CN101085129A - Acorus gramineus total phenylpropanoid extraction and total phenols extraction and method for preparing simultaneously - Google Patents
Acorus gramineus total phenylpropanoid extraction and total phenols extraction and method for preparing simultaneously 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 Rhizoma Acori Graminei and total phenols extract and preparation method thereof, method of quality control, and in the application of medicine and field of health care food.
Background technology
Rhizoma Acori Graminei is a conventional Chinese medicine, derives from Araeceae Acorus Rhizoma Acori Graminei Acorus tatarinowiiSchott. and belongs to the dry rhizome of other plant together.Traditional Chinese medicine theory thinks that Rhizoma Acori Graminei has the eliminating phlegm of having one's ideas straightened out, the refreshment Fructus Alpiniae Oxyphyllae, hearing-improing and eyesight improving, the effect of removing dampness appetizing and cold expelling eliminating impediment, cure mainly stupor, epilepsy, demented, coronary heart disease, angina pectoris, arrhythmia, apoplexy, dizzy, tinnitus, deaf, atrophic gastritis, cerebral trauma, retarded, cards such as nasal sinusitis, modern pharmacological research shows that Rhizoma Acori Graminei has calmness, anti-frightened, spasmolytic is relievingd asthma, antidepressant, promote memory, blood fat reducing, anticancer, multiple efficacies such as arrhythmia, wide clinical application is in the treatment epilepsy, syncope due to accumulation of phlegm, the calentura coma, forgetful, deafness with qi stagnation, the ambition unhappiness, energy-stagnation stomachache, diseases such as arthralgia chiefly caused by damp pathogen.Mainly contain compositions such as the plain class of phenylpropyl alcohol, phenols, flavonoid, alkaloids, triterpenes in the Rhizoma Acori Graminei.So far, the pharmacologically active of relevant Rhizoma Acori Graminei chemical constituent, application and preparation method, rarely seen have an invention disclosed patent 97106786.4, the preparation method that relates to alkaloids composition in the Rhizoma Acori Graminei is not seen the patent that relates to Rhizoma Acori Graminei total phenylpropanoid extract and total phenols extract and its production and use.
Summary of the invention
The object of the present invention is to provide a kind of Rhizoma Acori Graminei total phenylpropanoid extract and preparation method thereof.
Another object of the present invention is to provide a kind of Rhizoma Acori Graminei total phenols extract and preparation method thereof.
A further object of the present invention is to provide the metallic salt derivant of a kind of Rhizoma Acori Graminei total phenols extract and some alkali or slaine formation.
A further object of the present invention is to provide the metal complex of a kind of Rhizoma Acori Graminei total phenols extract and the formation of some metal ion.
The Rhizoma Acori Graminei 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 YAOSHI Rhizoma Acori Graminei, and wherein the main compound structure is as follows:
The Rhizoma Acori Graminei total phenols extract that the present invention proposes is the combination that contains multiple phenolic active components of therefrom extracting in the YAOSHI Rhizoma Acori Graminei, and wherein the main compound structure is as follows:
Raw material Rhizoma Acori Graminei of the present invention derives from any one plant of Araeceae Acorus.As the raw material that extracts Rhizoma Acori Graminei total phenylpropanoid and total phenols, it can be commercially available Rhizoma Acori Graminei decoction pieces, can be arbitrary position or the whole plant such as stem, leaf, spica, fruit, underground rhizome and root of these plants, the dry rhizome of scape not be taken out at wherein preferred medical material position for these plants yet.Above-mentioned described Rhizoma Acori Graminei comprises crude drug and the decoction pieces of handling without any process of preparing Chinese medicine, also comprises various processed products.
Rhizoma Acori Graminei total phenylpropanoid extract of the present invention, be meant to extract and obtain from any position of above-mentioned arbitrary plant, the compositions 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 compositions of the plain active component of multiple phenylpropyl alcohol from Acorustatarinowii Schott..The plain constituents of these phenylpropyl alcohols mainly comprise beta-Asarone, α-asaricin, Eudesmin, galgravin, veraguensin and are other derivant of parent nucleus with it.
