CN106674181A - Method for extracting natural flavonoids from malvaceae okra plant - Google Patents
Method for extracting natural flavonoids from malvaceae okra plant Download PDFInfo
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- CN106674181A CN106674181A CN201610979600.6A CN201610979600A CN106674181A CN 106674181 A CN106674181 A CN 106674181A CN 201610979600 A CN201610979600 A CN 201610979600A CN 106674181 A CN106674181 A CN 106674181A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/34—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 3 only
- C07D311/36—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 3 only not hydrogenated in the hetero ring, e.g. isoflavones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
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- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a method for extracting natural flavonoids from a malvaceae okra plant. The method comprises the steps of taking the malvaceae okra plant, namely dried hibiscus manihot flowers as a raw material, cleaning, drying and crushing the raw material; adding ethanol for dissolution, carrying out ultrasonic extraction and vacuum distillation recovery of ethanol and carrying out pretreatment by using a plate-and-frame filter press; and separating, purifying and concentrating a flavonoid solution by using a combined membrane separation technology under certain pressure and carrying out freeze drying to obtain a pure flavonoid product. The method provided by the invention is a method for separating, purifying and concentrating the natural flavonoids by using a combined membrane technology, and has the characteristics of easiness in operation, low energy consumption, low pollution and high purification rate.
Description
Technical field
The invention belongs to food and pharmaceutical technology field, more particularly to one kind are extracted from Malvaceae Flos abelmoschi manihot platymiscium, divided
From, purification, concentrated natural flavone process.
Background technology
At present, the biological flavone purity of the merchandized handling with Semen Ginkgo, Semen sojae atricolor as primary raw material is 40%, due to technique side
Method falls behind, it is impossible to produce high purity product, price is only 1100 yuan/kilogram, and more than 90% high-purity isoflavone value exists
10000 yuan per gram.
Floristics of the China rich in biological flavone enrich, but the exploitation of resource are started late, and extraction process is much
The countries such as day, moral, method, U.S. are lagged behind, product is single, lack the research of depth, utilization rate of raw materials is low, thick product can only be processed
Product, lack the competitiveness of international market.
The refined purifying technique of natural flavone is a lot, mainly has resin extractions, microwave extraction at present, ultrasonic extraction, surpasses
Critical extraction etc..These techniques there are problems that it is a lot, such as：Technical process is loaded down with trivial details, easy polluted product or cause dirt to environment
Dye, low, the not easy to operate response rate, dangerous height, not high purity, high energy consumption, equipment cost height are difficult to realize large-scale production etc..
The content of the invention
It is an object of the invention to overcome the shortcomings of to provide a kind of process is simple, easy to operate, energy consumption in background technology
Low, pollution less, high separations of natural biological flavone, purification, the method for concentration of purification rate, it is a kind of to be carried out using combining membrane technology
Separation, purification, the method for concentrated natural flavone.
In Malvaceae Flos abelmoschi manihot platymiscium, containing substantial amounts of bioactive substance, wherein isoflavone content be up to 5% with
On, than at present in the production of biological isoflavone wide variety of Semen Ginkgo, Semen sojae atricolor equal size are high tens times, be to be currently known plant money
Content highest in source.
Membrane separation technique is a kind of pure physical separation purification technique, and it is big according to the molecular shape and molecular weight of material
It is little, by the selectivity of film through effect, the component of different molecular weight in mixtures of materials is separated, reach target substance
Separation, purification, concentration.This process equipment is simple and convenient to operate, energy consumption is low, product purity is high, will not polluted product, also not
To environment, and continuous production can be capable of achieving.
The technical scheme is that：
A kind of method that pure natural flavone is extracted in Flos abelmoschi manihot platymiscium from Malvaceae, the method step includes：Take Malvaceae
Flos abelmoschi manihot platymiscium-vegetable Furong dry flower through cleaning, drying, is crushed as raw material, is subsequently adding ethanol dissolving, coordinates ultrasound wave
Ethanol is reclaimed in extraction, Jing vacuum distillations, is made after pretreatment of filter press, under a certain pressure, using combination membrance separation skill
Art separates flavonoids solution, purification, concentration, then freeze-dried flavone sterling.
Wherein, described pressure is：0.05-3Mpa.
Described combination membrane separation technique is film, the film of PSPP, the multi-form being made from a different material
Film between combination technique.Molecular size range, molecular shape and the polarity of raw material molecule, group can according to the actual requirements be selected
The different film of synthesis, so that flavone sterling reaches required purification purity.
