CN101095724A - Technics for extracting lotus leaf flavone - Google Patents
Technics for extracting lotus leaf flavone Download PDFInfo
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- CN101095724A CN101095724A CNA2006100856262A CN200610085626A CN101095724A CN 101095724 A CN101095724 A CN 101095724A CN A2006100856262 A CNA2006100856262 A CN A2006100856262A CN 200610085626 A CN200610085626 A CN 200610085626A CN 101095724 A CN101095724 A CN 101095724A
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- ethanol
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- lotus
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- 229930003944 flavone Natural products 0.000 title claims abstract description 64
- 235000011949 flavones Nutrition 0.000 title claims abstract description 64
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title claims abstract description 63
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 title claims abstract description 60
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 45
- 240000002853 Nelumbo nucifera Species 0.000 title claims abstract description 35
- 235000006508 Nelumbo nucifera Nutrition 0.000 title claims abstract description 35
- 235000006510 Nelumbo pentapetala Nutrition 0.000 title claims abstract description 35
- 229920005989 resin Polymers 0.000 claims abstract description 79
- 239000011347 resin Substances 0.000 claims abstract description 79
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000000605 extraction Methods 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 16
- 238000010521 absorption reaction Methods 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000012528 membrane Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 54
- -1 flavonoid compounds Chemical class 0.000 claims description 38
- 239000012535 impurity Substances 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 27
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 26
- 238000000108 ultra-filtration Methods 0.000 claims description 25
- 238000005516 engineering process Methods 0.000 claims description 22
- 229930003935 flavonoid Natural products 0.000 claims description 17
- 235000017173 flavonoids Nutrition 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 14
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 239000000284 extract Substances 0.000 claims description 10
- 239000003208 petroleum Substances 0.000 claims description 10
- 239000011148 porous material Substances 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 10
- 238000000502 dialysis Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 238000010936 aqueous wash Methods 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- 238000001179 sorption measurement Methods 0.000 claims description 6
- 239000003463 adsorbent Substances 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 5
- 235000013824 polyphenols Nutrition 0.000 claims description 5
- 229920003002 synthetic resin Polymers 0.000 claims description 5
- 239000000057 synthetic resin Substances 0.000 claims description 5
- 229920002521 macromolecule Polymers 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 239000002932 luster Substances 0.000 claims description 2
- 238000001471 micro-filtration Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract 1
- 230000008021 deposition Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 18
- 239000000706 filtrate Substances 0.000 description 12
- 238000010828 elution Methods 0.000 description 5
- 238000010790 dilution Methods 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- 239000003480 eluent Substances 0.000 description 4
- 150000002213 flavones Chemical class 0.000 description 4
- 230000008719 thickening Effects 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000003916 acid precipitation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 238000000247 postprecipitation Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 208000008589 Obesity Diseases 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 230000002490 cerebral effect Effects 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000001077 hypotensive effect Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000020824 obesity Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to a process of extracting flavone from lotus leaf, which comprises following steps: deposition-extraction-ultra-filtering-micro porous absorption resin column: condensing and dealcoholizing to remove water insoluble foreign matter through depostion, extracting with ligarine to remove fat soluble foreign matter, ultra-filtering to remove water soluble micro-molecular foreign matter, using macroporous absorption column to absorb chromocor selectively, washing and collecting different types of high-purity chromocor. The invention is characterized in that it removes water insoluble foreign matter through deposition, and removes fat soluble foreign matter through extraction with benzinum purificatum, and eliminates water soluble macromolecular foreign matter through ultra filtering membrane, after the processes, the foreign matter is effectively removed from upper column and reduces influence to resin absorption, the absorption performance to chromocor is greatly improved, the absorption volume is increased from 83mg/ ml to 200 mg/ ml. It is suitable for mass production.
Description
Technical field
The present invention relates to a kind of specifically is the preparation technology who extracts total flavones from Folium Nelumbinis from natural plants; particularly extract the Folium Nelumbinis total flavones with precipitation, ultrafiltration, macroporous adsorbent resin technology; stepwise elution is collected the preparation method of dissimilar lotus flavones, and is applicable to large-scale production usefulness.
