of impurities, the removal of impurities flow velocity is 1.0mL/min, 4 times of resin volumes of 90% ethanol elution, and elution flow rate is 2.0mL/min, collect 50% ethanol eluate, reclaim solvent, drying under reduced pressure is the total phenol extraction thing of Rhizome of Grass leaf Sweelflag.
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| CN102836297B (en) * | 2011-06-24 | 2014-06-18 | 遵义医学院附属医院 | Method for extracting rhizoma acori graminei volatile oil by microwaves |
| CN102499953B (en) * | 2011-11-23 | 2013-06-19 | 天津科技大学 | Process for extracting total phenyl propanoid from paulownia bark of paulownia tomentosa (original variety) by adopting supercritical CO2 fluid technology |
| CN102895439B (en) * | 2012-11-13 | 2014-08-27 | 中国医学科学院药用植物研究所 | Rhizoma acori graminei extract for treating Alzheimer and method for extracting rhizoma acori graminei extract for treating Alzheimer |
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| CN105130762A (en) * | 2015-07-23 | 2015-12-09 | 广州市香雪制药股份有限公司 | Method of separating preparation of volatile components from acorus tatarinowii |
| CN106432160A (en) * | 2015-08-07 | 2017-02-22 | 天津中医药大学 | Phenylpropanoid compound and preparation method and application thereof |
| WO2018208739A1 (en) * | 2017-05-08 | 2018-11-15 | Thomas Cahill | Pharmaceutical compositions comprising caffeic acid chelates |
| CN112552150B (en) * | 2020-12-07 | 2022-02-01 | 山东大学 | Method for preparing asarone monomer based on coordination effect |
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