Film made by the different materials, including:Inorganic (ceramic membrane), polysulfones (PS), cellulose acetate
(CA), polyacrylonitrile (PAN), polyamide (PA), Kynoar (PVDF), polyether sulfone (PES) etc..
The film of the PSPP, including：Ceramic membrane, molecular cut off is 20000~100000dalton；It is super
Filter membrane, molecular cut off is 1000~50000dalton；NF membrane, molecular cut off is 100~1000dalton.
The film of the multi-form, including:Flat Membrane, tubular membrane, hollow-fibre membrane and rolled film.
A kind of refined purification, the method for concentrated natural flavone, the method step includes：
(A), the feed liquid kettle of separating natural flavone is set；The ceramic film component connected with feed liquid kettle is externally provided with feed liquid kettle；
The separator intermediate storage tank that setting is connected with ceramic film component；By the flavone after ethonal extraction, decompression and solvent recovery
Extracting solution is placed in feed liquid kettle, makes feed liquid flow through ceramic film component by pressurization, removes the impurity in solution；Permeation ceramic membrane group
The permeate of part, Jing ceramic film component permeate mouth flows into intermediate storage tank；The solution Jing ceramic membrane concentrated solutions of non-permeation ceramic membrane
Mouth returns feed liquid kettle；Pure water is continuously added in feed liquid kettle, is filtered, so that flavone as far as possible many in feed liquid is through ceramics
Membrane module, improves yield；
(B), the intermediate storage tank of purification natural flavone is set；The ultrafilter membrane being connected with intermediate storage tank is externally provided with intermediate storage tank
Component；The separator intermediate storage tank that setting is connected with hyperfiltration membrane assembly；Feed liquid in intermediate storage tank is made into feed liquid stream by pressurization
Jing hyperfiltration membrane assemblies, remove the non-flavonoid substance in solution；Through the permeate of ultrafilter membrane, during Jing ultrafiltration membrane permeate liquid mouth is flowed into
Between storage tank；Not through the solution of ultrafilter membrane, Jing ultrafilter membrane concentrated solutions mouth returns intermediate storage tank；It is continuously added in intermediate storage tank pure
Water purification, is filtered, so that flavone as far as possible many in feed liquid passes through hyperfiltration membrane assembly, improves yield；
(C), the intermediate storage tank of concentrated natural flavone is set；The NF membrane being connected with intermediate storage tank is externally provided with intermediate storage tank
Component；Make feed liquid flow through nanofiltration membrane component by pressurization the feed liquid in intermediate storage tank, the water in solution is removed as much as possible
Divide and metal ion；Through the permeate of NF membrane, Jing NF membrane outlet discharge system；Not through the solution of NF membrane, Jing receives
Filter membrane concentrated solution mouth returns intermediate storage tank；Jing is constantly circulated, and sterling natural flavone is finally obtained in intermediate storage tank.
(D), the flavonoids solution after concentration is added in manifold vacuum freeze drier carries out lyophilization, obtains solid yellow
Ketone sterling.
The invention has the advantages that：Application combination membrane technology of the present invention is separated, purified, the method for concentrated natural flavone, is had
Easy to operate, energy consumption is low, pollution less, the characteristics of purification rate is high.The present invention breaches traditional handicraft by combined films process
Yoke, it is high-purity isoflavone that purification biological flavone out is refined from Malvaceae Flos abelmoschi manihot platymiscium, current international market pair
The annual requirement of biological flavone is up to 1500 tons, and actual production is only 300 tons, and wherein China's annual production is only 50 tons, therefore this
Invention has larger good effect.
Description of the drawings
Fig. 1 is the production process equipment flow chart of the present invention.
Label declaration in figure：
Feed liquid kettle 1, intermediate storage tank 2,2 ', force (forcing) pump 4,
Inorganic tubular ceramic membrane module 5, polysulfone hollow fibre ultrafilter membrane 6, polyamide rolling NF membrane 7,
Ceramic membrane concentrated solution 8, ceramic membrane permeate 9,
Ultrafilter membrane concentrated solution 10, ultrafiltration membrane permeate liquid 11,
NF membrane concentrated solution 12, NF membrane permeate 13,
Pure water 14.
Specific embodiment
Below in conjunction with the accompanying drawings and embodiment, the invention will be further described.