Background technology
The medicinal basic research of Folium Nelumbinis has confirmed that Folium Nelumbinis has the effect of certain Weight-reducing and lipid-lowering, and the preserved material of Folium Nelumbinis and decoct can directly spread blood vessel, cause the moderate blood pressure lowering, and Folium Nelumbinis has hypotensive effect, but the auxiliary therapy secondary obesity.Contain bioactive ingredients such as chromocor compound, alkaloid, terpenoid in the Folium Nelumbinis.These compositions have great antioxidation, and can remove free radical superfluous in the organism, prevent the peroxidating of organizer inner lipid, improve the immunity of human body body etc., be the natural drug of the treatment cardiovascular and cerebrovascular disease of first-selection.It is reported that flavone compound is for improving the heart, cerebral blood circulation, blood lipid regulation, reducing serum cholesterol etc. has better curative effect.
At present, the lotus flavone production technology mainly contains solvent extraction, alkali extraction and acid precipitation, supercritical CO 2 extraction and resin adsorption method, solvent extraction cost height wherein, and alkali extraction and acid precipitation can only extract the part lotus flavone, and supercritical extraction equipment has high input.Lotus flavone does not also drop into suitability for industrialized production at present, and its technology still is in the research exploratory stage.Existing defective about lotus flavone resin extraction research and patented technology is, with extracting the removal oil-soluble impurities before the macroporous resin adsorption, more do not remove macromole impurity, behind the upper prop, big to resin stain, adsorption capacity is very low, makes that resin absorption is not suitable for using in the suitability for industrialized production, and the product purity that obtains is not good enough yet; Secondly, desorbing does not consider that lotus flavone is the chemical compound that a class formation difference, polarity do not wait, and lotus flavone is not carried out stepwise elution and separates, and it is concrete inadequately to separate roguing.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing the refining lotus flavone of precipitation-extraction-ultrafiltration-absorption with macroporous adsorbent resin multiple techniques; concentrate the dealcoholysis postprecipitation and removed water-insoluble impurity; petroleum ether extraction removes oil-soluble impurities; ultrafilter membrane is removed water-soluble macromolecule impurity; macroporous adsorbent resin selective absorption lotus flavone; stepwise elution is collected the preparation method of dissimilar high-purity flavone, uses the technology of the extraction lotus flavone that large-scale production is provided for pharmaceuticals industry.
Technical scheme of the present invention is to follow these steps to order carry out:
1) with clean new lotus leaf drying, pulverizing, makes Lotus Leaf;
2) with Lotus Leaf and 50～70% ethanol, insert in the lixiviate still by weight 1: 25～30 mixing, be warming up to 70～80 ℃, left standstill 40～60 minutes, make the lotus flavone lixiviating solution;
3) lixiviating solution is inserted the vacuum concentration still, remove the ethanol in the lixiviating solution, when quality of material is 9～11 times of Folium Nelumbinis quality to still, stop to remove ethanol, must concentrate lixiviating solution, refilter and remove the precipitate that concentrates in the lixiviating solution;
4) the concentrated lixiviating solution after will filtering is inserted extraction kettle, adds petroleum ether, stirs, leaves standstill 30 minutes, and oil-soluble impurities is removed in extraction, raffinate;
5) pH value of adjusting raffinate is 8.0～10, filter and remove the alkali insoluble impurities, regulate pH value to previous level, 30～50 times the water that adds used Folium Nelumbinis quality dilutes, and reuse MWCO carries out ultrafiltration at 5～100,000 ultrafilter membranes, remove water-soluble macromolecule impurity, be room temperature during ultrafiltration, pressure is 0.10～0.20MPa, remains at 15～30% o'clock until feed liquid, add water dialysis at least twice, make flavone hyperfiltration treatment liquid;
6) adopting adsorption capacity is 196mg flavone/mL macroporous resin, with its wet method resin column of packing into, after the water washing balance, hyperfiltration treatment liquid is slowly fed resin column, last column flow rate is 4～6BV/h, detects to spill liquid flavone concentration and reach 10 of initial concentration～20% and o'clock stop upper prop;
7) to adsorbing saturated resin column, the pH value that adopts 1.0～2.0 times of resin volumes is 3～5, temperature is 10～15 ℃ water washing, effectively removes impurity; Then with the flavonoid compounds of about 10% the ethanol aqueous wash deresination absorption of 1.0～2.0 times of resin volumes, the flavonoid compounds of purity＞50%; Follow the flavonoid chromocor compound of the middle polarity of adsorbing, get the flavonoid chromocor compound of the middle polarity of purity＞85% with 20～40% ethanol aqueous wash deresinations of 1.0～2.0 times of resin volumes; 45～50% ethanol water eluting of 1.0～2.0 times of resin volumes of reuse, this washing liquid is abandoned; At last, the flavone compound that the polarity of adsorbing in about 60% the ethanol aqueous wash deresination with 1.0～2.0 times of resin volumes is weak, the weak flavone compound of polarity of purity＞50%;
8) will go up step and separate three kinds of lotus flavone compounds stripping liquids that obtain, carry out vacuum concentration respectively, reclaim ethanol, get three kinds of extractum, again three kinds of extractum be carried out vacuum drying, pulverizing respectively, get three kinds of meticulous powder of lotus flavone.
