CN101062078B - Extract of stevia whole stevioside and stevia whole flavone and the preparing method thereof - Google Patents
Extract of stevia whole stevioside and stevia whole flavone and the preparing method thereof Download PDFInfo
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Abstract
The invention discloses a preparing method of sweet chrysanthemum glycosides and chromocor extract from sweet leaf chrysanthemum, which is characterized by the following: comprising sweet chrysanthemum glycosides, labroid glycosides A, cyanidenon, meletin, cyanidenon-7-0-beta-D glycosides, celery element-7-0-beta-D-glycosides, quercetin, meletin-3-0-beta-D-arabinoside, meletin-3-0-[4-0-trans-coffe acyl-alpha-L-isodulcitol-(1-6)-beta-D-arabinoside], derivant and so on; choosing one or several methods from solvent extraction, solvent extraction process, macroreticular absorption resin method, column chromatography, supercritical fluid chromatography, liquid-liquid counter-current partition chromatography and so on; producing extract; counting 5-100%(w/w) of each sweet chrysanthemum glycosides element and chromocor element content in sweet chrysanthemum glycosides and chromocor extract; setting the chromocor element sum in sweet chrysanthemum glycosides, labroid glycosides A, cyanidenon-7-0-beta-D glycosides, quercetin, meletin-3-0-[4-0-trans-coffe acyl-alpha-L-isodulcitol-(1-6)-beta-D-arabinoside] at 5-100%(w/w).
Description
Technical field
The invention belongs to natural drug extracts active ingredients field.Be specifically related to Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract and preparation method, method of quality control and in the application of medicine and field of health care food.
Background technology
In recent years, the problem of people's overnutrition was serious day by day, and the cry of guarding against sugar is more and more higher, and the excessive numerous harm that bring to people of edible sucrose impel scientist constantly to seek the sugared source of development of new.Stevioside in the Folium Stevlae Rebaudianae blade extract and other diterpene glucosides correlative more and more are subjected to consumers in general's favor as the high sugariness of a class, low-calorie natural sweetener product.It not only meets the requirement of modern diet health, and for diabetes, obesity, hypertension, cardiopathic patient provide the sweet taste substitute that does not bring out the state of an illness, is arranged wide development prospect.In recent years, stevioside is described as the world " trisaccharide source " having obtained application widely aspect food, beverage and the medical and health.In June, 1985 China's Ministry of Public Health authorization approval stevioside can use in various food, beverage and medicine.
Folium Stevlae Rebaudianae (Stevia Rebaudiana Bertoni.) belongs to Compositae Stevia herbaceos perennial, the another name Folium hydrangeae strigosae.Folium Stevlae Rebaudianae originates in Paraguay northeast and visits the mountain range with Oman that Brazil borders on, and the local resident drinks the history in existing more than 100 year to it as sweet medicine.The Folium Stevlae Rebaudianae nature and flavor are sweet, flat, are rich in the stevioside constituents in the leaf of Folium Stevlae Rebaudianae, in addition, also contain sterols and flavones ingredient.At present, the preparation method of stevioside constituents all has report both at home and abroad in the Folium Stevlae Rebaudianae, but simultaneously extraction separation prepares stevioside constituents and flavones ingredient in the leaf of Folium Stevlae Rebaudianae, reaches method more than 50% and make stevioside constituents and flavones ingredient content in the Stevia rebaudiana (Bertoni) Hemsl extract, does not appear in the newspapers.
Summary of the invention
The object of the present invention is to provide Flos Chrysanthemi glycoside and flavone extract and preparation method thereof in a kind of leaf of Folium Stevlae Rebaudianae.
Another object of the present invention is to provide in a kind of leaf of Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract as the application in food, medicines and health protection field of sweet ignorant agent, medicine adjuvant and correctives.
Another object of the present invention is to provide in a kind of leaf of Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract to share as preparation or with some hypertension and hyperlipemia medicine separately and makes dosage form, is applied to the medicines and health protection field.
Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract that the present invention proposes are the Flos Chrysanthemi glycoside that extracts from leaf of Folium Stevlae Rebaudianae and the combination of flavonoid active component, and wherein the main compound structure is as follows:
Folium Stevlae Rebaudianae of the present invention, derive from whole plant or any position of Compositae Stevia herbaceos perennial Folium Stevlae Rebaudianae SteviaRebaudiana Bertoni., RUGEN, rhizome, stem, leaf, spica, fruit etc., wherein preferred medical material position is its dried leaves.
Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside of the present invention and flavone extract comprise the composition of active components of Flos Chrysanthemi glycoside and flavonoid, and these composition components mainly comprise stevioside, Lai Baodi glycosides A; Luteolin; Quercetin; luteolin-7-O-β-D-glucoside; apigenin-7-O-beta-D-glucoside; Quercitroside; Quercetin-3-O-β-D-galactoside, Quercetin-3-O-[4-O-is trans-coffee acyl-α-L-rhamnose-(1 → 6)-β-D-galactoside] and derivant etc.
As Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract, wherein the summation of Flos Chrysanthemi glycoside and flavones ingredient percentage composition is 5～100% (w/w), wherein 50～100% (w/w) preferably.
Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside of the present invention and flavone extract except that can be applicable to food industry, also can be used for medical industry and make correctives (correcting different different, the strange taste of some drugs) and adjuvant (tablet, pill, capsule etc.).But and because the stevioside acid and alkali-resistance, in pH4～10 scopes, 100 ℃ of heating down, its chemical constitution does not change, does not decompose yet, does not produce the needed glucose of microorganism, is to belong to non-fermentable material, helps food fresh keeping and medicine mildew-resistant yet.
Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside of the present invention and flavone extract can be made preparation separately or share with other blood pressure lowerings, fat-reducing medicament, are used for hypertension, treatment of diabetes.These preparations have pharmacologically active and the purposes identical or close with flavone extract with above-mentioned Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside.
Among the various active component that Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside of the present invention and flavone extract are contained, most importantly stevioside, Lai Baodi glycosides A and flavones ingredient.
The invention allows for the preparation technology of described Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone 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) macroporous adsorbent resin method; (4) supercritical fluid extraction; (5) column chromatography; (6) liquid-liquid adverse current partography.Wherein preferable methods is the 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 dry blade of Folium Stevlae Rebaudianae 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.) extraction weeding of grease solubility impurity, use the solvent of suitable polarity then, as chloroform, ethyl acetate, acetone, n-butyl alcohol etc., or the mixture of these solvents, extraction obtains Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone 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, 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, D101 etc.Used eluant is water and aqueous ethanol, methanol, acetone etc., wherein 0～100% ethanol preferably.
Preferred Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract resin purification technology are: select for use middle polarity such as AB-8, HPD400 or low pole macroporous adsorbent resin as the purification resin, Folium Stevlae Rebaudianae ethanol extraction sample solution concentration 1: 4～1: 12 (with crude drug amount (g): disperse a milliliter number), absorption flow velocity 2～9BV/h, resin column blade diameter length ratio 1: 5～1: 10, applied sample amount is 100～500mg/mL (in the crude drug amount), 1～4 times of resin volume of 0～40% ethanol elution carries out remove impurity, with 3～6 times of resin volumes of 40～90% ethanol elutions, elution flow rate is 2～9BV/h.
When adopting supercritical fluid extraction to be prepared, can directly extract the Folium Stevlae Rebaudianae 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, macroporous adsorbent resin 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, macroporous adsorbent resin 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.) extraction weeding of grease solubility impurity, use the solvent of suitable polarity then, as chloroform, ethyl acetate, acetone, n-butyl alcohol etc., or the mixture of these solvents, extraction obtains Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract.
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.
Method of quality control of the present invention can comprise one or both in the following content assaying method:
1. total flavones
Precision takes by weighing Quercitroside reference substance an amount of (about 5mg), puts in the 10mL measuring bottle, adds dissolve with methanol and is diluted to scale, shakes up, in contrast product solution.Accurate Quercitroside reference substance solution 0.5,1,2,3, the 3.5ml of drawing adds 5%NaNO in the 25ml measuring bottle
2Solution 1ml shakes up, and places 6min; Add 10%Al (NO then
3)
3Solution 1ml shakes up, and places 6min; Add 4%NaOH solution 10ml again, be settled to scale with rare alcohol dilution at last, shake up, place 15min, and accompany and do blank, measure absorbance in 506nm wavelength place.With Quercitroside reference substance concentration is abscissa, and absorbance is a vertical coordinate, the drawing standard curve.