Embodiment 1：
The present invention extracts the method and step of natural flavone from Malvaceae Flos abelmoschi manihot platymiscium to be included：
A, material Malvaceae Flos abelmoschi manihot platymiscium -1 kilogram of vegetable Furong dry flower is taken, cleaned；
B, by heated-air circulation dryer (model：Nanjing CT-C) dry to moisture content 5%-10%, operation temperature 50-
80℃；
C, the material after drying is put in jet mill (model QWJ), carries out being crushed to 80-120 mesh；
D, the material after dries pulverizing is put in 500L rustless steel vacuum distillation reactors again, and its built-in ultrasound wave is sent out
Raw device (model JTM-1030)；
C, the ethanol solution for adding 20-70%, solid-liquid ratio is：1/5-1/100；
D, rustless steel vacuum distillation reactor is warming up to into 40-60 DEG C；
E, unlatching ultrasound wave, by frequency 30-40KHz is adjusted to, and extracts 20-90 minutes；
Ethanol is reclaimed in F, vacuum distillation；
G and then, do pretreatment with filter press, obtain flavone crude product solution.
As shown in figure 1, the manufacturing technique method of the refined purification natural flavone of the present invention, including：
1), flavone crude product solution is put in rustless steel feed liquid kettle 1；Pressurized pump 4 pressurizes, under 0.05-3Mpa pressure,
Flavonoids solution is filtered using the inorganic tubular ceramic membrane module 5 that molecular cut off is 20000~100000dalton, remove impurity is gone
Matter；
2), enter in intermediate storage tank 2 through the ceramic membrane permeate 9 of inorganic tubular ceramic membrane module 5；Non- permeation parts are returned
Feed back liquid kettle 1；During constantly in feed liquid kettle 1 add pure water 14, with as often as possible eluting flavone；
3), the gathering with 1000~50000dalton of molecular cut off by the flavonoids solution gone after the removal of impurity in intermediate storage tank 2
Sulfone hollow fiber ultrafiltration membrane6, pressurized pump 4 pressurizes, and the purification of flavone is carried out under 0.05-3Mpa pressure, by other molecular weight
Material discharge flavonoids solution, obtain flavonoids solution merely；
4), ultrafiltration membrane permeate liquid 11 enters intermediate storage tank 2 '；
5), ultrafilter membrane concentrated solution 10 is back in intermediate storage tank 2；With the generation of ultrafiltration membrane permeate liquid 11, constantly in
Between add pure water in storage tank 2, as often as possible to exclude non-flavonoid substance；
6), using the polyamide rolling NF membrane 7 of 100~1000dalton of molecular cut off, pressurized pump 4 pressurizes,
Under 0.05-3Mpa pressure, to intermediate storage tank 2 ' in pure flavonoids solution concentrate, discharge most of moisture and small molecule salt；
The discharge system of Jing NF membrane permeate 13, NF membrane concentrated solution 12 is back in intermediate storage tank 2 ', Jing 5-10 minutes, in middle storage
Flavonoids solution must be concentrated in tank 2 '；
7), the flavonoids solution after concentration is added in manifold vacuum freeze drier carries out lyophilization, obtains solid yellow
Ketone sterling.
Wherein, described inorganic tubular ceramic membrane 5, refers to that the film is ceramic membrane, and the material of the film is inorganic material, the film
Form be tubular type.
Described polysulfone hollow fibre ultrafilter membrane 6, refers to that the film is ultrafilter membrane, and the material of the film is polysulfones (PS), the film
Form be doughnut.
Described polyamide rolling NF membrane 7, refers to that the film is NF membrane, and the material of the film is polyamide (PA), the film
Form be rolling.
Embodiment 2：
The present invention extracts the method and step of natural flavone from Malvaceae Flos abelmoschi manihot platymiscium to be included：
A, material Malvaceae Flos abelmoschi manihot platymiscium -1 kilogram of vegetable Furong dry flower is taken, cleaned；
B, by heated-air circulation dryer (model：Nanjing CT-C) dry to moisture content 10%, 70 DEG C of operation temperature；
C, the material after drying is put in jet mill (model QWJ), carries out being crushed to 100 mesh；
D, the material after dries pulverizing is put in 500L rustless steel vacuum distillation reactors again, and its built-in ultrasound wave is sent out
Raw device (model JTM-1030)；
C, the ethanol solution for adding 60%, solid-liquid ratio is：1/20；
D, rustless steel vacuum distillation reactor is warming up to into 60 DEG C；
E, unlatching ultrasound wave, by frequency 30KHz is adjusted to, and is extracted 45 minutes；
Ethanol is reclaimed in F, vacuum distillation；
G and then, do pretreatment with filter press, obtain flavone crude product solution.