The principle of taking of new lotus leaf is Rhizoma Nelumbinis growth and maturity phase, lovely luster, immaculate Folium Nelumbinis.
Toward step 2) add 50～70% ethanol with weight ratio 1: 15～10 in the filtering residue that makes, set by step 2) temperature, time extract once again, and this extracting solution is added step 2) extracting solution that makes.
The boiling range that adds 2/3～1 times of volume in the concentrated lixiviating solution of step 4) is 60 ℃ a petroleum ether, and extracting twice is removed oil-soluble impurities.
Raffinate is regulated pH 8～9, regulate pH behind the microfiltration to previous level 5.6～5.9, thin up, 30～50 times to used Folium Nelumbinis quality stop to add water, carry out ultrafiltration again, to proceed to feed liquid surplus 15～30% the time when ultrafiltration, adds water dialysis 3～6 times, and the amount of water of at every turn dialysing is 2～4 times of Folium Nelumbinis quality.
Macroporous adsorbent resin is the YZ-006 resin, and resin material is a phenolic aldehyde synthetic resin, specific surface area 400-500m
2/ g, pore volume 0.80～1.0ml/g, average pore size 70～80 dusts, wet true density 1.02～1.12.
Resin behind the eluting flavone compound in the step 7) is added 2.0～4.0 times of resin volumes respectively, and concentration is that 2～5% alkali, acid, 95% ethanol wash, and makes resin recover absorption property.
The advantage that the present invention has: present patent application technology; adopt concentrated dealcoholysis postprecipitation to remove water-insoluble impurity to lixiviating solution; next adopts petroleum ether extraction to remove oil-soluble impurities; and adopt ultrafilter membrane to remove water-soluble macromolecule impurity; through after these pretreatment; upper prop liquid has effectively been removed impurity; alleviated interference to resin absorption; resin is strengthened greatly to the absorbability of flavone; the flavone adsorption capacity increases to the 200mg/ml resin from the 83mg/ml resin, more can adapt to the needs that scale is extracted.The more effective basic law of following separating and purifying technology series connection use of such treatment step promptly precipitates, extracts easily and implements, and the roguing obvious results is preferentially used, and the isolating means of precision such as absorption, chromatography should be used in subsequent technique.The eluting roguing is except washing the post with clear water, and is many according to 45～55% ethanol water eluting section component impurity, the characteristics that flavones content is few, and discarded this section gradient elution component has effectively been removed impurity.Gradient elution obtains, 20%～40% ethanol water eluting component lotus flavone purity＞85%, the purity that is higher than existing patented technology 50%～70%, 10% ethanol water eluting component obtains the strong flavonoid compounds of polarity, purity＞50%, 60% ethanol water eluting component obtains the weak flavone compound of polarity, and purity＞50% all satisfies the requirement of national two kind new medicine raw materials.Extracting method safety of the present invention, easy, reasonable economy, be applicable to large-scale production.
The specific embodiment
Embodiment 1
The washing of the new lotus leaf gathered in the scene, air-dry or oven dry, pulverize, obtain Lotus Leaf; Of the ethanol water lixiviate of 5kg Lotus Leaf with 125L60%, 75 ℃ of temperature, extraction time 40min collects filtrate, and filtering residue extracts once with 60% ethanol of 75L again, merges filtrate twice; The concentrating under reduced pressure lixiviating solution reclaims ethanol to the 50L, filters and removes water-insoluble impurity; Is that 50,000 ultrafilter membranes carry out ultrafiltration with the thickening filtration lixiviating solution with 33.3L petroleum ether (60 ℃ of boiling ranges) extraction two, the ultrafiltration technology condition is: operative temperature room temperature, ultrafiltration pressure 0.15MPa, when ultrafiltration keeps liquid, raffinate is regulated pH9, filter and remove the small amount of precipitate that occurs; After adding the dilution of 100L water, be reduced to about 20L with MWCO, divide respectively to add the dialysis of 20L water for four times, guarantee that flavone thoroughly sees through film, final filtrate volume is 50 times (L/kg) of initial Folium Nelumbinis quality, and flavone transmitance＞90% makes flavone hyperfiltration treatment liquid.
