CN106543768B - The method for extracting stalk pigment using steam explosion technology - Google Patents
The method for extracting stalk pigment using steam explosion technology Download PDFInfo
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- CN106543768B CN106543768B CN201610852092.5A CN201610852092A CN106543768B CN 106543768 B CN106543768 B CN 106543768B CN 201610852092 A CN201610852092 A CN 201610852092A CN 106543768 B CN106543768 B CN 106543768B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C403/00—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
- C07C403/24—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains four or more hetero rings
Abstract
The invention discloses a kind of methods for extracting stalk pigment using steam explosion technology, belong to stalk comprehensive utilization technical field.The present invention obtains high-purity flavones, carotenoid and chloroplast pigment simultaneously by stalk, and the above-mentioned stalk pigment component of high-purity, high quality has been refined out by measures such as cryogenic high pressure, steam explosion technology, inert environments, organic solvents.The present invention can be created when implementing, can also make full use of it is existing it is numerous or paper-making pulping enterprise on the verge of bankrupt slightly transformation can be produced on the basis ofs its workshop, equipment, facility etc., put into that small, the period is short, easy popularization.
Description
Technical field
The invention belongs to stalk comprehensive utilization technical fields, and in particular to a kind of to extract stalk pigment using steam explosion technology
Method.
Background technique
According to statistics, China can harvest more than 900,000,000 tons of various crop materials every year.Stalk described here, including wheat, corn,
It is remained after the herbage harvestings seed such as the crops such as rice, cotton, sorghum, crudefiber crop, soybean, peanut, potato, melon and clover, prairie milk vetch
Remaining stem, leaf, skin (shell), climing rattan (seedling) etc. and sugarcane (slag), reed, bamboo etc..Water content when with stalk cutting is different,
Stalk is divided into following two class: first kind stalk, 35% or more moisture content, such as: melon seedling (moisture content is 80% or more), part are beautiful
Rice kind (50% or more moisture content, harvest season be still green), sugarcane (50% or more moisture content), herbage (moisture content 70% with
On) etc.；Second class stalk, water content 35% is hereinafter, include most of stalk, such as wheat straw, straw, corn, cotton are being received
Obtain the stalk of season collection.
Pigment rich in stalk.Crop material pigment includes chloroplast pigment and cell liquid pigment, the former exists
It is related with photosynthesis in chloroplaset, such as chlorophyll, lutein；The latter is present in vacuole, as Flavonoid substances (including
Anthocyanidin, isoflavones etc.).Stalk pigment is distributed mainly on the positions such as the bar of stalk, stem, rattan, seedling, Ye, Miho.
Function value, the action value of natural colour chlorins compound are increasingly paid close attention to by people.Flavones is a major class day
Right pigment family, most essential physiological function are antioxidation.Flavone compound is got over as the effect of functional component
Come more important, have to the main function of the mankind: antitumor, antiallergy, antiviral, strengthen immunity improve cardiovascular and cerebrovascular, adjust
Save endocrine, anti-aging etc..Most well known in flavones is isoflavones.Crop flavones content highest at the maturity period,
Thus crop material is the good raw material for preparing flavones.
And carotenoid and chloroplast pigment are industrially a kind of colorants of important foods and cosmetics.It is existing
In technology, extracting flavones, carotenoid and chloroplast pigment does not have feasible solution also simultaneously from stalk, cannot give full play to
The utility value of stalk.
Summary of the invention
In order to make up for the deficiencies of the prior art, the present invention, which provides one kind, can effectively extract Flavonoid substances and class in stalk
The method of carrotene and chloroplast pigment.
