CN101007064B - Isolation and purification method of lotus leaf extract by macroporous resin and its application thereof - Google Patents
Isolation and purification method of lotus leaf extract by macroporous resin and its application thereof Download PDFInfo
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Abstract
The invention provides a process for preparing lotus leaf extract through macroscopic adsorption resin separation and purification, as well as the use of the extract, the process consists of obtaining lotus leaf extract through film separation and purification, charging water to form suspending liquid, macropore resin adsorbing till saturation, water scrubbing the polarity impurity, eluting and concentrating in vacuum. The obtained lotus leaf extract can be used for preparing medicament having functions of fat-reducing, blood fat lowering, bacterium resisting, detoxicating, drug rehabilitating and oxidizing. The extract can be prepared into dose forms of capsules, granules, tablets, oral liquids, syrups, tiny capsules, powders or dripping pills.
Description
Technical field
The present invention relates to a kind of from plant the Green Chemistry preparation method of separation and purification active pharmaceutical ingredients, more specifically relate to a kind of preparation method and purposes that adopts the Lotus Leafextract of macroporous adsorbent resin separation and purification.
Background technology
In China, the lotus leaf aboundresources, cheap and easy to get, drug effect is clear and definite, for rare can intensive processing and large natural medicine-food dual purpose plant resource of comprehensive development and utilization.A large amount of lotus leaves are used as waste and are not used appropriately, and cause the significant wastage of resource, also bring environmental pollution to a certain degree but at source.
Nymphaeaceae plant lotus (Nelumbo nucifera Gaertn), be a kind of medicine food dual purpose plant, at China's the South and the North plantation is arranged all, plantation history reaches more than 3000 year, abound with in Fujian at present, province such as Jiangxi, Hubei, Hunan and Zhejiang, especially white lotus of producing with Jianning, Fujian (building lotus) and the Hunan Dongting Lake Area red lotus (Hunan lotus seeds) of producing is known far and wide at home and abroad.
Lotus leaf (Nelumbo nucifera leaf) is the leaf of lotus, have another name called lotus leaf or lotus root leaf, the plant register of selected ministry of Health of China " being food; be again medicine ", food and the medicine of being widely used as among the people, also often be used for the treatment of obesity and hyperlipidaemia on the clinical medicine with rough machined compound preparation, curative effect is obvious, but less to furtheing investigate such as effective part groups such as lotus flavone and lotus leaf alkaloids.
Traditional medicine thinks, the lotus leaf nature and flavor are cold, has clearing summer-heat and damp, Weight-reducing and lipid-lowering, clears away heart-fire and reduce phlegm and internal heat, stop blooding the activity of Li Shui, can develop protective foodss such as making teabag, beverage, electuary, capsule.Modern pharmacological research shows that the biological activity of compositions such as flavones that lotus leaf is contained and alkaloid is higher, is active pharmaceutical ingredients main in the lotus leaf, and content can reach 1.5% and 0.3% respectively.Lotus flavone and lotus leaf alkaloid have tangible fat-reducing, lipopenicillinase, function [Kong Wenqi etc., " traditional Chinese medicine research and information ", 2005,7 (6): 22-24] such as antibacterial, anti-oxidant.These achievements in research will provide scientific basis for the application of lotus leaf in food, medicine.The preparation method and the purposes of research lotus flavone and lotus leaf alkaloid have certain directive significance for the intensive processing and the series product development of lotus leaf.
Macroporous adsorbent resin is that a class is not with the macroporous structure polymeric sorbent of ion-exchange group, genus polyporus sexual intercourse linked polymer, it is the novel separating medium of a class that behind ion exchange resin, grows up, have that reticulated structure is good, specific surface area is big, stability is high, many characteristics such as regeneration is easy, analysis condition is gentle, life cycle is long, cost saving, be widely used in the separation and purification of natural product and effective components of Chinese medicinal [Feng Tao etc. Guangzhou foodstuffs industry science and technology, 2003,19 (1): 9-11].According to the polarity of functional group, that macroporous adsorbent resin can be divided into is nonpolar, low-pole, Semi-polarity and polarity etc.
The macroporous adsorbent resin separating and purifying technology is a physical property adsorptive power of utilizing resin, selective adsorption enrichment organism from solution, thereby reach the isolating purpose of target substance and impurity, mainly wait and realize by surface adsorption, surface electrical behavior or formation hydrogen bond.The enriching and purifying effect of macroporous adsorbent resin is not only relevant with structure with the physico-chemical property of resin, and is also relevant with factors such as the character of the character of sample, medium and working method.The factor that influences the macroporous resin adsorption performance has the work-ing life of the kind of resin, dynamic adsorption condition, dynamic desorption condition and resin etc.
[" Chinese medicinal materials ", 2005,28 (9): 832-834 such as Cai Weirong etc. [" Jiangsu food and fermentation ", 2002,24 (4): 1-5] and Zhao Jun; " Chinese medicinal materials ", 2003,26 (9): 669-670] once disclosed about adopting macroporous resin D4006 behind the water extraction, NKA-9, though D201 produces a kind of method of lotus leaf medicinal ingredients. this method helps the purity of alkaloid and flavones in the Lotus Leafextract to improve, but because the protein that remains in the Lotus Leafextract, polysaccharide and other biomacromolecule solid substance impurity, separation and purification efficient and the unit resin saturated extent of adsorption of macroporous adsorbent resin to lotus flavone and lotus leaf alkaloid will be had a strong impact on, even cause the non-renewable of macroporous adsorbent resin, thereby have a strong impact on the work-ing life of macroporous adsorbent resin, cause product yield lower, preparation cost is high.
The present invention will provide that a kind of equipment is simple, resin long service life, separation and purification is effective, product yield is high, production cost is low Lotus Leafextract preparation method.
Summary of the invention
One of purpose of the present invention is to provide a kind of preparation method who adopts the Lotus Leafextract of macroporous adsorbent resin separation and purification, this method not only helps the yield and the quality that are further purified, greatly improve product of main Weight-reducing and lipid-lowering active pharmaceutical ingredients such as lotus flavone and lotus leaf alkaloid, and can obviously prolong work-ing life, the reduction preparation cost of macroporous adsorbent resin.