As Rhizoma Acori Graminei 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 Rhizoma Acori Graminei total phenylpropanoid extract of the present invention is contained, compositions such as beta-Asarone, α-asaricin, Eudesmin, galgravin, veraguensin most importantly.As Rhizoma Acori Graminei total phenylpropanoid extract, the content of beta-Asarone, two kinds of compositions of α-asaricin accounts for 5～100% (w/w) of whole total phenylpropanoid content.
Rhizoma Acori Graminei total phenols extract of the present invention, be meant to extract and obtain from any position of above-mentioned arbitrary plant, the compositions that comprises multiple phenolic active components, wherein preferably from Acorus tatarinowiiSchott. dry rhizome, extract and to prepare, contain the compositions of multiple phenolic active components.These phenols components mainly comprise caffeic acid, protocatechuic acid, ferulic acid, vanillic acid and are glucoside compound and other derivant of parent nucleus with it.
As Rhizoma Acori Graminei total phenols extract, the summation of wherein various phenols component percentage compositions is 5～100% (w/w), wherein 50～100% (w/w) preferably.
Rhizoma Acori Graminei total phenols extract of the present invention, can with slaines (as sodium carbonate, potassium carbonate, calcium carbonate, sodium acetate, zinc acetate etc.) such as some alkali (as sodium hydroxide, potassium hydroxide etc.) and sodium salt, potassium salt, calcium salt, zinc salt, form the metallic salt derivant.These derivants have and identical or close pharmacologically active and the purposes of above-mentioned Rhizoma Acori Graminei total phenols extract.
Rhizoma Acori Graminei total phenols extract of the present invention can also form metal complex with metal ions such as sodium, potassium, calcium, ferrum, aluminum, zinc, copper, barium, chromium, strontiums.These metal complexs have and identical or close pharmacologically active or the purposes of above-mentioned Rhizoma Acori Graminei total phenols extract.
Among the various phenolic active components that Rhizoma Acori Graminei total phenols extract of the present invention is contained, most importantly caffeic acid, protocatechuic acid, ferulic acid, vanillic acid, 4-{[(E)-(4-hydroxylbenzoyl) diazenyl] carbonyl}phenol, 3,5,4 '-trihydroxy-6, compositions such as 7-methylene-dioxy flavone, emodin.As Rhizoma Acori Graminei total phenols extract, the content of caffeic acid, protocatechuic acid composition accounts for 5～100% (w/w) of whole total phenol contents.
The invention allows for the preparation technology of described Rhizoma Acori Graminei total phenylpropanoid extract and total phenols extract, it can adopt following any one method, or the combination in any of these methods is prepared: (1) solvent extraction method; (2) solvent extraction; (3) sedimentation method; (4) supercritical fluid extraction; (5) column chromatography; (6) liquid-liquid adverse current partography.Wherein preferable methods is the sedimentation 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, merceration, percolation, microwave extraction, high pressure extract etc.
Preferred extraction process is: the Rhizoma Acori Graminei medical material adds 30～90% ethanol, and reflux, extract, 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, sucking filtration, ultrafiltration, filter pressing, use or do not use following any one clarifier or its combination: the precipitate with ethanol agent, gelatin, Kaolin, various resins, Polyethylene 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, spray drying, lyophilization etc.
When adopting solvent extraction to be prepared, general earlier extract mixture being suspended from the water, then with low polar esters, alkanes or ether solvent (as petroleum ether, ether, hexane, gasoline, ethyl acetate etc.) chloroform, ethyl acetate or the mixture of these solvents, extraction obtains total phenylpropanoid composition and total phenols composition wherein, obtains total phenylpropanoid extract and total phenols extract.
When adopting the sedimentation method to be prepared, preferred Rhizoma Acori Graminei phenylpropyl alcohol extract preparation technology is: Rhizoma Acori Graminei medical material ethanol extraction adds the distilled water of certain volume, makes that the medical 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, will precipitate with 2～5BV (crude drug amount) petroleum ether 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, alkalescence or faintly acid, 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 eluant is water and aqueous ethanol, methanol, acetone etc., wherein 0～100% ethanol preferably.
Preferred Rhizoma Acori Graminei phenols extract resin purification technology is: select for use middle polarity such as AB-8, HPD400 or low pole macroporous adsorbent resin as the purification resin, Rhizoma Acori Graminei ethanol extraction sample solution concentration 2～4mg/mL (in the total phenols 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 the total phenols amount), 1～2 times of resin volume of water elution carries out remove impurity, the remove impurity 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.