In internal diameter Φ is the 80mm resin column, wet method pack into the height 1000mm the YZ-006 resin (the resin characteristic parameter: material is a phenolic aldehyde synthetic resin, specific surface area 400-500m
2/ g, pore volume 0.80～1.0ml/g, average pore size 70～80 dusts, wet true density 1.02～1.12), after hyperfiltration treatment liquid is regulated about pH to 5.8, slow upper prop, adopt acid pH 4 water washings of low temperature below 15 ℃ of 1.5 times of resin volumes effectively to remove impurity, use 10% ethanol water eluting flavonoid compounds of 1.0～2.0 times of resin volumes then, the vacuum concentration oven dry pulverize dry powder 50.03g, purity＞50%; The back is with the flavonoid chromocor compound of 40% ethanol water eluting middle polarity of 1.5 times of resin volumes, vacuum concentration dry pulverize dry powder 120.21g, purity＞85%; 50% ethanol water eluting of 1.5 times of resin volumes of reuse discards this part eluent, uses the weak flavone compound of 60% ethanol water eluting polarity of 1.5 times of resin volumes at last, the vacuum concentration oven dry pulverize dry powder 16.54g, purity＞50%.
Embodiment 2
The washing of the new lotus leaf gathered in the scene, air-dry or oven dry, pulverize, obtain Lotus Leaf; Of the ethanol water lixiviate of 5kg Lotus Leaf with 150L60%, 70 ℃ of temperature, extraction time 60min collects filtrate, and filtering residue extracts once with 60% ethanol of 50L again, merges filtrate twice; The concentrating under reduced pressure lixiviating solution reclaims ethanol to the 50L, filters and removes water-insoluble impurity; Is that 50,000 ultrafilter membranes carry out ultrafiltration with the thickening filtration lixiviating solution with 35L petroleum ether (60 ℃ of boiling ranges) extraction two, the ultrafiltration technology condition is: operative temperature room temperature, ultrafiltration pressure 0.15MPa, when ultrafiltration keeps liquid, raffinate is regulated pH8, filter and remove the small amount of precipitate that occurs; After adding the dilution of 100L water, be reduced to about 20L with MWCO, respectively add the dialysis of 80L water at twice, guarantee that flavone thoroughly sees through film, final filtrate volume is 50 times (L/kg) of initial Folium Nelumbinis quality, and flavone transmitance＞90% makes flavone hyperfiltration treatment liquid.
In internal diameter Φ is the 80mm resin column, wet method pack into the height 1100mm the YZ-006 resin, after hyperfiltration treatment liquid is regulated about pH to 5.8, slow upper prop, adopt acid pH 4 water washings of low temperature below 15 ℃ of 2.0 times of resin volumes effectively to remove impurity, use 10% ethanol water eluting flavonoid compounds of 2.0 times of resin volumes then, the vacuum concentration oven dry pulverize dry powder 50.92g, purity＞50%; The back is with the flavonoid chromocor compound of 40% ethanol water eluting middle polarity of 2.0 times of resin volumes, vacuum concentration dry pulverize dry powder 120.86g, purity＞85%; 50% ethanol water eluting of 1.0～2.0 times of resin volumes of reuse, discard this part eluent, use the weak flavone compound of 60% ethanol water eluting polarity of 1.0～2.0 times of resin volumes at last, the vacuum concentration oven dry pulverize dry powder 16.32g, purity＞50%.