Precision takes by weighing each 3 parts in dry Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract sample, and every part of 20mg puts in the 10mL measuring bottle, adds 50% ethanol ultrasonic dissolution and is diluted to scale, shakes up.The above-mentioned sample solution 2mL of accurate respectively absorption, Quercitroside reference substance solution 0.5mL, 3.5mL add 5%NaNO in the 25ml measuring bottle
2Solution 1ml shakes up, and places 6min; Add 10%Al (NO then
3)
3Solution 1ml shakes up, and places 6min; Add 4%NaOH solution 10ml again, be settled to scale with rare alcohol dilution at last, shake up, place 15min, measure absorbance in 506nm wavelength place, the external standard two-point method calculates content.
2. stevioside, Lai Baodi glycosides A
Chromatographic condition: chromatographic column Phenomenex Luna NH
2(250mm*4.6mm, 5 μ m); Mobile phase: acetonitrile-water (78: 22); Flow velocity: 1ml/min; Detect wavelength: 210hm; Column temperature: 35 ℃.
Standard curve is drawn: accurate respectively absorption stevioside reference substance solution (concentration is 0.67 μ g/ μ L), Lai Baodi glycosides A reference substance solution (concentration is 0.72 μ g/ μ L), 0,2,4,6,8,10 μ L inject chromatograph of liquid, measure each chromatograph peak-to-peak area, (μ g) is abscissa with the reference substance sample size, the chromatographic peak peak area is a vertical coordinate, the drawing standard curve.
Assay: precision takes by weighing each 3 parts in 3 batches of Folium Stevlae Rebaudianae Flos Chrysanthemi glycosides and flavone extract sample, and every part of about 20mg puts in the 10mL measuring bottle, add 70% acetonitrile ultrasonic dissolution, and be diluted to scale, shake up, as the need testing solution of stevioside, Lai Baodi glycosides A assay.The above-mentioned need testing solution 5 μ L of accurate absorption inject chromatograph of liquid, measure each chromatograph peak-to-peak area, calculate content.
Luteolin-7-O-β-D-glucoside, Quercitroside and Quercetin-3-O-[4-O-trans-coffee acyl-α-L-rhamnose-(1 → 6)-β-D-galactoside]
Chromatographic condition: chromatographic column: Hypersil ODS2 (250mm*4.6mm, 5 μ m); Mobile phase: acetonitrile-0.2% phosphoric acid water gradient elution, 17% acetonitrile～25% acetonitrile (0～30min), 25% acetonitrile～35% acetonitrile (30min～40min); Flow velocity: 1.0mL/min; Detect wavelength: 254nm; Column temperature: 35 ℃.
Standard curve is drawn: accurate respectively draw luteolin-7-O-β-D-glucoside reference substance solution (concentration is 0.082 μ g/ μ L), Quercitroside reference substance solution (concentration is 0.0232 μ g/ μ l) and Quercetin-3-O-[4-O-trans-coffee acyl-α-L-rhamnose-(1 → 6)-β-D-galactoside] (concentration is 0.08 μ g/ μ L) 0,2,4,6,8,10 μ L inject chromatograph of liquid; measure each chromatograph peak-to-peak area; (μ g) is abscissa with the reference substance sample size; the chromatographic peak peak area is a vertical coordinate, the drawing standard curve.
Assay: precision takes by weighing each 3 parts in 3 batches of extract samples; every part of about 20mg; put in the 10mL measuring bottle; add 20% acetonitrile ultrasonic dissolution; and be diluted to scale; shake up, as luteolin-7-O-β-D-glucoside, Quercitroside and Quercetin-3-O-[4-O-trans-coffee acyl-α-L-rhamnose-(1 → 6)-β-D-galactoside] need testing solution measured.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.