When adopting supercritical fluid extraction to be prepared, can directly extract the Rhizoma Acori Graminei raw 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 method, solvent extraction, the sedimentation method or supercritical fluid extraction preliminary purification.Used immobile phase can be silica gel, polyamide, aluminium oxide, glucosan (Sephadex series or Sephadex LH-20 series), C-8, C-18, active carbon, cellulose etc., used eluent is different because of the difference of immobile phase, generally the mixed solvent of being made up of water, methanol, ethanol, acetone, chloroform, ethyl acetate, petroleum ether 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 method, solvent extraction, the sedimentation method or supercritical fluid extraction preliminary purification.General earlier extract mixture being suspended from the water, then with low polar esters, alkanes or ether solvent (as petroleum ether, ether, hexane, gasoline, ethyl acetate etc.), chloroform, ethyl acetate, or the mixture of these solvents, extraction obtains total phenylpropanoid composition and total phenols composition wherein, gets total phenylpropanoid extract and total phenols extract.
Rhizoma Acori Graminei total phenylpropanoid extract and total phenols extract can be separately, combination or press the arbitrary proportion compatibility with other any Chinese and western drugs or food, be used to prepare medicine or functional food, prepared medicine or functional food can be capsule, tablet, pill, granule, oral liquid, syrup, electuary, medicated wine, injection, unguentum, powder, beverage etc.
Method of quality control of the present invention can comprise one or both in the following content assaying method:
1. total phenylpropanoid
Precision takes by weighing α-asaricin 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 absolute methanol and it is dissolved fully and is diluted to scale, shakes up, in contrast product solution.Accurate α-asaricin 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 absolute methanol standardize solution, measures absorbance in the 260nm place.With α-asaricin reference substance sampling amount is abscissa, and absorbance is a vertical coordinate, the drawing standard curve.
Precision takes by weighing each 3 parts in Rhizoma Acori Graminei 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 absolute 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-asaricin reference substance solution 2.0, the 4.0mL of drawing puts in the 10mL measuring bottle, and each measuring bottle adds the absolute methanol standardize solution, measures absorbance in the 260nm place.The external standard two-point method calculates content.
2. beta-Asarone, α-asaricin
Chromatographic condition: chromatographic column: kromasil ODS C
18Post (4.6mm * 250mm, 5 μ m); Mobile phase: methanol-water (56: 44); Flow velocity: 1.0mL/min; Detect wavelength: 257nm; Column temperature: room temperature.
Standard 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-asaricin 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-asaricin reference substance storing solution (every 1mL contains α-asaricin 0.08mg).
Accurate respectively beta-Asarone and α-each 2.0mL of asaricin reference substance storing solution, the 0.5mL of drawing puts in the same 10mL volumetric flask, adds the methanol dilution and is settled to scale, shakes up, and promptly gets beta-Asarone, α-asaricin 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 vertical coordinate, and reference substance sample size (μ g) is an abscissa, the drawing standard curve,
Assay: precision takes by weighing each 3 parts in 3 batches of Rhizoma Acori Graminei 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 absolute methanol to scale, shake up, filter with 0.45 μ m microporous filter membrane, as the need testing solution of beta-Asarone and α-asaricin assay.The above-mentioned need testing solution 10 μ L of accurate absorption inject chromatograph of liquid, measure each chromatograph peak-to-peak area, calculate content.
3. total phenols
Precision takes by weighing caffeic 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 caffeic 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% ferric chloride-0.9% potassium ferricyanide (1: 0.9) the mixed solution 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 solution to scale, in the dark place 20min, measure absorbance at 720nm wavelength place.With caffeic acid reference substance sampling amount is abscissa, and absorbance is a vertical coordinate, the drawing standard curve.
Precision takes by weighing each 3 parts in Rhizoma Acori Graminei total phenols extract sample, and every part of 10mg puts in the 25mL measuring bottle, it is an amount of to add 50% alcoholic solution, supersound process 5 minutes is diluted to scale with 50% alcoholic solution, 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, caffeic 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% ferric chloride-0.9% potassium ferricyanide (1: 0.9) the mixed solution 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 solution to scale, in the dark place 20min, measure absorbance at 720nm wavelength place.The external standard two-point method calculates content.