Two of purpose of the present invention is prepared lotus leaf crude extract, the Lotus Leafextract behind the membrane separation purification, the Lotus Leafextract behind the resin separation purification, all can be according to the formulation method of routine, be made into any medicinal preparation for oral administration applicatory clinically with fat-reducing, lipopenicillinase, antibacterial, antiviral or antioxygenation, as: capsule, granule, tablet, oral liquid, syrup, microcapsule, powder, pill or pill etc.
Lotus Leafextract of employing macroporous adsorbent resin of the present invention separation and purification and preparation method thereof is achieved in that with the Lotus Leafextract behind lotus leaf crude extract or the membrane separation purification be raw material, add suitable quantity of water, it is stirred into suspension, make suspension proportion reach 1.1～1.2, it is saturated to adopt the macroporous adsorbent resin enrichment to be adsorbed to then, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, use again 4～8 times of amount of resin 30～60% final concentrations the polar organic solvent aqueous solution with 1～3 times of amount of resin/hour flow velocity (V/V) wash-out target substance, filtrate-0.05～-0.09MPa, under 50～65 ℃ of conditions, through decompression and solvent recovery, the Lotus Leafextract after the separation and purification of vacuum concentration resin.
The preparation method of the Lotus Leafextract of employing macroporous adsorbent resin of the present invention separation and purification, the preparation method of the lotus leaf crude extract of wherein said water extraction is: be raw material with the lotus leaf, adopt the water of 10～30 times of lotus leaf dry weights (W/W), under 50～80 ℃ of conditions, extract 1～3 time, each 1～3 hour, united extraction liquid, filter, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, through decompression and solvent recovery, vacuum concentration becomes the lotus leaf crude extract.
The preparation method of the Lotus Leafextract of employing macroporous adsorbent resin of the present invention separation and purification, the preparation method of the lotus leaf crude extract that wherein said polar organic solvent extracts is: be raw material with the lotus leaf, the final concentration that adopts 10～20 times of lotus leaf dry weights (W/W) is 30～65% the polar organic solvent aqueous solution, under 50 ℃～80 ℃ conditions, extract 1～3 time, each 1～3 hour, united extraction liquid, filter, filtrate-0.05～-0.09MPa, 50～65 ℃ of conditions under, through decompression and solvent recovery, vacuum concentration becomes the lotus leaf crude extract.
Above-mentioned polar organic solvent can be one or more mixed solvents in methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol or the acetone, preferentially selects methyl alcohol or acetone for use.Mainly the extraction effect based on methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol or acetone isopolarity organic solvent is suitable for this, but for other polar organic solvent, the boiling point of methyl alcohol or acetone is lower, energy consumption is littler, can significantly reduce the preparation cost of product.
The preparation method of the Lotus Leafextract of employing macroporous adsorbent resin of the present invention separation and purification, the preparation method of the Lotus Leafextract of wherein said membrane separation for removing impurities is: the lotus leaf crude extract that extracts with water extraction or polar organic solvent is a raw material, add suitable quantity of water, the lotus leaf crude extract is stirred into suspension, make suspension proportion reach 1.05～1.30, under 0.2～1.0MPa,, remove the Lotus Leafextract that promptly gets behind protein and polysaccharide and other macromole solid substance behind the membrane separation purification through membrane separation for removing impurities.
Above-mentioned membrane separation for removing impurities process can be selected the separatory membrane of 10000 molecular weight cut-offs～0.22 μ m membrane pore size for use.
The separation membrane material of above-mentioned membrane separation for removing impurities process can be one or more hybrid films materials in inorganic ceramic film, polysulfone membrane or the polyvinylidene fluoride film, preferentially selects polysulfone membrane or polyvinylidene fluoride film for use.
The preparation method of the Lotus Leafextract of employing macroporous adsorbent resin of the present invention separation and purification, macroporous adsorbent resin can be one or more hybrid resins among HZ801, AB-8, HZ806, D101, DK110, D113, HZ802, HZ803, HZ816, the HZ818, preferentially selects HZ801, HZ802, HZ803, HZ806, HZ816, HZ818 for use.
One of major advantage of preparation technology of the present invention is: the water extraction or the polar organic solvent extraction step that comprise the lotus leaf crude extract, the membrane separation for removing impurities step of Lotus Leafextract, the macroporous adsorbent resin purification procedures of Lotus Leafextract, by membrane separation for removing impurities to Lotus Leafextract, remove biomacromolecule impurity such as protein and polysaccharide, can not only eliminate the blocking action of biomacromolecule impurity to macroporous adsorbent resin, the work-ing life of significant prolongation macroporous adsorbent resin, and can eliminate of the adsorptive capacity influence of biomacromolecule impurity such as protein and polysaccharide to macroporous adsorbent resin, separation and purification efficient and the unit resin saturated extent of adsorption of macroporous adsorbent resin to lotus flavone and lotus leaf alkaloid will obviously be improved, the work-ing life of significant prolongation macroporous adsorbent resin, can greatly improve the yield and the quality of product, significantly reduce the preparation cost of product.
Two of preparation method's of the present invention major advantage is: combination adopts water extraction or polar organic solvent to extract, membrane separation for removing impurities, the method of macroporous adsorbent resin separation and purification, Lotus Leafextract product that can not only the suitability for industrialized production different purity, be used for follow-up fat-reducing, the preparation of lipid-reducing function product, and the lotus leaf waste residue that commercial process produces can be further used for preparing lotus leaf food fibre additive product after simple process, and the concentrated solution behind the membrane separation for removing impurities of macromole impurity such as rich in proteins and polysaccharide can be further used for preparing lotus leaf fertilizer or lotus leaf feedstuff additive product after simple fermentative processing, thereby safety veritably, easy, rationally, realize the total composition comprehensive utilization of lotus leaf and the suitability for industrialized production of series product economically, demonstrate fully the theory of Green Chemistry production and the strategy of recycling economy, it is theoretical novel to have, reasonable in technology, operational safety, technology is easy, economically feasible, advantages of environment protection.