The technical solution of the present invention is as follows:
A method of stalk pigment is extracted using steam explosion technology, comprising the following steps:
The extraction of A flavones
A1) stalk segment is placed in steam-explosion jar, is passed through after inert gas empties air in tank and is sealed into the steam-explosion jar
Mouthful；Then it is forced into 1-5 MPa, pressure maintaining is spurted after 20-120 minutes, obtains stalk slurry；
A2) the stalk slurry is placed in steam-explosion jar, ether is added, inert gas is passed through into the steam-explosion jar will
Air seals after emptying in tank；Then inert gas is intermittently passed through into tank, to maintain pressure inside the tank for 1-5 Mpa, temperature
Degree is 16-20 DEG C, and pressure maintaining is spurted after 20-180 minutes；
A3 it) is separated by solid-liquid separation, obtains filter residue one and filtrate one；Filter residue one, ether solution and filtrate after washing are washed using ether
One merges, and obtains amalgamation liquid one；
A4 the solid phase particles in amalgamation liquid one) are removed, the amalgamation liquid after removing solid phase particles successively passes through ultrafiltration, reverse osmosis
UF membrane obtains the chloroplaset that molecular weight is greater than 1000 dalton between the flavones clarified solution and molecular weight of 300-1000 dalton
Pigment clarified solution；
A5) evaporation removes the solvent ether in the flavones clarified solution, and residue is washed repeatedly with ethyl alcohol, through yellowly dry
Ketone finished product；
The preparation of B carotenoid
B1) evaporation removes the solvent ether in the chloroplast pigment clarified solution, and residue is solid after being washed repeatedly with ethyl alcohol
Liquid separation, obtains filter residue two and filtrate two, and filter residue two is carotenoid；
B2) filter residue two is using after petroleum ether dissolution, and evaporation removes solvent petroleum ether, after residue is washed repeatedly with petroleum ether
Obtain the petroleum ether solution of carotenoid；
B3) petroleum ether solution of the carotenoid using fibre column chromatography be separated into alpha-carotene, beta carotene,
Three kinds of pigments of gamma carotene, are eluted with ethyl alcohol-petroleum ether mixed solvent, and 3 kinds of pigments are collected separately in different time
In the eluent of section；
B4 vehicle of ethanol-petroleum ether the mixed solvent for removing three kinds of eluents, residue ethyl alcohol -) are evaporated respectively
Petroleum ether mixed solvent repeated washing, is dried to obtain alpha-carotene, beta carotene, gamma carotene finished product；
The preparation of C chloroplast pigment
C1) vaporization removal step B1) gained filtrate two in solvent, residue washed repeatedly with ethyl alcohol after chloroplaset color
The ethanol solution of element；
C2) ethanol solution of the chloroplast pigment is separated into chlorophyll a, chlorophyll b, leaf Huang using fibre column chromatography
Element is eluted with ethyl alcohol-petroleum ether mixed solvent, and 3 kinds of pigments are collected separately in eluent in different time periods；
C3 vehicle of ethanol-petroleum ether the mixed solvent for removing three kinds of eluents, residue ethyl alcohol weight) are evaporated respectively
After backwashing is washed, and chlorophyll a, chlorophyll b, lutein finished product are dried to obtain.
Preferably, step A1) described in stalk segment obtaining step are as follows: harvest fresh straw removes sandstone, miscellaneous
The segment of 1-3cm is washed, is cut into after object with clear water.
Preferably, step A1) in stalk segment be added steam-explosion jar in amount be steam explosion tank volume 5-50%.
Further, step A1) described in stalk dissection process completely cut off air, flavones is easily oxidized, air insulating treatment,
It can guarantee the integrality of flavones.
Further, step A2) in ether volume is added is 1-20 times of stalk slurry.
Preferably, step A2) in steam-explosion jar temperature controlled by inert gas, the holding vessel of the inert gas
It is externally provided with interlayer, Cryogenic air is full of in interlayer, it is 16-18 DEG C that Cryogenic air, which controls inert gas temperature in holding vessel,.Using
Lower temperature and inert gas environment purpose are that decomposition, oxidation of pigment component molecule etc. is avoided to react.
Further, step A2) in be passed through the volume of inert gas in steam-explosion jar be 1-10 times of steam explosion tank volume.