The specific embodiment
Embodiment 1: Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract preparation technology
The dry blade 1kg of Folium Stevlae Rebaudianae, 50% ethanol 14L reflux, extract, 3 times, the each extraction 1 hour, decompression and solvent recovery gets extract, adds the aqueous dispersion dissolving, making concentration of aqueous solution is 1: 8 (crude drug amount: disperse the milliliter number), by 4L AB-8 macroporous adsorbent resin, absorption flow velocity 2BV/h, the resin column blade diameter length ratio is 1: 6, applied sample amount is 250mg/mL (in the crude drug amount), 3 times of resin volumes of water elution carry out remove impurity, 5 times of resin volumes of 50% ethanol elution, and elution flow rate is 2BV/h, collect 50% ethanol elution, reclaim solvent, drying under reduced pressure is Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract.Measure that general flavone content is 36% in Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and the flavone extract, wherein luteolin-7-O-β-D-glucoside, Quercitroside and Quercetin-3-O-[4-O-trans-coffee acyl-α-L-rhamnose-(1 → 6)-β-D-galactoside] content of three kinds of compositions is 4%.Stevioside content is 34%, and Lai Baodi glycosides content is 10%.
Embodiment 2: Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract preparation technology
The dry blade 2kg of Folium Stevlae Rebaudianae, 70% ethanol 12L, reflux, extract, 3 times, the each extraction 1.5 hours reclaimed solvent, and extract adds the aqueous dispersion dissolving, making concentration of aqueous solution is 1: 6 (crude drug amount: disperse the milliliter number), by 6L AB-8 macroporous adsorbent resin, absorption flow velocity 4BV/h, the resin column blade diameter length ratio is 1: 7, applied sample amount is 400mg/mL (in the crude drug amount), 2 times of resin volumes of water elution carry out remove impurity, 4 times of resin volumes of 70% ethanol elution, and elution flow rate is 4BV/h, collect 70% ethanol elution, reclaim solvent, drying under reduced pressure is Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract.Measure that general flavone content is 32% in Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and the flavone extract, wherein luteolin-7-O-β-D-glucoside, Quercitroside and Quercetin-3-O-[4-O-trans-coffee acyl-α-L-rhamnose-(1 → 6)-β-D-galactoside] content of three kinds of compositions is 3%.Stevioside content is 30%, and Lai Baodi glycosides content is 7%.
Embodiment 3: Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract preparation technology
The dry blade 10kg of Folium Stevlae Rebaudianae, 70% ethanol 12L reflux, extract, 2 times, the each extraction 2 hours, reclaim solvent, extract adds the aqueous dispersion dissolving, and making concentration of aqueous solution is 1: 4 (crude drug amount: disperse the milliliter number), by the 7LAB-8 macroporous adsorbent resin, absorption flow velocity 4BV/h, the resin column blade diameter length ratio is 1: 9, and applied sample amount is 350mg/mL (in the crude drug amount), and 4 times of resin volumes of water elution carry out remove impurity, 4 times of resin volumes of 90% ethanol elution, elution flow rate is 4BV/h, collects 90% ethanol elution, reclaims solvent, drying under reduced pressure is Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract.Measure that general flavone content is 30% in Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and the flavone extract, wherein luteolin-7-O-β-D-glucoside, Quercitroside and Quercetin-3-O-[4-O-trans-coffee acyl-α-L-rhamnose-(1 → 6)-β-D-galactoside] content of three kinds of compositions is 3%.Stevioside content is 40%, and Lai Baodi glycosides content is 15%.
Embodiment 4: Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract preparation technology
The dry blade 10kg of Folium Stevlae Rebaudianae, 70% ethanol 12L reflux, extract, 2 times, the each extraction 2 hours, reclaim solvent, extract adds the aqueous dispersion dissolving, and making concentration of aqueous solution is 1: 10 (crude drug amount: disperse the milliliter number), by 7L AB-8 macroporous adsorbent resin, absorption flow velocity 4BV/h, the resin column blade diameter length ratio is 1: 4, and applied sample amount is 150mg/mL (in the crude drug amount), and 2 times of resin volumes of water elution carry out remove impurity, 4 times of resin volumes of 70% ethanol elution, elution flow rate is 2.0mL/min, collects 70% ethanol elution, reclaims solvent, drying under reduced pressure is Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract.Measure that general flavone content is 31% in Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and the flavone extract, wherein luteolin-7-O-β-D-glucoside, Quercitroside and Quercetin-3-O-[4-O-trans-coffee acyl-α-L-rhamnose-(1 → 6)-β-D-galactoside] content of three kinds of compositions is 3%.Stevioside content is 30%, and Lai Baodi glycosides content is 12%.