4. caffeic acid, protocatechuic acid
Chromatographic condition: chromatographic column: kromasil ODS C
18Post (4.6mm * 250mm, 5 μ m); Mobile phase: methanol-1% acetic acid aqueous solution (25: 75); Flow velocity: 1.0mL/min; Detect wavelength: 300nm; Column temperature: room temperature.
Standard curve is drawn:
Get caffeic 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 caffeic acid reference substance storing solution (every 1mL contains caffeic 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 caffeic acid and each 2.0mL of protocatechuic acid reference substance storing solution put in the same 10mL volumetric flask, add the methanol dilution and are settled to scale, shake up, and promptly get reference substance solution (every 1mL contains caffeic 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 abscissa with the sample size (μ g) of reference substance, and peak area is a vertical coordinate, the drawing standard curve.
Assay: precision takes by weighing each 3 parts in 3 batches of Rhizoma Acori Graminei total phenols extract samples, and every part of about 10mg puts in the 10mL measuring bottle, it is an amount of to add 50% alcoholic solution, supersound process 5 minutes is diluted to scale with 50% alcoholic solution, 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 chromatograph of liquid, measure each chromatograph peak-to-peak area, calculate content.
The specific embodiment
Embodiment 1: Rhizoma Acori Graminei total phenylpropanoid extract and total phenols extract preparation technology
Get Rhizoma Acori Graminei decoction pieces 1kg, 50% ethanol 10L reflux, extract, 2 times was extracted 2 hours at every turn, and decompression and solvent recovery gets extract, added the aqueous dispersion dissolving of certain volume, made that medical material amount and dispersion back liquor capacity ratio are 1: 6.With 5000 rev/mins speed centrifugal 40 minutes again, inclining supernatant, will precipitate with the 2500mL petroleum ether 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 Rhizoma Acori Graminei total phenylpropanoid extract.Supernatant 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 the total phenols amount), 1.7 times of resin volumes of water elution carry out remove impurity, the remove impurity 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 elution, reclaim solvent, drying under reduced pressure is Rhizoma Acori Graminei total phenols extract.
Total phenylpropanoid content is 72% in the mensuration total phenylpropanoid extract, and wherein the content of beta-Asarone, two kinds of compositions of α-asaricin accounts for 70% of whole total phenylpropanoid content.Total phenol content is 52% in the mensuration total phenols extract, and wherein the content of caffeic acid, two kinds of compositions of protocatechuic acid accounts for 15% of whole total phenol contents.
Embodiment 2: Rhizoma Acori Graminei total phenylpropanoid extract and total phenols extract preparation technology
Get Rhizoma Acori Graminei decoction pieces 1kg, 50% ethanol 15L reflux, extract, 3 times was extracted 1.5 hours at every turn, and decompression and solvent recovery gets extract, added the aqueous dispersion dissolving of certain volume, made that medical material amount and dispersion back liquor capacity ratio are 1: 7.With 5000 rev/mins speed centrifugal 40 minutes again, inclining supernatant, will precipitate with the 3000mL petroleum ether 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 Rhizoma Acori Graminei total phenylpropanoid extract.Supernatant 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 the total phenols amount), 2 times of resin volumes of water elution carry out remove impurity, the remove impurity 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 elution, reclaim solvent, drying under reduced pressure is Rhizoma Acori Graminei total phenols extract.
Total phenylpropanoid content is 73% in the mensuration total phenylpropanoid extract, and wherein the content of beta-Asarone, two kinds of compositions of α-asaricin accounts for 71% of whole total phenylpropanoid content.Total phenol content is 54% in the mensuration total phenols extract, and wherein the content of caffeic acid, two kinds of compositions of protocatechuic acid accounts for 15% of whole total phenol contents.