Three of preparation technology's of the present invention major advantage is to adopt modernization of Chinese medicine production technology to extract the Chinese medical extract that the main active pharmaceutical ingredients of lotus leaf is made the current international practice, " three height ", " three is little " and advantages such as " three just " with modern Chinese herbal medicine product, energy adapts to and satisfies modern Chinese medicine clinical application demand, meets the modernization of Chinese medicine and international industry policy that country advocates.
Embodiment
The present invention adopts the preparation method of the Lotus Leafextract of macroporous adsorbent resin separation and purification, the water extraction or the polar organic solvent extraction step that comprise the lotus leaf crude extract, the membrane separation for removing impurities step of Lotus Leafextract, it is characterized in that: with the Lotus Leafextract behind lotus leaf crude extract or the membrane separation purification is raw material, add suitable quantity of water, it is stirred into suspension, make suspension proportion reach 1.1～1.2, it is saturated to adopt the macroporous adsorbent resin enrichment to be adsorbed to then, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, use again 4～8 times of amount of resin 30～60% final concentrations the polar organic solvent aqueous solution with 1～3 times of amount of resin/hour flow velocity (V/V) wash-out target substance, filtrate-0.05～-0.09MPa, under 50～65 ℃ of conditions, through decompression and solvent recovery, the Lotus Leafextract after the separation and purification of vacuum concentration resin.
Above-mentioned macroporous adsorbent resin can be one or more hybrid resins among HZ801, AB-8, HZ806, D101, DK110, D113, HZ802, HZ803, HZ816, the HZ818, preferentially selects HZ801, HZ802, HZ803, HZ806, HZ816, HZ818 for use.
The preparation method of the Lotus Leafextract of employing macroporous adsorbent resin of the present invention separation and purification, the preparation method of the lotus leaf crude extract of wherein said water extraction is: be raw material with the lotus leaf, adopt the water of 10～30 times of lotus leaf dry weights (W/W), under 50～80 ℃ of conditions, extract 1～3 time, each 1～3 hour, united extraction liquid, filter, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, through decompression and solvent recovery, vacuum concentration becomes the lotus leaf crude extract.
The preparation method of the Lotus Leafextract of employing macroporous adsorbent resin of the present invention separation and purification, the preparation method of the lotus leaf crude extract that wherein said polar organic solvent extracts is: be raw material with the lotus leaf, the final concentration that adopts 10～20 times of lotus leaf dry weights (W/W) is 30～65% the polar organic solvent aqueous solution, under 50 ℃～80 ℃ conditions, extract 1～3 time, each 1～3 hour, united extraction liquid, filter, filtrate-0.05～-0.09MPa, 50～65 ℃ of conditions under, through decompression and solvent recovery, vacuum concentration becomes the lotus leaf crude extract.
Above-mentioned polar organic solvent can be one or more mixed solvents in methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol or the acetone, preferentially selects methyl alcohol or acetone for use.Mainly the extraction effect based on methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol or acetone isopolarity organic solvent is suitable for this, but for other polar organic solvent, the boiling point of methyl alcohol or acetone is lower, energy consumption is littler, can significantly reduce the preparation cost of product.
The preparation method of the Lotus Leafextract of employing macroporous adsorbent resin of the present invention separation and purification, the preparation method of the Lotus Leafextract of wherein said membrane separation for removing impurities is: the lotus leaf crude extract that extracts with water extraction or polar organic solvent is a raw material, add suitable quantity of water, the lotus leaf crude extract is stirred into suspension, make suspension proportion reach 1.05～1.30, under 0.2～1.0MPa,, remove the Lotus Leafextract that promptly gets behind protein and polysaccharide and other macromole solid substance behind the membrane separation purification through membrane separation for removing impurities.
Above-mentioned membrane separation for removing impurities process can be selected the separatory membrane of 10000 molecular weight cut-offs～0.22 μ m membrane pore size for use.
The separation membrane material of above-mentioned membrane separation for removing impurities process can be one or more hybrid films materials in inorganic ceramic film, polysulfone membrane or the polyvinylidene fluoride film, preferentially selects polysulfone membrane or polyvinylidene fluoride film for use.
Lotus Leafextract behind lotus leaf crude extract of the present invention, the membrane separation purification, the purposes of the Lotus Leafextract behind the resin separation purification are: the medicinal preparation for oral administration that can have fat-reducing, lipopenicillinase, antibacterial, detoxifcation, drug rehabilitation, antiviral or antioxygenation according to the preparation of the formulation method of routine.Described medicinal preparation for oral administration is: capsule, granule, tablet, oral liquid, syrup, microcapsule, powder, pill or pill etc.
The physical and chemical parameter measuring method of each prepared product of the present invention is as follows:
(1) assay of lotus flavone: adopting high performance liquid chromatography, is contrast with the Quercetin.Chromatographic condition: chromatographic column is selected Waters Nova-Pak C18 post (Φ 3.9 * 15mm, 4 μ m) for use, and pre-column C18 (3.9mm * 15mm), moving phase is methyl alcohol: 0.2% phosphate aqueous solution (45: 55), flow velocity 1.0mL/min, 34 ℃ of column temperatures, detect wavelength 365nm, sample size 20 μ L.The mensuration of sample: get liquid 4mL to be measured (or determinand powder 0.1g, be dissolved in the 4mL solvent), add methyl alcohol 6mL and 12mol/L hydrochloric acid 1mL, shake up rearmounted 80 ℃ of water-bath back hydrolysis 1h.Then hydrolyzed solution is changed in the 50mL volumetric flask, be diluted to scale, as HPLC liquid to be measured with 50% methyl alcohol.Adopting external standard method quantitative in the HPLC mensuration process, is contrast with the Quercetin, and the content of each aglycon after the calculating hydrolysis is unified with the factor 2.51 calculating lotus flavone content.
(2) qualitative judgement of lotus flavone: adopting aluminium salt colorimetry, is contrast with the rutin.Sample solution is diluted to certain multiple, gets 1mL in test tube, add 0.1mL 5%NaNO
2Solution shakes up, and adds 0.1mL 10%Al (NO behind the 5min
3)
3Solution adds 1mL 1mol/L NaOH solution again behind the 6min, mixing, behind the 10min if producing redness or red-purple shows and has lotus flavone, with reagent as blank.