As shown in figure 1, the manufacturing technique method of the refined purification natural flavone of the present invention, including：
1), flavone crude product solution is put in rustless steel feed liquid kettle 1；Pressurized pump 4 pressurizes, and under 0.1Mpa pressure, makes
Flavonoids solution is filtered with the inorganic tubular ceramic membrane module 5 that molecular cut off is 80000dalton, the removal of impurity is gone；
2), enter in intermediate storage tank 2 through the ceramic membrane permeate 9 of inorganic tubular ceramic membrane module 5；Non- permeation parts are returned
Feed back liquid kettle 1；During constantly in feed liquid kettle 1 add pure water 14, with as often as possible eluting flavone；
3), by the flavonoids solution gone after the removal of impurity in intermediate storage tank 2 polysulfone hollow of molecular cut off 20000dalton
Fiber ultrafiltration membrane6, pressurized pump 4 pressurizes, and the purification of flavone is carried out under 0.15Mpa pressure, and the material of other molecular weight is arranged
Go out flavonoids solution, obtain flavonoids solution merely；
4), ultrafiltration membrane permeate liquid 11 enters intermediate storage tank 2 '；
5), ultrafilter membrane concentrated solution 10 is back in intermediate storage tank 2；With the generation of ultrafiltration membrane permeate liquid 11, constantly in
Between add pure water in storage tank 2, as often as possible to exclude non-flavonoid substance；
6), using the polyamide rolling NF membrane 7 of molecular cut off 500dalton, pressurized pump 4 pressurizes, in 1.5Mpa
Under pressure, to intermediate storage tank 2 ' in pure flavonoids solution concentrate, discharge most of moisture and small molecule salt；Jing NF membrane is saturating
The discharge system of liquid 13 is crossed, NF membrane concentrated solution 12 is back in intermediate storage tank 2 ', Jing 8 minutes must be concentrated in intermediate storage tank 2 '
Flavonoids solution；
7), the flavonoids solution after concentration is added in manifold vacuum freeze drier carries out lyophilization, obtains solid yellow
Ketone sterling.
Embodiment 3：
The present invention extracts the method and step of natural flavone from Malvaceae Flos abelmoschi manihot platymiscium to be included：
A, material Malvaceae Flos abelmoschi manihot platymiscium -1 kilogram of vegetable Furong dry flower is taken, cleaned；
B, by heated-air circulation dryer (model：Nanjing CT-C) dry to moisture content 10%, 50 DEG C of operation temperature；
C, the material after drying is put in jet mill (model QWJ), carries out being crushed to 120 mesh；
D, the material after dries pulverizing is put in 500L rustless steel vacuum distillation reactors again, and its built-in ultrasound wave is sent out
Raw device (model JTM-1030)；
C, the ethanol solution for adding 65%, solid-liquid ratio is：1/5；
D, rustless steel vacuum distillation reactor is warming up to into 40 DEG C；
E, unlatching ultrasound wave, by frequency 30KHz is adjusted to, and is extracted 40 minutes；
Ethanol is reclaimed in F, vacuum distillation；
G and then, do pretreatment with filter press, obtain flavone crude product solution.