Embodiment 5: the preparation of Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract sheet
Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone 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 Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract compound preparation
Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract 50g
Citrus aurantium total flavone extract 50g
Semen Ginkgo extrac 100g
The said components mix homogeneously, in the hard gelatin capsule of packing into, totally 2000 capsules.
Claims (5)
1. the preparation method of Stevia rebaudiana (Bertoni) Hemsl extract, it is characterized in that: select for use AB-8, HPD400 middle polarity or low pole macroporous adsorbent resin as the purification resin, the Folium Stevlae Rebaudianae ethanol extraction is in crude drug amount g: the sample solution concentration 1: 2～1: 14 of disperseing the milliliter number, absorption flow velocity 2～9BV/h, resin column blade diameter length ratio 1: 5～1: 10, applied sample amount in the crude drug amount is 100～300mg/mL, 1～4 times of resin volume of 0～20% ethanol elution carries out remove impurity, with 3～6 times of resin volumes of 40～90% ethanol elutions, elution flow rate is 2～9BV/h.
2. the preparation method of Stevia rebaudiana (Bertoni) Hemsl extract, it is characterized in that: the dry blade 1kg of Folium Stevlae Rebaudianae, 50% ethanol 14L reflux, extract, 3 times was extracted decompression and solvent recovery 1 hour at every turn, get extract, add aqueous dispersion dissolving, make the concentration of aqueous solution dose of making a living: disperse a milliliter number=1: 8, by 4L AB-8 macroporous adsorbent resin, absorption flow velocity 2BV/h, the resin column blade diameter length ratio is 1: 6, and applied sample amount is counted 250mg/mL with the crude drug amount, and 3 times of resin volumes of water elution carry out remove impurity, 5 times of resin volumes of 50% ethanol elution, elution flow rate is 2BV/h, collects 50% ethanol elution, reclaims solvent, drying under reduced pressure is Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract.
3. the preparation method of Stevia rebaudiana (Bertoni) Hemsl extract, it is characterized in that: the dry blade 2kg of Folium Stevlae Rebaudianae, 70% ethanol 12L, reflux, extract, 3 times was extracted 1.5 hours at every turn, reclaim solvent, extract adds aqueous dispersion dissolving, makes the concentration of aqueous solution dose of making a living: disperse a milliliter number=1: 6, by 6L AB-8 macroporous adsorbent resin, absorption flow velocity 4BV/h, the resin column blade diameter length ratio is 1: 7, and applied sample amount is counted 400mg/mL with the crude drug amount, and 2 times of resin volumes of water elution carry out remove impurity, 4 times of resin volumes of 70% ethanol elution, elution flow rate is 4BV/h, collects 70% ethanol elution, reclaims solvent, drying under reduced pressure is Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract.
4. the preparation method of Stevia rebaudiana (Bertoni) Hemsl extract, it is characterized in that: the dry blade 10kg of Folium Stevlae Rebaudianae, 70% ethanol 12L reflux, extract, 2 times, the each extraction 2 hours reclaimed solvent, and extract adds the aqueous dispersion dissolving, make the concentration of aqueous solution dose of making a living: disperse a milliliter number=1: 4, by 7L AB-8 macroporous adsorbent resin, absorption flow velocity 4BV/h, the resin column blade diameter length ratio is 1: 9, applied sample amount is counted 350mg/mL with the crude drug amount, 4 times of resin volumes of water elution carry out remove impurity, 4 times of resin volumes of 90% ethanol elution, and elution flow rate is 4BV/h, collect 90% ethanol elution, reclaim solvent, drying under reduced pressure is Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract.