(3) assay of lotus leaf alkaloid: adopting high performance liquid chromatography, is contrast with the Nuciferine.Chromatographic condition is: chromatographic column is selected Waters Nova-Pak C for use
18Post (Φ 3.9 * 15mm, 4 μ m), pre-column C
18(3.9mm * 15mm), moving phase is methyl alcohol: H
2O: diethylamine (75: 25: 0.01, pH value 9.0～10.5), flow velocity 1.0mL/min, 34 ℃ of column temperatures detect wavelength 270nm, sample size 20 μ L.
(4) lotus leaf alkaloid qualitative judgement: adopting the IKI colorimetry, is contrast with the Nuciferine.Sample solution is diluted to certain multiple, gets 1mL in test tube, add 1～2 Wagner's reagent solution, shake up, place 5min, if produce brown or the brown precipitation shows and has lotus leaf alkaloid, with reagent as blank.
(5) measurement of the polysaccharide content: adopting the phenolsulfuric acid method, is contrast with glucose or D-semi-lactosi.
(6) mensuration of protein content: adopting FoLin-phenol method to measure, is contrast with the bSA.
(7) water content adopts quick moisture content tester to measure.
Medicinal preparation for oral administration preparation method of the present invention is as follows:
(1) the spraying drying condition is: feeding liquid concentration 10～20 degree Beaume (60 ℃), 160～250 ℃ of PG-5 type spray-drier inlet temperatures, 60～110 ℃ of temperature outs, centrifugal head operating pressure 1.6～3.0kgf/cm
2
(2) lyophilize condition is: drying temperature-10～-60 ℃, 35～70 ℃ of sublimation temperatures, pressure 0.05～0.18mbar, time of drying 20～40h.
(3) vacuum-drying condition: 45～75 ℃ of drying temperatures, pressure-0.06～-0.095MPa, time of drying 15～50h.
(4) capsule preparation: according to the formulation method of routine, select No. 1 hard capsule, the about 0.30g of the tolerant loadings of every intragranular, on the full-automatic hard capsule filler of NJP-1000B type, carry out the medicinal powder filling, on the flat Autoblisterpackagingmachine of JPB-25IIB type, carry out the aluminium foil Blister Package, can be made into clinical suitable Lotus Leafextract oral capsule.
(5) granule preparation: according to the formulation method of routine, granulation on SHK-220 type efficient wet mixer-granulator is packed on JXD-30A type particle automatic packing machine, can be made into clinical suitable Lotus Leafextract oral granular formulation.
(6) pill preparation: according to the formulation method of routine, adjust the temperature controlling system of the general dripping pill machine of TZDW-1 type, make the water dropper temperature remain on 50～85 ℃, the temperature of refrigerants such as whiteruss remains on-4～40 ℃; Get the glycogelatin of Lotus Leafextract and 1～9 times of weight thereof, place well heater, suspension is made in heating under agitation condition, be placed in the water dropper jar of dripping pill machine, splash in the refrigerant by water dropper, the dripping pill that will be shunk moulding by the outlet of dripping pill machine takes out, and removes the refrigerant on surface, is dried to the agent of Lotus Leafextract oral drip-pill.
Preparation method's of the present invention embodiment is presented below:
Embodiment 1
Producing lotus leaf with Jianning, Fujian Province is raw material, with new lotus leaf washing, dry (air-dry, all can dry or dry), pulverize, cross 16～20 mesh sieves and get Lotus Leaf, the 3.0kg Lotus Leaf is put into extractor, with 40% methanol aqueous solution of 10 times of dry weights of Lotus Leaf (W/W), under 63 ℃ of conditions, extract 3 times each 2 hours, united extraction liquid, filter, filtrate-0.05～-0.09MPa, 50～65 ℃ of conditions under, become the lotus leaf crude extract through decompression and solvent recovery, vacuum concentration.After measured, the extraction yield of lotus flavone is 96.7%, and the extraction yield of lotus leaf alkaloid is 95.9%.
Then, earlier the lotus leaf crude extract is added suitable quantity of water and stir into suspension, make suspension proportion reach 1.05, adopting molecular weight cut-off then is 10000 polysulfone membrane, under 1.0MPa, carry out membrane separation for removing impurities, remove the Lotus Leafextract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the lotus flavone rate of recovery is 95.2%, and the lotus leaf alkaloid rate of recovery is 95.6%, and the protein removal rate is 96.1%, and the polysaccharide clearance is 96.9%.
To the Lotus Leafextract behind the membrane separation purification, adopt the HZ806 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, use 60% aqueous ethanolic solution of 8 times of amount of resin again, with 3 times of amount of resin/hour flow velocity (V/V) wash-out target substance, reclaim the Lotus Leafextract that promptly gets behind the solvent behind the resin separation purification.After measured, the rate of recovery 96.2% of lotus flavone, the rate of recovery 95.8% of lotus leaf alkaloid.
To lotus leaf resin concentration purifying thing, promptly get the Lotus Leafextract product after spray-dried.After measured, extract product water content 4.2%, lotus flavone is 49.6%, lotus leaf alkaloid is 39.8%, lotus flavone total recovery 80.9%, lotus leaf alkaloid total recovery 80.1%.
Embodiment 2
16～20 order Lotus Leaf 2.5kg are put into extractor, 30% methanol aqueous solution with 20 times of dry weights of Lotus Leaf (W/W), under 50 ℃ of conditions, extract 2 times, each 3 hours, united extraction liquid, filter, filtrate-0.05～-0.09MPa, 50～65 ℃ of conditions under, become the lotus leaf crude extract through decompression and solvent recovery, vacuum concentration.After measured, the extraction yield of lotus flavone is 93.4%, and the extraction yield of lotus leaf alkaloid is 92.3%.
The lotus leaf crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.18, adopting molecular weight cut-off then is 60000 polyvinylidene fluoride film, under 0.6MPa, carry out membrane separation for removing impurities, remove the Lotus Leafextract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the lotus flavone rate of recovery is 95.8%, and the lotus leaf alkaloid rate of recovery is 95.9%, and the protein removal rate is 94.6%, and the polysaccharide clearance is 96.2%.