As shown in figure 1, the manufacturing technique method of the refined purification natural flavone of the present invention, including：
1), flavone crude product solution is put in rustless steel feed liquid kettle 1；Pressurized pump 4 pressurizes, and under 0.2Mpa pressure, makes
Flavonoids solution is filtered with the inorganic tubular ceramic membrane module 5 that molecular cut off is 70000dalton, the removal of impurity is gone；
2), enter in intermediate storage tank 2 through the ceramic membrane permeate 9 of inorganic tubular ceramic membrane module 5；Non- permeation parts are returned
Feed back liquid kettle 1；During constantly in feed liquid kettle 1 add pure water 14, with as often as possible eluting flavone；
3), by the flavonoids solution gone after the removal of impurity in intermediate storage tank 2 polyvinylidene fluoride of molecular cut off 20000dalton
Alkene (PVDF) hollow fiber ultrafiltration membrane6, pressurized pump 4 pressurizes, and the purification of flavone is carried out under 0.12Mpa pressure, by other points
The material of son amount discharges flavonoids solution, obtains flavonoids solution merely；
4), ultrafiltration membrane permeate liquid 11 enters intermediate storage tank 2 '；
5), ultrafilter membrane concentrated solution 10 is back in intermediate storage tank 2；With the generation of ultrafiltration membrane permeate liquid 11, constantly in
Between add pure water in storage tank 2, as often as possible to exclude non-flavonoid substance；
6), using the polyamide rolling NF membrane 7 of molecular cut off 400dalton, pressurized pump 4 pressurizes, in 1.0Mpa
Under pressure, to intermediate storage tank 2 ' in pure flavonoids solution concentrate, discharge most of moisture and small molecule salt；Jing NF membrane is saturating
The discharge system of liquid 13 is crossed, NF membrane concentrated solution 12 is back in intermediate storage tank 2 ', Jing 6 minutes must be concentrated in intermediate storage tank 2 '
Flavonoids solution；
7), the flavonoids solution after concentration is added in manifold vacuum freeze drier carries out lyophilization, obtains solid yellow
Ketone sterling.
Embodiment 4：
The present invention extracts the method and step of natural flavone from Malvaceae Flos abelmoschi manihot platymiscium to be included：
A, material Malvaceae Flos abelmoschi manihot platymiscium -1 kilogram of vegetable Furong dry flower is taken, cleaned；
B, by heated-air circulation dryer (model：Nanjing CT-C) dry to moisture content 10%, 80 DEG C of operation temperature；
C, the material after drying is put in jet mill (model QWJ), carries out being crushed to 120 mesh；
D, the material after dries pulverizing is put in 500L rustless steel vacuum distillation reactors again, and its built-in ultrasound wave is sent out
Raw device (model JTM-1030)；
C, the ethanol solution for adding 40%, solid-liquid ratio is：1/50；
D, rustless steel vacuum distillation reactor is warming up to into 60 DEG C；
E, unlatching ultrasound wave, by frequency 35KHz is adjusted to, and is extracted 60 minutes；
Ethanol is reclaimed in F, vacuum distillation；
G and then, do pretreatment with filter press, obtain flavone crude product solution.
As shown in figure 1, the manufacturing technique method of the refined purification natural flavone of the present invention, including：
1), flavone crude product solution is put in rustless steel feed liquid kettle 1；Pressurized pump 4 pressurizes, and under 0.08Mpa pressure, makes
Flavonoids solution is filtered with the inorganic tubular ceramic membrane module 5 that molecular cut off is 50000dalton, the removal of impurity is gone；
2), enter in intermediate storage tank 2 through the ceramic membrane permeate 9 of inorganic tubular ceramic membrane module 5；Non- permeation parts are returned
Feed back liquid kettle 1；During constantly in feed liquid kettle 1 add pure water 14, with as often as possible eluting flavone；
3), by the flavonoids solution gone after the removal of impurity in intermediate storage tank 2 polyacrylonitrile of molecular cut off 20000dalton
(PAN) flat plate ultrafiltration membrane6, pressurized pump 4 pressurizes, and the purification of flavone is carried out under 0.15Mpa pressure, by the thing of other molecular weight
Matter discharges flavonoids solution, obtains flavonoids solution merely；
4), ultrafiltration membrane permeate liquid 11 enters intermediate storage tank 2 '；
5), ultrafilter membrane concentrated solution 10 is back in intermediate storage tank 2；With the generation of ultrafiltration membrane permeate liquid 11, constantly in
Between add pure water in storage tank 2, as often as possible to exclude non-flavonoid substance；
6), using the polyamide rolling NF membrane 7 of molecular cut off 300dalton, pressurized pump 4 pressurizes, in 1.6Mpa
Under pressure, to intermediate storage tank 2 ' in pure flavonoids solution concentrate, discharge most of moisture and small molecule salt；Jing NF membrane is saturating
The discharge system of liquid 13 is crossed, NF membrane concentrated solution 12 is back in intermediate storage tank 2 ', Jing 5 minutes must be concentrated in intermediate storage tank 2 '
Flavonoids solution；
7), the flavonoids solution after concentration is added in manifold vacuum freeze drier carries out lyophilization, obtains solid yellow
Ketone sterling.