Embodiment 3
The washing of the new lotus leaf gathered in the scene, air-dry or oven dry, pulverize, obtain Lotus Leaf; Of the ethanol water lixiviate of 5kg Lotus Leaf with 125L50%, 80 ℃ of temperature, extraction time 40min collects filtrate, and filtering residue extracts once with 50% ethanol of 50L again, merges filtrate twice; The concentrating under reduced pressure lixiviating solution reclaims ethanol to the 40L, filters and removes water-insoluble impurity; Is that 50,000 ultrafilter membranes carry out ultrafiltration with the thickening filtration lixiviating solution with 40L petroleum ether (60 ℃ of boiling ranges) extraction two, the ultrafiltration technology condition is: operative temperature room temperature, ultrafiltration pressure 0.15MPa, when ultrafiltration keeps liquid, raffinate is regulated pH9, filter and remove the small amount of precipitate that occurs; After adding the dilution of 100L water, be reduced to about 20L with MWCO, divide respectively to add the dialysis of 20L water for four times, guarantee that flavone thoroughly sees through film, final filtrate volume is 50 times (L/kg) of initial Folium Nelumbinis quality, and flavone transmitance＞90% makes flavone hyperfiltration treatment liquid.
In internal diameter Φ is the 80mm resin column, wet method pack into the height 1000mm the YZ-006 resin (the resin characteristic parameter: material is a phenolic aldehyde synthetic resin, specific surface area 400-500m
2/ g, pore volume 0.80～1.0ml/g, average pore size 70～80 matter, wet true density 1.02～1.12), after hyperfiltration treatment liquid is regulated about pH to 5.8, slow upper prop, adopt acid pH 4 water washings of low temperature below 15 ℃ of 1.5 times of resin volumes effectively to remove impurity, use 10% ethanol water eluting flavonoid compounds of 1.0～2.0 times of resin volumes then, the vacuum concentration oven dry pulverize dry powder 51.20g, purity＞50%; The back is with the flavonoid chromocor compound of 40% ethanol water eluting middle polarity of 1.5 times of resin volumes, vacuum concentration dry pulverize dry powder 117.66g, purity＞85%; 45% ethanol water eluting of 1.5 times of resin volumes of reuse discards this part eluent, uses the weak flavone compound of 60% ethanol water eluting polarity of 1.5 times of resin volumes at last, the vacuum concentration oven dry pulverize dry powder 13.75g, purity＞50%.
Embodiment 4
The washing of the new lotus leaf gathered in the scene, air-dry or oven dry, pulverize, obtain Lotus Leaf; Of the ethanol water lixiviate of 5kg Lotus Leaf with 125L70%, 75 ℃ of temperature, extraction time 40min collects filtrate, and filtering residue extracts once with 70% ethanol of 75L again, merges filtrate twice; The concentrating under reduced pressure lixiviating solution reclaims ethanol to the 50L, filters and removes water-insoluble impurity; Is that 50,000 ultrafilter membranes carry out ultrafiltration with the thickening filtration lixiviating solution with 30L petroleum ether (60 ℃ of boiling ranges) extraction two, the ultrafiltration technology condition is: operative temperature room temperature, ultrafiltration pressure 0.15MPa, when ultrafiltration keeps liquid, raffinate is regulated pH9, filter and remove the small amount of precipitate that occurs; After adding the dilution of 100L water, be reduced to about 20L with MWCO, divide respectively to add the dialysis of 20L water for four times, guarantee that flavone thoroughly sees through film, final filtrate volume is 50 times (L/kg) of initial Folium Nelumbinis quality, and flavone transmitance＞90% makes flavone hyperfiltration treatment liquid.
In internal diameter Φ is the 80mm resin column, wet method pack into the height 1000mm the YZ-006 resin (the resin characteristic parameter: material is a phenolic aldehyde synthetic resin, specific surface area 400-500m
2/ g, pore volume 0.80～1.0ml/g, average pore size 70～80 dusts, wet true density 1.02～1.12), after hyperfiltration treatment liquid is regulated about pH to 5.8, slow upper prop, adopt acid pH 4 water washings of low temperature below 15 ℃ of 1.5 times of resin volumes effectively to remove impurity, use 10% ethanol water eluting flavonoid compounds of 1.0～2.0 times of resin volumes then, the vacuum concentration oven dry pulverize dry powder 48.95g, purity＞50%; The back is with the flavonoid chromocor compound of 40% ethanol water eluting middle polarity of 1.5 times of resin volumes, vacuum concentration dry pulverize dry powder 121.18g, purity＞85%; 50% ethanol water eluting of 1.5 times of resin volumes of reuse discards this part eluent, uses the weak flavone compound of 60% ethanol water eluting polarity of 1.5 times of resin volumes at last, the vacuum concentration oven dry pulverize dry powder 17.11g, purity＞50%.
Resin behind the eluting flavone compound of the present invention adds 2.0～4.0 times of resin volumes respectively, and concentration is that 2～5% alkali, acid, 95% ethanol wash, and makes resin recover absorption property.Make resin regeneration.