To the Lotus Leafextract behind the membrane separation purification, adopt the HZ801 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 45% aqueous ethanolic solution of using 6 times of amount of resin again with 1 times of amount of resin/hour flow velocity (V/V) wash-out target substance, reclaim the Lotus Leafextract that promptly gets behind the solvent behind the resin separation purification.After measured, the rate of recovery 97.2% of lotus flavone, the rate of recovery 98.3% of lotus leaf alkaloid.
To lotus leaf resin concentration purifying thing, after lyophilize, promptly get the Lotus Leafextract product.After measured, extract product water content 6.6%, lotus flavone is 47.3%, lotus leaf alkaloid is 38.4%, lotus flavone total recovery 80.1%, lotus leaf alkaloid total recovery 82.8%.
Embodiment 3
16～20 order Lotus Leaf 2.5kg are put into extractor, 65% methanol aqueous solution with 17 times of dry weights of Lotus Leaf (W/W), refluxing extraction is 1 hour under 80 ℃ of conditions, filter, filtrate-0.05～-0.09MPa, 50～65 ℃ of conditions under, become the lotus leaf crude extract through decompression and solvent recovery, vacuum concentration.After measured, the extraction yield of lotus flavone is 92.7%, and the extraction yield of lotus leaf alkaloid is 91.2%.
The lotus leaf crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.30, adopting membrane pore size then is the inorganic ceramic film of 0.22 μ m, carries out membrane separation for removing impurities under 0.2MPa, removes the Lotus Leafextract that promptly gets behind the macromole impurity such as protein and polysaccharide behind the membrane separation purification.After measured, the lotus flavone rate of recovery is 96.2%, and the rate of recovery of lotus leaf alkaloid is 96.4%, and the protein removal rate is 93.1%, and the polysaccharide clearance is 95.4%.
To the Lotus Leafextract behind the membrane separation purification, adopt the HZ816 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 30% aqueous ethanolic solution of using 8 times of amount of resin again with 2 times of amount of resin/hour flow velocity (V/V) wash-out target substance, reclaim the Lotus Leafextract that promptly gets behind the solvent behind the resin separation purification.After measured, the rate of recovery 95.4% of lotus flavone, the rate of recovery 95.9% of lotus leaf alkaloid.
To lotus leaf resin concentration purifying thing, after vacuum-drying, promptly get the Lotus Leafextract product.After measured, extract product water content 5.5%, lotus flavone is 48.9%, lotus leaf alkaloid is 39.2%, lotus flavone total recovery 82.6%, lotus leaf alkaloid total recovery 83.5%.
Embodiment 4
Producing lotus leaf with Jianning, Fujian Province is raw material, with new lotus leaf washing, dry (air-dry, all can dry or dry), pulverize, cross 16～20 mesh sieves and get Lotus Leaf, the 3.0kg Lotus Leaf is put into extractor, 65% aqueous ethanolic solution with 20 times of dry weights of Lotus Leaf (W/W), under 80 ℃ of conditions, extracted 1 hour, filter, filtrate-0.05～-0.09MPa, 50～65 ℃ of conditions under, become the lotus leaf crude extract through decompression and solvent recovery, vacuum concentration. after measured, the extraction yield of lotus flavone is 92.1%, and the extraction yield of lotus leaf alkaloid is 90.4%.
Earlier the lotus leaf crude extract is added suitable quantity of water and stir into suspension, make suspension proportion reach 1.15, adopting molecular weight cut-off then is 80000 polyvinylidene fluoride films, under 0.4MPa, carry out membrane separation for removing impurities, remove the Lotus Leafextract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the lotus flavone rate of recovery is 96.0%, and the lotus leaf alkaloid rate of recovery is 96.1%, and the protein removal rate is 94.1%, and the polysaccharide clearance is 95.8%.
To the Lotus Leafextract behind the membrane separation purification, adopt the D101 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 40% methanol aqueous solution of using 4 times of amount of resin again with 2 times of amount of resin/hour flow velocity (V/V) wash-out target substance, reclaim the Lotus Leafextract that promptly gets behind the solvent behind the resin separation purification.After measured, the rate of recovery 96.3% of lotus flavone, the rate of recovery 96.4% of lotus leaf alkaloid.
To lotus leaf resin concentration purifying thing, after lyophilize, promptly get the Lotus Leafextract product.After measured, extract product water content 6.0%, lotus flavone is 47.2%, lotus leaf alkaloid is 39.5%, lotus flavone total recovery 84.6%, lotus leaf alkaloid total recovery 86.4%.
Embodiment 5
16～20 order Lotus Leaf 2.5kg are put into extractor, tap water with 30 times of dry weights of Lotus Leaf (W/W), under 50 ℃ of conditions, extract 2 times, each 2 hours, united extraction liquid, filter, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, become the lotus leaf crude extract through decompression and solvent recovery, vacuum concentration.After measured, the extraction yield of lotus flavone is 92.1%, and the extraction yield of lotus leaf alkaloid is 90.5%.
The lotus leaf crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.30, adopting membrane pore size then is the inorganic ceramic film of 0.22 μ m, under 0.2MPa, carry out membrane separation for removing impurities, remove the Lotus Leafextract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the lotus flavone rate of recovery is 96.3%, and the rate of recovery of lotus leaf alkaloid is 96.2%, and the protein removal rate is 93.4%, and the polysaccharide clearance is 95.3%.
To the Lotus Leafextract behind the membrane separation purification, adopt the DK110 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 30% methanol aqueous solution of using 6 times of amount of resin again with 3 times of amount of resin/hour flow velocity (V/V) wash-out target substance, reclaim the Lotus Leafextract that promptly gets behind the solvent behind the resin separation purification.After measured, the rate of recovery 93.9% of lotus flavone, the rate of recovery 94.7% of lotus leaf alkaloid.
To lotus leaf resin concentration purifying thing, after vacuum-drying, promptly get the Lotus Leafextract product.After measured, extract product water content 4.9%, lotus flavone is 49.2%, lotus leaf alkaloid is 39.4%, lotus flavone total recovery 82.7%, lotus leaf alkaloid total recovery 82.4%.