Claims (10)
1. a kind of method that pure natural flavone is extracted in Flos abelmoschi manihot platymiscium from Malvaceae, it is characterised in that：The method step includes：
Malvaceae Flos abelmoschi manihot platymiscium-vegetable Furong dry flower is taken as raw material, through cleaning, drying, is crushed, be subsequently adding ethanol dissolving, matched somebody with somebody
Ultrasonic-leaching is closed, Jing vacuum distillations are reclaimed ethanol, made after pretreatment of filter press, under a certain pressure, using combination
Membrane separation technique separates flavonoids solution, purification, concentration, then freeze-dried flavone sterling.
2. the method that pure natural flavone is extracted in a kind of Flos abelmoschi manihot platymiscium from Malvaceae according to claim 1, its feature
It is：Described combination membrane separation technique is film, the film of PSPP, the film of multi-form being made from a different material
Between combination technique；Molecular size range, molecular shape and the polarity of raw material molecule can be according to the actual requirements selected, is combined into
Different film, so that flavone sterling reaches required purification purity.
3. the method that pure natural flavone is extracted in a kind of Flos abelmoschi manihot platymiscium from Malvaceae according to claim 2, its feature
It is：Film made by described different materials includes:It is inorganic, polysulfones (PS), cellulose acetate (CA), polyacrylonitrile (PAN), poly-
Amide (PA), Kynoar (PVDF), polyether sulfone (PES).
4. the method that pure natural flavone is extracted in a kind of Flos abelmoschi manihot platymiscium from Malvaceae according to claim 2, its feature
It is：The film of described PSPP includes：Ceramic membrane, molecular cut off is 20000~100000dalton；Ultrafiltration
Film, molecular cut off is 1000~50000dalton；NF membrane, molecular cut off is 100~1000dalton.
5. the method that pure natural flavone is extracted in a kind of Flos abelmoschi manihot platymiscium from Malvaceae according to claim 2, its feature
It is：The film of described multi-form includes:Flat Membrane, tubular membrane, hollow-fibre membrane and rolled film.
6. a kind of refined purification, the method for concentrated natural flavone, it is characterised in that：The method step includes：
(A), the feed liquid kettle of separating natural flavone is set；The ceramic film component connected with feed liquid kettle is externally provided with feed liquid kettle；Arrange
The separator intermediate storage tank connected with ceramic film component；By the extracting flavonoids after ethonal extraction, decompression and solvent recovery
Liquid is placed in feed liquid kettle, makes feed liquid flow through ceramic film component by pressurization, removes the impurity in solution；Permeation ceramic membrane component
Permeate, Jing ceramic film component permeate mouth flows into intermediate storage tank；The solution Jing ceramic membrane concentrated solution mouths of non-permeation ceramic membrane are returned
Feed back liquid kettle；Pure water is continuously added in feed liquid kettle, is filtered, so that flavone permeation ceramic membrane group as far as possible many in feed liquid
Part, improves yield；
(B), the intermediate storage tank of purification natural flavone is set；The ultrafilter membrane group being connected with intermediate storage tank is externally provided with intermediate storage tank
Part；The separator intermediate storage tank that setting is connected with hyperfiltration membrane assembly；Feed liquid is flowed through by pressurization the feed liquid in intermediate storage tank
Hyperfiltration membrane assembly, removes the non-flavonoid substance in solution；Through the permeate of ultrafilter membrane, Jing ultrafiltration membrane permeate liquid mouth flows into middle
Storage tank；Not through the solution of ultrafilter membrane, Jing ultrafilter membrane concentrated solutions mouth returns intermediate storage tank；It is continuously added in intermediate storage tank pure
Water, is filtered, so that flavone as far as possible many in feed liquid passes through hyperfiltration membrane assembly, improves yield；
(C), the intermediate storage tank of concentrated natural flavone is set；The NF membrane group being connected with intermediate storage tank is externally provided with intermediate storage tank
Part；Make feed liquid flow through nanofiltration membrane component by pressurization the feed liquid in intermediate storage tank, the moisture in solution is removed as much as possible
And metal ion；Through the permeate of NF membrane, Jing NF membrane outlet discharge system；Not through the solution of NF membrane, Jing nanofiltrations
Membrance concentration liquid mouth returns intermediate storage tank；Jing is constantly circulated, and sterling natural flavone is finally obtained in intermediate storage tank.
7. a kind of refined purification according to claim 6, the method for concentrated natural flavone, it is characterised in that：The method is walked
Suddenly also include：
(D), the flavonoids solution after concentration is added in manifold vacuum freeze drier carries out lyophilization, obtains solid flavone pure
Product.