Embodiment 3: Rhizoma Acori Graminei total phenylpropanoid extract and total phenols extract preparation technology
Get Rhizoma Acori Graminei decoction pieces 1kg, 70% ethanol 12L reflux, extract, 2 times was extracted 2 hours at every turn, and decompression and solvent recovery gets extract, added the aqueous dispersion dissolving of certain volume, made that medical material amount and dispersion back liquor capacity ratio are 1: 8.With 5000 rev/mins speed centrifugal 40 minutes again, inclining supernatant, will precipitate with the 2500nL petroleum ether 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 Rhizoma Acori Graminei total phenylpropanoid extract.Supernatant 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 the total phenols amount), 2 times of resin volumes of water elution carry out remove impurity, the remove impurity 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 elution, reclaim solvent, drying under reduced pressure is Rhizoma Acori Graminei total phenols extract.
Total phenylpropanoid content is 69% in the mensuration total phenylpropanoid extract, and wherein the content of beta-Asarone, two kinds of compositions of α-asaricin accounts for 66% of whole total phenylpropanoid content.Total phenol content is 68% in the mensuration total phenols extract, and wherein the content of caffeic acid, two kinds of compositions of protocatechuic acid accounts for 14% of whole total phenol contents.
Embodiment 4: Rhizoma Acori Graminei total phenylpropanoid extract and total phenols extract preparation technology
Get Rhizoma Acori Graminei decoction pieces 1kg, 70% ethanol 12L reflux, extract, 2 times was extracted 2 hours at every turn, and decompression and solvent recovery gets extract, added the aqueous dispersion dissolving of certain volume, made that medical material amount and dispersion back liquor capacity ratio are 1: 10.With 5000 rev/mins speed centrifugal 60 minutes again, inclining supernatant, will precipitate with the 3000mL petroleum ether 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 Rhizoma Acori Graminei total phenylpropanoid extract.Supernatant 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 the total phenols amount), 2 times of resin volumes of water elution carry out remove impurity, the remove impurity 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 elution, reclaim solvent, drying under reduced pressure is Rhizoma Acori Graminei total phenols extract.
Total phenylpropanoid content is 70% in the mensuration total phenylpropanoid extract, and wherein the content of beta-Asarone, two kinds of compositions of α-asaricin accounts for 68% of whole total phenylpropanoid content.Total phenol content is 56% in the mensuration total phenols extract, and wherein the content of caffeic acid, two kinds of compositions of protocatechuic acid accounts for 13% of whole total phenol contents.
Embodiment 5: the preparation of Rhizoma Acori Graminei total phenylpropanoid sheet
Rhizoma Acori Graminei total phenylpropanoid extract 100g
Starch 100g
The said components mix homogeneously, it is an amount of to add Pulvis Talci, is pressed into 1000.
Embodiment 6: the preparation of Rhizoma Acori Graminei total phenols sheet
Rhizoma Acori Graminei total phenols extract 100g
Starch 100g
The said components mix homogeneously, it is an amount of to add Pulvis Talci, is pressed into 1000.
Embodiment 7: the preparation of Rhizoma Acori Graminei total phenols compound preparation
Rhizoma Acori Graminei total phenols extract 250g
Radix Polygalae total saponins extract 250g
The said components mix homogeneously, in the hard gelatin capsule of packing into, totally 2000 capsules.
Claims (12)
1, a kind of Rhizoma Acori Graminei total phenylpropanoid extract is characterized in that this extract obtains by extracting in the Chinese medicine Rhizoma Acori Graminei, and contains the plain constituents of following phenylpropyl alcohol: beta-Asarone, α-asaricin, Eudesmin, galgravin, veraguensin.
2, a kind of Rhizoma Acori Graminei total phenols extract, it is characterized in that this extract obtains by extracting in the Chinese medicine Rhizoma Acori Graminei, and contain following phenols component: caffeic acid, protocatechuic acid, ferulic acid, vanillic acid, 4-{[(E)-(4-hydroxylbenzoyl) diazenyl] carbonyl] phenol, 3,5,4 '-trihydroxy-6,7-methylene-dioxy flavone, emodin.
3, as claim 1,2 described Rhizoma Acori Graminei total phenylpropanoid extract and total phenols extracts, it is characterized in that Rhizoma Acori Graminei is whole plant or any position of commercially available Rhizoma Acori Graminei decoction pieces or any plant of Araeceae Acorus, RUGEN, rhizome, stem, leaf, spica, fruit etc. also comprise the various processed products through concocting.