Embodiment 6
16～20 order Lotus Leaf 2.5kg are put into extractor, 38% aqueous ethanolic solution with 10 times of dry weights of Lotus Leaf (W/W), under 50 ℃ of conditions, extract 3 times, each 3 hours, united extraction liquid, filter, filtrate-0.05～-0.09MPa, 50～65 ℃ of conditions under, become the lotus leaf crude extract through decompression and solvent recovery, vacuum concentration.After measured, the extraction yield of lotus flavone is 94.7%, and the extraction yield of lotus leaf alkaloid is 95.1%.
The lotus leaf crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.05, adopting molecular weight cut-off then is 20000 polysulfone membrane, carries out membrane separation for removing impurities under 0.8MPa, removes the Lotus Leafextract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the lotus flavone rate of recovery is 95.4%, and the lotus leaf alkaloid rate of recovery is 95.9%, and the protein removal rate is 94.8%, and the polysaccharide clearance is 96.4%.
To the Lotus Leafextract behind the membrane separation purification, adopt the AB-8 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 60% methanol aqueous solution of using 6 times of amount of resin again with 1 times of amount of resin/hour flow velocity (V/V) wash-out target substance, reclaim the Lotus Leafextract that promptly gets behind the solvent behind the resin separation purification. after measured, the rate of recovery 95.7% of lotus flavone, the rate of recovery 96.4%. of lotus leaf alkaloid
To lotus leaf resin concentration purifying thing, promptly get the Lotus Leafextract product after spray-dried.After measured, extract product water content 3.7%, lotus flavone is 50.4%, lotus leaf alkaloid is 40.3%, lotus flavone total recovery 82.9%, lotus leaf alkaloid total recovery 82.6%.
Embodiment 7
Producing lotus leaf with Jianning, Fujian Province is raw material, with new lotus leaf washing, dry (air-dry, all can dry or dry), pulverize, cross 16～20 mesh sieves and get Lotus Leaf, the 3.0kg Lotus Leaf is put into extractor, with 30% aqueous acetone solution of 14 times of dry weights of Lotus Leaf (W/W), under 50 ℃ of conditions, extract 3 times each 3 hours, united extraction liquid, filter, filtrate-0.05～-0.09MPa, 50～65 ℃ of conditions under, become the lotus leaf crude extract through decompression and solvent recovery, vacuum concentration.After measured, the extraction yield of lotus flavone is 94.6%, and the extraction yield of lotus leaf alkaloid is 93.8%.
The lotus leaf crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.30, adopting membrane pore size then is the polyvinylidene fluoride film of 0.22 μ m, under 0.3MPa, carry out membrane separation for removing impurities, remove the Lotus Leafextract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the lotus flavone rate of recovery is 96.2%, and the lotus leaf alkaloid rate of recovery is 96.3%, and the protein removal rate is 93.6%, and the polysaccharide clearance is 95.1%.
To the Lotus Leafextract behind the membrane separation purification, adopt the D113 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 30% aqueous acetone solution of using 4 times of amount of resin again with 1 times of amount of resin/hour flow velocity (V/V) wash-out target substance, reclaim the Lotus Leafextract that promptly gets behind the solvent behind the resin separation purification.After measured, the rate of recovery 95.8% of lotus flavone, the rate of recovery 96.1% of lotus leaf alkaloid.
To lotus leaf resin concentration purifying thing, after vacuum-drying, promptly get the Lotus Leafextract product.After measured, extract product water content 5.4%, lotus flavone is 49.1%, lotus leaf alkaloid is 38.7%, lotus flavone total recovery 81.9%, lotus leaf alkaloid total recovery 81.6%.
Embodiment 8
16～20 order Lotus Leaf 2.5kg are put into extractor, 65% aqueous acetone solution with 10 times of dry weights of Lotus Leaf (W/W), refluxing extraction is 2 times under 80 ℃ of conditions, each 1 hour, united extraction liquid, filter, filtrate-0.05～-0.09MPa, 50～65 ℃ of conditions under, become the lotus leaf crude extract through decompression and solvent recovery, vacuum concentration.After measured, the extraction yield of lotus flavone is 93.2%, and the extraction yield of lotus leaf alkaloid is 92.1%.
The lotus leaf crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.21, adopting molecular weight cut-off then is 50000 polysulfone membrane, carries out membrane separation for removing impurities under 0.5MPa, removes the Lotus Leafextract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the lotus flavone rate of recovery is 95.2%, and the lotus leaf alkaloid rate of recovery is 96.2%, and the protein removal rate is 95.0%, and the polysaccharide clearance is 96.1%.
To the Lotus Leafextract behind the membrane separation purification, adopt the HZ802 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 60% aqueous acetone solution of using 4 times of amount of resin again with 2 times of amount of resin/hour flow velocity (V/V) wash-out target substance, reclaim the Lotus Leafextract that promptly gets behind the solvent behind the resin separation purification.After measured, the rate of recovery 93.6% of lotus flavone, the rate of recovery 94.3% of lotus leaf alkaloid.
To lotus leaf resin concentration purifying thing, promptly get the Lotus Leafextract product after spray-dried.After measured, extract product water content 4.0%, lotus flavone is 50.3%, lotus leaf alkaloid is 40.0%, lotus flavone total recovery 80.5%, lotus leaf alkaloid total recovery 81.0%.
Embodiment 9
16～20 order Lotus Leaf 2.5kg are put into extractor, with the tap water of 20 times of dry weights of Lotus Leaf (W/W), under 80 ℃ of conditions, extracted 2 hours, filter, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, become the lotus leaf crude extract through decompression and solvent recovery, vacuum concentration.After measured, the extraction yield of lotus flavone is 90.8%, and the extraction yield of lotus leaf alkaloid is 90.1%.
The lotus leaf crude extract is added suitable quantity of water stir into suspension, make suspension proportion reach 1.16, adopting molecular weight cut-off then is 100000 inorganic ceramic film, under 0.3MPa, carry out membrane separation for removing impurities, remove the Lotus Leafextract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification.After measured, the lotus flavone rate of recovery is 96.0%, and the lotus leaf alkaloid rate of recovery is 96.2%, and the protein removal rate is 94.1%, and the polysaccharide clearance is 95.7%.