5. the preparation method of Stevia rebaudiana (Bertoni) Hemsl extract, it is characterized in that: the dry blade 10kg of Folium Stevlae Rebaudianae, 70% ethanol 12L reflux, extract, 2 times, the each extraction 2 hours reclaimed solvent, and extract adds the aqueous dispersion dissolving, make the concentration of aqueous solution dose of making a living: disperse a milliliter number=1: 10, by 7L AB-8 macroporous adsorbent resin, absorption flow velocity 4BV/h, the resin column blade diameter length ratio is 1: 4, applied sample amount is counted 150mg/mL with the crude drug amount, 2 times of resin volumes of water elution carry out remove impurity, 4 times of resin volumes of 70% ethanol elution, and elution flow rate is 2.0mL/min, collect 70% ethanol elution, reclaim solvent, drying under reduced pressure is Folium Stevlae Rebaudianae Flos Chrysanthemi glycoside and flavone extract.
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| CN2007101113149A CN101062078B (en) | 2007-06-18 | 2007-06-18 | Extract of stevia whole stevioside and stevia whole flavone and the preparing method thereof |
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| CN2007101113149A CN101062078B (en) | 2007-06-18 | 2007-06-18 | Extract of stevia whole stevioside and stevia whole flavone and the preparing method thereof |
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Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL2826386T3 (en) | 2009-06-16 | 2023-03-13 | Sweet Green Fields International Co., Limited | Stevia composition comprising rebaudioside A and D |
| CN103068262A (en) * | 2010-08-23 | 2013-04-24 | 伊比西(北京)植物药物技术有限公司 | Superfine powdered stevia |
| US9578895B2 (en) | 2010-08-23 | 2017-02-28 | Epc (Beijing) Natural Products Co., Ltd. | Rebaudioside A and stevioside compositions |
| US9795156B2 (en) | 2011-03-17 | 2017-10-24 | E.P.C (Beijing) Plant Pharmaceutical Technology Co., Ltd | Rebaudioside B and derivatives |
| CN104098734B (en) * | 2013-04-09 | 2016-08-10 | 江南大学 | The preparation method of phenylboric acid base group modification macroporous resin and the application in rebaudioside A separates with stevioside thereof |
| CN103385903A (en) * | 2013-08-02 | 2013-11-13 | 石任兵 | Stevia rebaudiana phenol extract and application thereof in preparing lipid-lowering products |
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| US10357052B2 (en) | 2014-06-16 | 2019-07-23 | Sweet Green Fields USA LLC | Rebaudioside A and stevioside with improved solubilities |
| US10485256B2 (en) | 2014-06-20 | 2019-11-26 | Sweet Green Fields International Co., Limited | Stevia sweetener with improved solubility with a cyclodextrin |
| CN105362325A (en) * | 2014-09-02 | 2016-03-02 | 天津药物研究院 | Traditional Chinese medicine chrysanthemum indicum extract and preparation method, pharmaceutical composition and application thereof |
| CN107184452A (en) * | 2017-05-13 | 2017-09-22 | 吴杰 | A kind of preparation method, method of testing and the application of tealeaves general flavone |
| CN108997457B (en) * | 2018-07-10 | 2022-03-08 | 宁夏医科大学 | Method for extracting luteolin and quercetin-3-o-beta-glucopyranoside from populus tomentosa leaves |
| CN109293712B (en) | 2018-09-30 | 2022-05-27 | 晨光生物科技集团股份有限公司 | Industrialized utilization method of stevia rebaudiana and stevioside and chlorogenic acid thereof |
| EP3863428A4 (en) * | 2018-10-12 | 2023-03-22 | EPC Natural Products Co., Ltd. | Water soluble flavor compositions, methods of making and methods of use thereof |
| CN109432153B (en) * | 2018-10-25 | 2021-07-27 | 东台市浩瑞生物科技有限公司 | Method for preparing stevia rebaudiana polyphenol by using composite chitosan flocculation method |
| CN113271793A (en) * | 2018-11-26 | 2021-08-17 | 伊比西(北京)植物药物技术有限公司 | Water-soluble flavor composition, preparation method and application method thereof |
| CN112047986B (en) * | 2019-06-06 | 2023-11-17 | 南京宸翔医药研究有限责任公司 | Preparation method of stevioside |
| CN110426475B (en) * | 2019-08-12 | 2022-04-01 | 宿州学院 | Detection method of health-care herbal tea |
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| CN1317540A (en) * | 2000-04-07 | 2001-10-17 | 山名俊彦 | Powdered stevia rebaudiana and enriched liquid and mfg. process thereof |
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