Preferably, step B3) in the volume ratio of ethyl alcohol-petroleum ether in the mixed solvent ethyl alcohol and petroleum ether used be
(1-3): (1-9).
Preferably, step C2) in the volume ratio of ethyl alcohol-petroleum ether in the mixed solvent ethyl alcohol and petroleum ether used be
(1-7): (1-9).
Preferably, step A5), C1), C3) described in ethyl alcohol volume fraction be 95%.
The invention has the benefit that
The present invention obtains high-purity flavones, carotenoid and chloroplast pigment simultaneously by stalk, passes through cryogenic high pressure, vapour
The measures such as quick-fried technology, inert environments, organic solvent have refined out the above-mentioned stalk pigment component of high-purity, high quality.
The present invention can be created when implementing, and can also make full use of existing numerous papermaking for or frequently facing bankruptcy
Slurrying enterprise, slightly transformation can be produced on the basis ofs its workshop, equipment, facility etc., and investment is small, the period is short, easy popularization.
Specific embodiment
Embodiment 1
A method of stalk pigment is extracted using steam explosion technology, comprising the following steps:
The extraction of A flavones
A1) corn stover segment is placed in steam-explosion jar, and stalk segment additional amount reaches the 15% of tank volume, to the vapour
It is passed through after inert gas empties air in tank and seals in quick-fried tank；Then 1.5 MPa are forced into, pressure maintaining is spurted after 100 minutes, obtained
Stalk slurry；It is packed into hermetic bag, is filled with inert gas, shady place is set and stores, is spare.
Step A1) in corn stover segment obtaining step are as follows: harvest fresh straw in the fall, used after removing sandstone, sundries
Clear water washing, the segment for being cut into 2-3cm then move into freezer and store, is stand-by；This kind corn is feed form corn variety,
Autumn is still green when harvesting.
Since phytochrome of the present invention has the characteristics that oxidizable, thus to be made in inert gas environment
It is standby, to guarantee the integrality of pigment composition.
Step A1) using the impact force from inside to outside that high pressure gas generates during spurting stalk cell wall is broken through,
Make stalk cellular content all " broken wall and go out ", conducive to next step component separation and refine；Because the present invention needs to prepare
Flavonoids product, and these ingredients almost exist only in into the cell, thus must broken wall.
A2) the stalk slurry is placed in steam-explosion jar, 8 times of volume ether are added, are passed through into the steam-explosion jar lazy
Property gas air will be sealed after emptying in tank, being passed through inert gas volume is 4 times of tank volume；Then intermittently into tank
It is passed through inert gas, to maintain pressure inside the tank for 1.5 Mpa, temperature is 16-20 DEG C, and pressure maintaining is spurted after 120 minutes.
Step A2) lower temperature and nitrogen environment are used in steam explosion separation process, it is therefore intended that avoid pigment component
The reaction such as decomposition, oxidation of molecule；Coming into full contact with for pigment and solvent ensure that using high pressure (being realized by being passed through nitrogen)
With dissolution.
Temperature in tank is controlled by the temperature of nitrogen.The holding vessel of nitrogen is externally provided with interlayer, inside there is Cryogenic air, thus
Nitrogen temperature in holding vessel is between 16-18 DEG C.
A3) press master shove separates, and obtains filter residue one and filtrate one, is pigment, the lipid etc. of dissolution, filter in filtrate one
Slag one is the slurry containing starch, protein, fibrous fraction etc.；It is washed twice of filter residue 1 using 3 times of ether, the second after washing
Ether liquid merges with filtrate one, obtains amalgamation liquid one；Filter residue one can be separated further and prepare other components.
A4 the solid phase particles in amalgamation liquid one) are removed, the amalgamation liquid after removing solid phase particles successively passes through ultrafiltration, reverse osmosis
UF membrane obtains the chloroplaset that molecular weight is greater than 1000 dalton between the flavones clarified solution and molecular weight of 300-1000 dalton
Pigment clarified solution.