To the Lotus Leafextract behind the membrane separation purification, adopt the HZ803 macroporous adsorbent resin, enrichment is adsorbed to saturated, earlier with water (V/V) the flush away polar impurity that is no less than 2 times of amount of resin, 45% aqueous acetone solution of using 8 times of amount of resin again with 3 times of amount of resin/hour flow velocity (V/V) wash-out target substance, reclaim the Lotus Leafextract that promptly gets behind the solvent behind the resin separation purification.After measured, the rate of recovery 93.8% of lotus flavone, the rate of recovery 94.2% of lotus leaf alkaloid.
To lotus leaf resin concentration purifying thing, after lyophilize, promptly get the Lotus Leafextract product.After measured, extract product water content 6.5%, lotus flavone is 46.5%, lotus leaf alkaloid is 39.1%, lotus flavone total recovery 80.3%, lotus leaf alkaloid total recovery 80.0%.
Explanation about Lotus Leafextract purposes of the present invention
The lotus leaf crude extract of embodiment 1 preparation, the Lotus Leafextract behind the membrane separation purification, the Lotus Leafextract behind the resin separation purification are carried out spraying drying respectively, and directly the oral capsule of clinical use is made in filling then, carries out the evaluation of Weight-reducing and lipid-lowering animal pharmacodynamics.
1 material
(body weight 14～16g) is provided by Medical University Of Fujian's animal center female mice.Basal feed is available from Medical University Of Fujian's animal center.High lipid food (basal feed 92.5%, salt 2%, yolk powder 2%, lard 3%, cholesterol 0.5%), this institute makes by oneself.Total cholesterol (TCH) test kit (CHOD-PAP method), Eastern Europe, Zhejiang biotechnology company limited.Triglyceride level (TG) test kit (GPO-PAP method), Eastern Europe, Zhejiang biotechnology company limited.Mda (MDA) test kit (TBA method), bio-engineering research institute is built up in Nanjing.Cholesterol, Shanghai are tried a chemical reagent company limited.
2 experimental techniques
Mouse is divided into A, B, C, D, E group, 10 every group, mouse ad lib and drinking-water at random with the basal feed raising after 5 days.Wherein administration group A, B, C, be respectively the Lotus Leafextract behind lotus leaf crude extract, the membrane separation purification, the Lotus Leafextract behind the resin separation purification, D organizes as high fat positive controls, and the E group is as normal negative control group.A, B, the modeling of C, D group employing high lipid food, the E group is raised with basal feed, and each is organized mouse and all begins administration after raising 7 days, and each medicine all is made into 1g/mL, and dosage is only sky of 0.6ml/, and wherein D group and E group make physiological saline into.Administration is 42 days respectively, plucks eyeball behind the fasting 12h and gets blood and dissection, carries out the mensuration of every biochemical indicator.TCH, TG and MDA all measure with the reagent corresponding box and in strict accordance with specification sheets.Data are carried out with SPSS software, adopt Independent-Sample T Test method that each group data is carried out average, standard error calculating and test of significance.
3 lipopenicillinase animal pharmacodynamic result
Different extracts see Table 1 to the influence of mice plasma total cholesterol, triglyceride level and MDA content.
After the administration 42 days, the cholesterol of high fat positive controls mice plasma has significantly improved 96.7% than normal negative control group, mouse hypercholesterolemia model modeling success under this experiment condition is described. find simultaneously, the mice plasma cholesterol level of administration group A, B, C, D and E all significantly is lower than high fat positive controls, best with A group effect, cholesterol level has significantly reduced 34.3%, B group and C group cholesterol level also significantly reduce more than 25%, illustrate that the Lotus Leafextract sample of different purity all has tangible reducing blood-fat, decreasing cholesterol effect.
(X ± SD) influences n=10 to the Lotus Leafextract of table 1 different purity to mice plasma total cholesterol, triglyceride level and mda content
A: lotus leaf crude extract; B: the Lotus Leafextract behind the membrane separation purification; C: the Lotus Leafextract behind the resin separation purification; D: high fat positive controls; E: normal negative control group.Compare *: P＜0.05 with high fat positive controls; *: P＜0.01; * *: P＜0.001.
Above embodiment is intended to further describe for example the present invention, rather than limits the present invention by any way.
The present invention is novel, and technology is simple, the extraction efficiency height, and production cost is low, meets the modernization of Chinese medicine and international industry policy that country advocates, has bigger dissemination.
Claims (9)
1. preparation method who adopts the Lotus Leafextract of macroporous adsorbent resin separation and purification, the polar organic solvent that comprises the lotus leaf crude extract extracts or the water extraction step, the membrane separation for removing impurities step of Lotus Leafextract, it is characterized in that: with the Lotus Leafextract behind the membrane separation purification is raw material, add suitable quantity of water, it is stirred into suspension, it is saturated to adopt the macroporous adsorbent resin enrichment to be adsorbed to then, wash depolarization impurity earlier with water, use polar organic solvent aqueous solution wash-out target substance again, filtrate is through decompression and solvent recovery, Lotus Leafextract after the separation and purification of vacuum concentration resin;
Described membrane separation for removing impurities method is: the lotus leaf crude extract with polar organic solvent extraction or water extraction is a raw material, add water, the lotus leaf crude extract is stirred into suspension, make suspension proportion reach 1.05～1.30, under 0.2～1.0MPa,, remove the Lotus Leafextract that promptly gets behind protein and polysaccharide and other macromole impurity behind the membrane separation purification through membrane separation for removing impurities;
Described macroporous adsorbent resin separation purification method is: with the Lotus Leafextract behind the membrane separation purification is raw material, add suitable quantity of water, it is stirred into suspension, make suspension proportion reach 1.1～1.2, it is saturated to adopt the macroporous adsorbent resin enrichment to be adsorbed to then, earlier with the washing depolarization impurity that is no less than 2 times of resin volumes, 30～60% the polar organic solvent aqueous solution of using 4～8 times of resin volumes again with 1～3 times of resin volume/hour flow velocity wash-out target substance, filtrate-0.05～-0.09MPa, under 50～65 ℃ of conditions, through decompression and solvent recovery, Lotus Leafextract after the separation and purification of vacuum concentration resin;
Described membrane separation for removing impurities process is selected the separatory membrane of 10000 molecular weight cut-offs～0.22 μ m membrane pore size for use.