4, as claim 1,2 described Rhizoma Acori Graminei total phenylpropanoid extract and total phenols extracts, it is characterized in that above-mentioned total phenylpropanoid constituents content summation is 5～100% by weight in the Rhizoma Acori Graminei total phenylpropanoid extract, above-mentioned total phenols component content summation is 5～100% by weight in the Rhizoma Acori Graminei total phenols extract.
5, as claim 1,2 described Rhizoma Acori Graminei total phenylpropanoid extract and total phenols extracts, it is characterized in that in the Rhizoma Acori Graminei total phenylpropanoid extract in the plain constituents of each phenylpropyl alcohol that it is 5～100% by weight that the content of beta-Asarone, two kinds of compositions of α-asaricin accounts for whole total phenylpropanoid content, in the Rhizoma Acori Graminei total phenols extract in each phenols component the content of caffeic acid, two kinds of compositions of protocatechuic acid to account for whole total phenol contents be 5～100% by weight.
6, Rhizoma Acori Graminei total phenols extract as claimed in claim 2, it is characterized in that above-mentioned phenols component, also comprise with the metallic salt derivant of slaines formation such as sodium salt, potassium salt, calcium salt, zinc salt and with metal ions such as sodium, potassium, calcium, ferrum, aluminum, zinc, copper, barium, chromium, strontiums forming metal complexs.
7, as claim 1～5 described Rhizoma Acori Graminei total phenylpropanoid extract and total phenols extract, it is characterized in that adopting solvent extraction method, solvent extraction, the sedimentation method, macroporous adsorbent resin method, supercritical fluid extraction, column chromatography, liquid-any one methods such as liquid adverse current partography, or the combination in any of these methods is prepared.
8, Rhizoma Acori Graminei total phenylpropanoid extract as claimed in claim 7 and total phenols method for preparing extractive is characterized in that, when these methods of use are prepared, comprise following one or several step:
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, merceration, percolation, microwave extraction, high pressure extract etc.;
Filter: comprise methods such as centrifugal, sucking filtration, ultrafiltration, filter pressing, use or do not use following any clarifier or its combination: the precipitate with ethanol agent, gelatin, Kaolin, various resins, Polyethylene Glycol, poly-second triol, chitosan and natural clarifying agent finished product are as 101 fruit juice clarifiers, ZTC+1 natural clarifying agent etc.;
Concentrate: comprise thin film evaporation, rotary evaporation and decocting and concentrating etc. under normal pressure or the reduced pressure;
Dry: as to comprise vacuum drying, spray drying, lyophilization etc.
9, Rhizoma Acori Graminei total phenylpropanoid method for preparing extractive as claimed in claim 7, it is characterized in that when adopting the sedimentation method to be prepared, selection process is: Rhizoma Acori Graminei medical material ethanol extraction adds the distilled water of certain volume, makes that the medical 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, will precipitate with 2～5BV (crude drug amount) petroleum ether to reflux 2～3 times, each 1.0～2.0 hours, merge petroleum ether extract, decompression low temperature reclaims solvent, and residue is the phenylpropyl alcohol extract.
10, Rhizoma Acori Graminei total phenols method for preparing extractive as claimed in claim 7, it is characterized in that when using the macroporous adsorbent resin method, used macroporous resin can be any types such as nonpolar, low pole, middle polarity, alkalescence or faintly acid, 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 eluant is water and aqueous ethanol, methanol, acetone etc.
11, Rhizoma Acori Graminei total phenols method for preparing extractive as claimed in claim 10, it is characterized in that: select AB-8 for use, middle polarity such as HPD400 or low pole macroporous adsorbent resin are as the purification resin, the Rhizoma Acori Graminei ethanol extraction is in the sample solution concentration 2～4mg/mL of total phenols amount, absorption flow velocity 3～9BV/h, resin column blade diameter length ratio 1: 5～1: 10, applied sample amount in the total phenols amount is 0.5～2.55mg/mL, 1～2 times of resin volume of water elution carries out remove impurity, the remove impurity 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.
12, as the application of claim 1,2,6 described extracts, it is characterized in that, this extract can be pressed the arbitrary proportion compatibility separately or with other any Chinese and western drugs or food, be used to prepare medicine or functional food, prepared medicine or functional food can be capsule, tablet, pill, granule, oral liquid, syrup, electuary, medicated wine, injection, unguentum, powder, beverage etc.
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