A5 it) is evaporated in vacuo the solvent ether removed in the flavones clarified solution, residue is washed repeatedly 3 times with 95% ethyl alcohol,
It is freeze-dried to obtain flavones finished product.
Through detecting, the quality of gained flavones is the 1.7% of corn stover butt quality.
The preparation of B carotenoid
B1) evaporation removes the solvent ether in the chloroplast pigment clarified solution, and residue is washed 3 times with dehydrated alcohol,
This step is repeated, spiral shell centrifuge separation of crouching obtains filter residue two and filtrate two, and filter residue two is carotenoid.
B2) filter residue two repeats to wash using removing solvent petroleum ether, residue petroleum ether after petroleum ether dissolution, is evaporated in vacuo
It washs 3 times, the petroleum ether solution of carotenoid is obtained after this step of repetition.
B3) petroleum ether solution of the carotenoid using fibre column chromatography be separated into alpha-carotene, beta carotene,
Three kinds of pigments of gamma carotene, are eluted with ethyl alcohol-petroleum ether mixed solvent, ethyl alcohol-petroleum ether in the mixed solvent ethyl alcohol with
The volume ratio of petroleum ether is 1:9, and 3 kinds of pigments are collected separately in eluent in different time periods.
B4 it) is evaporated in vacuo the vehicle of ethanol-petroleum ether mixed solvent for removing three kinds of eluents, residue second respectively
Alcohol-petroleum ether mixed solvent washes repeatedly 3 times, repeats this step, washes away impurity, freeze-dried to obtain alpha-carotene, β-Hu
Radish element, gamma carotene finished product.
Through detecting, the quality of gained carotenoid is the 1.3% of corn stover butt quality.
The preparation of C chloroplast pigment
C1) vaporization removal step B1) gained filtrate two in solvent, residue with 95% ethyl alcohol wash repeatedly 3 times after, weigh
Duplicate step, washes away impurity, obtains the ethanol solution of chloroplast pigment.
C2) ethanol solution of the chloroplast pigment is separated into chlorophyll a, chlorophyll b, leaf Huang using fibre column chromatography
Element is eluted with ethyl alcohol-petroleum ether mixed solvent, and the volume ratio of ethyl alcohol-petroleum ether in the mixed solvent ethyl alcohol and petroleum ether is
5:5,3 kinds of pigments are collected separately in eluent in different time periods.
C3) vehicle of ethanol-petroleum ether mixed solvent of evaporation removing three kinds of eluents, residue are used respectively respectively
95% ethyl alcohol washes repeatedly 3 times, repeats this step, washes away impurity, it is freeze-dried obtain chlorophyll a, chlorophyll b, lutein at
Product.
Through detecting, the quality of gained chlorophyll is the 1.1% of corn stover butt quality, and the quality of lutein is corn stalk
The 0.7% of stalk butt quality.
Embodiment 2
A method of stalk pigment is extracted using steam explosion technology, comprising the following steps:
The extraction of A flavones
A1) watermelon seedling segment is placed in steam-explosion jar, and watermelon seedling segment additional amount reaches the 20% of tank volume, to the vapour
It is passed through after inert gas empties air in tank and seals in quick-fried tank；Then 2 MPa are forced into, pressure maintaining is spurted after 90 minutes, obtains melon
Seedling slurry；It is packed into hermetic bag, is filled with inert gas, shady place is set and stores, is spare.
Step A1) Chinese and Western melon seedling segment obtaining step are as follows: harvest fresh watermelon seedling in the fall, used after removing sandstone, sundries
Clear water washing, the segment for being cut into 2-3cm then move into freezer and store, is stand-by.
Since phytochrome of the present invention has the characteristics that oxidizable, thus to be made in inert gas environment
It is standby, to guarantee the integrality of pigment composition.