8. a kind of method that natural flavone is extracted in Flos abelmoschi manihot platymiscium from Malvaceae, it is characterised in that：The method step includes：
A, to take material Malvaceae Flos abelmoschi manihot platymiscium-vegetable Furong dry flower some, cleaned；
B, dried to moisture content 5%-10%, operation temperature 50-80 DEG C by heated-air circulation dryer；
C, the material after drying is put in jet mill, carries out being crushed to 80-120 mesh；
D, the material after dries pulverizing is put in 500L rustless steel vacuum distillation reactors again, and its built-in ultrasound wave occurs
Device；
C, the ethanol solution for adding 20-70%, solid-liquid ratio is：1/5-1/100；
D, rustless steel vacuum distillation reactor is warming up to into 40-60 DEG C；
E, unlatching ultrasound wave, by frequency 30-40KHz is adjusted to, and extracts 20-90 minutes；
Ethanol is reclaimed in F, vacuum distillation；
G and then, do pretreatment with filter press, obtain flavone crude product solution.
9. the method that natural flavone is extracted in the Flos abelmoschi manihot platymiscium from Malvaceae according to claim 8, it is characterised in that：Should
Method and step also includes：
(1), flavone crude product solution is put in rustless steel feed liquid kettle 1；Pressurized pump 4 pressurizes, and under 0.05-3Mpa pressure, makes
Flavonoids solution is filtered with the inorganic tubular ceramic membrane module 5 that molecular cut off is 20000~100000dalton, the removal of impurity is gone；
(2), enter in intermediate storage tank 2 through the ceramic membrane permeate 9 of inorganic tubular ceramic membrane module 5；Non- permeation parts are returned
Feed liquid kettle 1；During constantly in feed liquid kettle 1 add pure water 14, with as often as possible eluting flavone；
(3), by the flavonoids solution gone after the removal of impurity in intermediate storage tank 2 polysulfones of 1000~50000dalton of molecular cut off
Hollow fiber ultrafiltration membrane 6, pressurized pump 4 pressurizes, and the purification of flavone is carried out under 0.05-3Mpa pressure, by other molecular weight
Material discharges flavonoids solution, obtains flavonoids solution merely；
(4), ultrafiltration membrane permeate liquid 11 enters intermediate storage tank 2 '；
(5), ultrafilter membrane concentrated solution 10 is back in intermediate storage tank 2；With the generation of ultrafiltration membrane permeate liquid 11, constantly to middle storage
Pure water is added in tank 2, as often as possible to exclude non-flavonoid substance；
(6), using the polyamide rolling NF membrane 7 of 100~1000dalton of molecular cut off, pressurized pump 4 pressurizes,
Under 0.05-3Mpa pressure, to intermediate storage tank 2 ' in pure flavonoids solution concentrate, discharge most of moisture and small molecule salt；
The discharge system of Jing NF membrane permeate 13, NF membrane concentrated solution 12 is back in intermediate storage tank 2 ', Jing 5-10 minutes, in middle storage
Flavonoids solution must be concentrated in tank 2 '；
(7), the flavonoids solution after concentration is added in manifold vacuum freeze drier carries out lyophilization, obtains solid flavone pure
Product.
10. the method that pure natural flavone is extracted in a kind of Flos abelmoschi manihot platymiscium from Malvaceae according to claim 6 or 9, its
It is characterised by：Molecular size range, molecular shape and the polarity of raw material molecule can be according to the actual requirements selected, is combined into different
Film, so that flavone sterling reaches required purification purity.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108379174A (en) * | 2018-05-16 | 2018-08-10 | 广东药科大学 | A kind of application of arrowleaf abelmoschus root extract in preparing antioxidant |
| CN108524406A (en) * | 2018-07-21 | 2018-09-14 | 河南中立宝花茶有限公司 | A kind of Golden flower facial mask and preparation method thereof |
-
2016
- 2016-11-08 CN CN201610979600.6A patent/CN106674181A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108379174A (en) * | 2018-05-16 | 2018-08-10 | 广东药科大学 | A kind of application of arrowleaf abelmoschus root extract in preparing antioxidant |
| CN108524406A (en) * | 2018-07-21 | 2018-09-14 | 河南中立宝花茶有限公司 | A kind of Golden flower facial mask and preparation method thereof |
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