Claims (7)
1, a kind of technology of extracting lotus flavone is characterized in that, this method follows these steps to order and carries out:
1) with clean new lotus leaf drying, pulverizing, makes Lotus Leaf;
2) with Lotus Leaf and 50～70% ethanol, insert in the lixiviate still by weight 1: 25～30 mixing, be warming up to 70～80 ℃, left standstill 40～60 minutes, make the lotus flavone lixiviating solution;
3) lixiviating solution is inserted the vacuum concentration still, remove the ethanol in the lixiviating solution, when quality of material is 9～11 times of Folium Nelumbinis quality to still, stop to remove ethanol, must concentrate lixiviating solution, refilter and remove the precipitate that concentrates in the lixiviating solution;
4) the concentrated lixiviating solution after will filtering is inserted extraction kettle, adds petroleum ether, stirs, leaves standstill 30 minutes, and oil-soluble impurities is removed in extraction, raffinate;
5) pH value of adjusting raffinate is 8.0～10, filter and remove the alkali insoluble impurities, regulate pH value to previous level, 30～50 times the water that adds used Folium Nelumbinis quality dilutes, and reuse MWCO carries out ultrafiltration at 5～100,000 ultrafilter membranes, remove water-soluble macromolecule impurity, be room temperature during ultrafiltration, pressure is 0.10～0.20MPa, remains at 15～30% o'clock until feed liquid, add water dialysis at least twice, make flavone hyperfiltration treatment liquid;
6) adopting adsorption capacity is 196mg flavone/mL macroporous resin, with its wet method resin column of packing into, after the water washing balance, hyperfiltration treatment liquid is slowly fed resin column, last column flow rate is 4～6BV/h, detects to spill liquid flavone concentration and reach 10 of initial concentration～20% and o'clock stop upper prop;
7) to adsorbing saturated resin column, the pH value that adopts 1.0～2.0 times of resin volumes is 3～5, temperature is 10～15 ℃ water washing, effectively removes impurity; Then with the flavonoid compounds of about 10% the ethanol aqueous wash deresination absorption of 1.0～2.0 times of resin volumes, the flavonoid compounds of purity＞50%; Follow the flavonoid chromocor compound of the middle polarity of adsorbing, get the flavonoid chromocor compound of the middle polarity of purity＞85% with 20～40% ethanol aqueous wash deresinations of 1.0～2.0 times of resin volumes; 45～50% ethanol water eluting of 1.0～2.0 times of resin volumes of reuse, this washing liquid is abandoned; At last, the flavone compound that the polarity of adsorbing in about 60% the ethanol aqueous wash deresination with 1.0～2.0 times of resin volumes is weak, the weak flavone compound of polarity of purity＞50%;
8) will go up step and separate three kinds of lotus flavone compounds stripping liquids that obtain, carry out vacuum concentration respectively, reclaim ethanol, get three kinds of extractum, again three kinds of extractum be carried out vacuum drying, pulverizing respectively, get three kinds of meticulous powder of lotus flavone.
2, a kind of technology of extracting lotus flavone as claimed in claim 1 is characterized in that, the principle of taking of new lotus leaf is Rhizoma Nelumbinis growth and maturity phase, lovely luster, immaculate Folium Nelumbinis.
3, a kind of technology of extracting lotus flavone as claimed in claim 1, it is characterized in that, toward step 2) add 50～70% ethanol with weight ratio 1: 15～10 in the filtering residue that makes, set by step 2) temperature, time extract once again, and this extracting solution is added step 2) extracting solution that makes.
4, a kind of technology of extracting lotus flavone as claimed in claim 1 is characterized in that, the boiling range that adds 2/3～1 times of volume in the concentrated lixiviating solution of step 4) is 60 ℃ a petroleum ether, and extracting twice is removed oil-soluble impurities.
5, a kind of technology of extracting lotus flavone as claimed in claim 1, it is characterized in that, raffinate is regulated pH8～9, regulate pH behind the microfiltration to previous level 5.6～5.9, thin up, extremely 30～50 times of used Folium Nelumbinis quality stop to add water, carry out ultrafiltration again, to proceed to feed liquid surplus 15～30% the time when ultrafiltration, adds water dialysis 3～6 times, and the amount of water of at every turn dialysing is 2～4 times of Folium Nelumbinis quality.