Step A1) using the impact force from inside to outside that high pressure gas generates during spurting melon seedling cell wall is broken through,
Make watermelon seedling cellular content all " broken wall and go out ", conducive to next step component separation and refine；Because the present invention needs to make
Standby flavonoids product, and these ingredients almost exist only in into the cell, thus must broken wall.
A2) the melon seedling slurry is placed in steam-explosion jar, 9 times of volume ether are added, are passed through into the steam-explosion jar lazy
Property gas air will be sealed after emptying in tank, being passed through inert gas volume is 5 times of tank volume；Then intermittently into tank
It is passed through inert gas, to maintain pressure inside the tank for 2 Mpa, temperature is 16-20 DEG C, and pressure maintaining is spurted after 110 minutes.
Step A2) lower temperature and nitrogen environment are used in steam explosion separation process, it is therefore intended that avoid pigment component
The reaction such as decomposition, oxidation of molecule；Coming into full contact with for pigment and solvent ensure that using high pressure (being realized by being passed through nitrogen)
With dissolution.
Temperature in tank is controlled by the temperature of nitrogen.The holding vessel of nitrogen is externally provided with interlayer, inside there is Cryogenic air, thus
Nitrogen temperature in holding vessel is between 16-18 DEG C.
A3) press master shove separates, and obtains filter residue one and filtrate one, is pigment, the lipid etc. of dissolution, filter in filtrate one
Slag one is the slurry containing starch, protein, fibrous fraction etc.；It is washed twice of filter residue 1 using 3 times of ether, the second after washing
Ether liquid merges with filtrate one, obtains amalgamation liquid one；Filter residue one can be separated further and prepare other components.
A4 the solid phase particles in amalgamation liquid one) are removed, the amalgamation liquid after removing solid phase particles successively passes through ultrafiltration, reverse osmosis
UF membrane obtains the chloroplaset that molecular weight is greater than 1000 dalton between the flavones clarified solution and molecular weight of 300-1000 dalton
Pigment clarified solution.
A5 it) is evaporated in vacuo the solvent ether removed in the flavones clarified solution, residue is washed repeatedly 3 times with 95% ethyl alcohol,
It is freeze-dried to obtain flavones finished product.
Through detecting, the quality of gained flavones is the 1.2% of watermelon seedling butt quality.
The preparation of B carotenoid
B1) evaporation removes the solvent ether in the chloroplast pigment clarified solution, and residue is washed 3 times with dehydrated alcohol,
This step is repeated, spiral shell centrifuge separation of crouching obtains filter residue two and filtrate two, and filter residue two is carotenoid.
B2) filter residue two repeats to wash using removing solvent petroleum ether, residue petroleum ether after petroleum ether dissolution, is evaporated in vacuo
It washs 3 times, the petroleum ether solution of carotenoid is obtained after this step of repetition.
B3) petroleum ether solution of the carotenoid using fibre column chromatography be separated into alpha-carotene, beta carotene,
Three kinds of pigments of gamma carotene, are eluted with ethyl alcohol-petroleum ether mixed solvent, ethyl alcohol-petroleum ether in the mixed solvent ethyl alcohol with
The volume ratio of petroleum ether is 2:8, and 3 kinds of pigments are collected separately in eluent in different time periods.
B4 it) is evaporated in vacuo the vehicle of ethanol-petroleum ether mixed solvent for removing three kinds of eluents, residue second respectively
Alcohol-petroleum ether mixed solvent washes repeatedly 3 times, repeats this step, washes away impurity, freeze-dried to obtain alpha-carotene, β-Hu
Radish element, gamma carotene finished product.
Through detecting, the quality of gained carotenoid is the 1.8% of watermelon seedling butt quality.
The preparation of C chloroplast pigment
C1) vaporization removal step B1) gained filtrate two in solvent, residue with 95% ethyl alcohol wash repeatedly 3 times after, weigh
Duplicate step, washes away impurity, obtains the ethanol solution of chloroplast pigment.