2. the preparation method of the Lotus Leafextract of employing macroporous adsorbent resin according to claim 1 separation and purification, it is characterized in that: the preparation method of the lotus leaf crude extract that described polar organic solvent extracts is: be raw material with the lotus leaf, adopting mass ratio is 30～65% the polar organic solvent aqueous solution of 10～20 times of lotus leaf dry weights, under 50～80 ℃ of conditions, extract 1～3 time, each 1～3 hour, united extraction liquid, filter, filtrate-0.05～-0.09MPa, 50～65 ℃ of conditions under, become the lotus leaf crude extract through decompression and solvent recovery, vacuum concentration.
3. the preparation method of the Lotus Leafextract of employing macroporous adsorbent resin according to claim 1 separation and purification, it is characterized in that: the preparation method of the lotus leaf crude extract of described water extraction is: be raw material with the lotus leaf, adopting mass ratio is the water of 10～30 times of lotus leaf dry weights, under 50～80 ℃ of conditions, extract 1～3 time, each 1～3 hour, united extraction liquid filtered, filtrate-0.06～-0.095MPa, 50～80 ℃ of conditions under, become the lotus leaf crude extract through decompression and solvent recovery, vacuum concentration.
4. the preparation method of the Lotus Leafextract of employing macroporous adsorbent resin according to claim 1 and 2 separation and purification is characterized in that: described polar organic solvent is one or more mixed solvents in methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol or the acetone.
5. the preparation method of the Lotus Leafextract of employing macroporous adsorbent resin according to claim 4 separation and purification is characterized in that: described polar organic solvent is selected methyl alcohol or acetone for use.
6. the preparation method of the Lotus Leafextract of employing membrane separation technique according to claim 1 separation and purification is characterized in that: the separation membrane material of membrane separation for removing impurities process is one or more hybrid films materials in inorganic ceramic film, polysulfone membrane or the polyvinylidene fluoride film.
7. the preparation method of the Lotus Leafextract of employing membrane separation technique according to claim 6 separation and purification is characterized in that: the separation membrane material of membrane separation for removing impurities process is polysulfone membrane or polyvinylidene fluoride film.
8. the preparation method of the Lotus Leafextract of employing membrane separation technique according to claim 1 separation and purification is characterized in that: macroporous adsorbent resin is one or more hybrid resins among HZ801, AB-8, HZ806, D101, DK110, D113, HZ802, HZ803, HZ816, the HZ818.
9. the preparation method of the Lotus Leafextract of employing membrane separation technique according to claim 8 separation and purification is characterized in that: macroporous adsorbent resin is one or more hybrid resins among HZ801, HZ802, HZ803, HZ806, HZ816 or the HZ818.
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| CN101139321B (en) * | 2007-09-01 | 2010-12-08 | 福州大学 | Method for separating and purifying nuciferine by employing cationic ion-exchange resin |
| CN101167805B (en) * | 2007-11-14 | 2010-12-29 | 复旦大学 | Use of medicinal composition containing lotus leaves and hypericum japonicum total flavone extraction in preparing medicine for hepatitis B virus |
| CN103285089A (en) * | 2013-05-13 | 2013-09-11 | 张娟 | Preparation process flow of lotus leaf extract |
| CN103479731B (en) * | 2013-09-27 | 2014-12-10 | 徐君 | Method for extracting high-purity lotus leaf flavones |
| CN103479730B (en) * | 2013-09-27 | 2014-11-26 | 周爱琴 | Method for synchronously separating lotus leaf flavone and chlorophyll from fresh lotus leaves |
| CN104844551B (en) * | 2015-04-01 | 2017-05-10 | 齐鲁工业大学 | Method for simultaneously separating and extracting lotus flavones and polysaccharide |
| CN105395614A (en) * | 2015-11-16 | 2016-03-16 | 郎溪县南湖莲藕产销专业合作社 | Lotus leaf alkaloid extracting method and application thereof |
| CN108094704A (en) * | 2018-01-22 | 2018-06-01 | 郑州木村农业科技有限公司 | A kind of livestock culturing Lotus Leafextract feed addictive and its manufacturing method |
| CN110624001A (en) * | 2019-10-25 | 2019-12-31 | 江西省科学院应用化学研究所 | Method for extracting polysaccharide and total flavonoids from camphor tree leaves |
| CN112768014A (en) * | 2021-01-08 | 2021-05-07 | 中国科学院兰州化学物理研究所 | Method for predicting type of macroporous adsorption resin for polysaccharide separation |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1431205A (en) * | 2002-01-11 | 2003-07-23 | 华中农业大学 | Extraction agent used for extracting proanthocyanidin from plants and extracting method |
| CN1472207A (en) * | 2003-06-26 | 2004-02-04 | 武汉大学 | Extracting method of polyphenol from lotus root |
| CN1482125A (en) * | 2002-09-13 | 2004-03-17 | 中国科学院武汉植物研究所 | Process for extracting lotus leaf flavone |
-
2006
- 2006-09-23 CN CN200610141954XA patent/CN101007064B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1431205A (en) * | 2002-01-11 | 2003-07-23 | 华中农业大学 | Extraction agent used for extracting proanthocyanidin from plants and extracting method |
| CN1482125A (en) * | 2002-09-13 | 2004-03-17 | 中国科学院武汉植物研究所 | Process for extracting lotus leaf flavone |
| CN1472207A (en) * | 2003-06-26 | 2004-02-04 | 武汉大学 | Extracting method of polyphenol from lotus root |
Non-Patent Citations (3)
| Title |
|---|
| 孔文琦，李严巍.荷叶活性化学成分及药理研究进展.中药研究与信息7 6.2005,7(6),22-25. |
| 孔文琦,李严巍.荷叶活性化学成分及药理研究进展.中药研究与信息7 6.2005,7(6),22-25. * |
| 王伟.精制山荷降脂方提取工艺及药效学的初步研究.第一军医大学-硕士论文.2004,28-41. * |
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