6, a kind of technology of extracting lotus flavone as claimed in claim 1 is characterized in that, macroporous adsorbent resin is the YZ-006 resin, and resin material is a phenolic aldehyde synthetic resin, specific surface area 400-500m
2/ g, pore volume 0.80～1.0ml/g, average pore size 70～80 dusts, wet true density 1.02～1.12.
7, a kind of technology of extracting lotus flavone as claimed in claim 1, it is characterized in that, resin behind the eluting flavone compound in the step 7) is added 2.0～4.0 times of resin volumes respectively, and concentration is that 2～5% alkali, acid, 95% ethanol wash, and makes resin recover absorption property.
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| CN101366829B (en) * | 2008-09-19 | 2011-03-02 | 杨红鸽 | Method for synchronously extracting flavone and alkaloid from folium nelumbinis |
| CN102764304A (en) * | 2012-08-15 | 2012-11-07 | 泸州品创科技有限公司 | Method for improving non-oxidation rate of flavonoids in lotus leaves |
| CN102764327A (en) * | 2012-08-15 | 2012-11-07 | 四川泰康药业有限公司 | Method for extracting lemon bioflavonoids |
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| CN102875508A (en) * | 2012-10-05 | 2013-01-16 | 南通四海植物精华有限公司 | Process for extracting flavonoids of lotus leaves |
| CN103285088A (en) * | 2013-05-13 | 2013-09-11 | 张娟 | Preparation process of lotus leaf extract |
| CN103285089A (en) * | 2013-05-13 | 2013-09-11 | 张娟 | Preparation process flow of lotus leaf extract |
| CN103479730A (en) * | 2013-09-27 | 2014-01-01 | 周爱琴 | Method for synchronously separating lotus leaf flavone and chlorophyll from fresh lotus leaves |
| CN103479731A (en) * | 2013-09-27 | 2014-01-01 | 徐君 | Method for extracting high-purity lotus leaf flavones |
| CN104194934A (en) * | 2014-08-29 | 2014-12-10 | 杨祝华 | Preparation method of lotus extractum |
| CN106749456A (en) * | 2016-12-20 | 2017-05-31 | 江苏宝莲生物科技股份有限公司 | A kind of method of the separating high-purity Hyperoside from lotus leaf |
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| CN1203067C (en) * | 2002-09-13 | 2005-05-25 | 中国科学院武汉植物研究所 | Process for extracting lotus leaf flavone |
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| CN101366829B (en) * | 2008-09-19 | 2011-03-02 | 杨红鸽 | Method for synchronously extracting flavone and alkaloid from folium nelumbinis |
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| CN102875508A (en) * | 2012-10-05 | 2013-01-16 | 南通四海植物精华有限公司 | Process for extracting flavonoids of lotus leaves |
| CN103285088A (en) * | 2013-05-13 | 2013-09-11 | 张娟 | Preparation process of lotus leaf extract |
| CN103285089A (en) * | 2013-05-13 | 2013-09-11 | 张娟 | Preparation process flow of lotus leaf extract |
| CN103479731A (en) * | 2013-09-27 | 2014-01-01 | 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 |
| CN103479731B (en) * | 2013-09-27 | 2014-12-10 | 徐君 | Method for extracting high-purity lotus leaf flavones |
| CN103479730A (en) * | 2013-09-27 | 2014-01-01 | 周爱琴 | Method for synchronously separating lotus leaf flavone and chlorophyll from fresh lotus leaves |
| CN104194934A (en) * | 2014-08-29 | 2014-12-10 | 杨祝华 | Preparation method of lotus extractum |
| CN104194934B (en) * | 2014-08-29 | 2016-06-22 | 佘延英 | A kind of preparation method of Flos Nelumbinis extractum |
| CN106749456A (en) * | 2016-12-20 | 2017-05-31 | 江苏宝莲生物科技股份有限公司 | A kind of method of the separating high-purity Hyperoside from lotus leaf |
| CN106749456B (en) * | 2016-12-20 | 2019-08-02 | 江苏宝莲生物科技股份有限公司 | A method of the separating high-purity Hyperoside from lotus leaf |
| CN113624897A (en) * | 2021-08-23 | 2021-11-09 | 武汉轻工大学 | Method for measuring phenolic substances in lotus roots |
| CN113624897B (en) * | 2021-08-23 | 2023-09-01 | 武汉轻工大学 | Method for measuring phenols in lotus root |
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