C2) ethanol solution of the chloroplast pigment is separated into chlorophyll a, chlorophyll b, leaf Huang using fibre column chromatography
Element is eluted with ethyl alcohol-petroleum ether mixed solvent, and the volume ratio of ethyl alcohol-petroleum ether in the mixed solvent ethyl alcohol and petroleum ether is
4:6,3 kinds of pigments are collected separately in eluent in different time periods.
C3) vehicle of ethanol-petroleum ether mixed solvent of evaporation removing three kinds of eluents, residue are used respectively respectively
95% ethyl alcohol washes repeatedly 3 times, repeats this step, washes away impurity, it is freeze-dried obtain chlorophyll a, chlorophyll b, lutein at
Product.
Through detecting, the quality of gained chlorophyll is the 1.3% of watermelon seedling butt quality, and the quality of lutein is dry for watermelon seedling
The 0.6% of matrix amount.
Embodiment 3
A method of stalk pigment is extracted using steam explosion technology, comprising the following steps:
The extraction of A flavones
A1) sugarcane segment is placed in steam-explosion jar, and sugarcane segment additional amount reaches the 25% of tank volume, to the steam-explosion jar
In be passed through inert gas will in tank air empty after seal；Then 2.5 MPa are forced into, pressure maintaining is spurted after 85 minutes, obtains sugarcane
Slurry；It is packed into hermetic bag, is filled with inert gas, shady place is set and stores, is spare.
Step A1) in sugarcane segment obtaining step are as follows: harvest fresh cane, go after sandstone, sundries to be washed with clear water, cut
At the segment of 2-3cm, then moves into freezer and store, is stand-by.
Since phytochrome of the present invention has the characteristics that oxidizable, thus to be made in inert gas environment
It is standby, to guarantee the integrality of pigment composition.
Step A1) using the impact force from inside to outside that high pressure gas generates during spurting sugarcane cell wall is broken through,
Make sugarcane cell content all " broken wall and go out ", conducive to next step component separation and refine；Because the present invention needs to prepare
Flavonoids product, and these ingredients almost exist only in into the cell, thus must broken wall.
A2) the sugarcane slurry is placed in steam-explosion jar, 10 times of volume ether are added, are passed through into the steam-explosion jar lazy
Property gas air will be sealed after emptying in tank, being passed through inert gas volume is 6 times of tank volume；Then intermittently into tank
It is passed through inert gas, to maintain pressure inside the tank for 2 .5Mpa, temperature is 16-20 DEG C, and pressure maintaining is spurted after 100 minutes.
Step A2) lower temperature and nitrogen environment are used in steam explosion separation process, it is therefore intended that avoid pigment component
The reaction such as decomposition, oxidation of molecule；Coming into full contact with for pigment and solvent ensure that using high pressure (being realized by being passed through nitrogen)
With dissolution.
Temperature in tank is controlled by the temperature of nitrogen.The holding vessel of nitrogen is externally provided with interlayer, inside there is Cryogenic air, thus
Nitrogen temperature in holding vessel is between 16-18 DEG C.
A3) press master shove separates, and obtains filter residue one and filtrate one, is pigment, the lipid etc. of dissolution, filter in filtrate one
Slag one is the slurry containing starch, protein, fibrous fraction etc.；It is washed twice of filter residue 1 using 3 times of ether, the second after washing
Ether liquid merges with filtrate one, obtains amalgamation liquid one；Filter residue one can be separated further and prepare other components.
A4 the solid phase particles in amalgamation liquid one) are removed, the amalgamation liquid after removing solid phase particles successively passes through ultrafiltration, reverse osmosis
UF membrane obtains the chloroplaset that molecular weight is greater than 1000 dalton between the flavones clarified solution and molecular weight of 300-1000 dalton
Pigment clarified solution.
A5 it) is evaporated in vacuo the solvent ether removed in the flavones clarified solution, residue is washed repeatedly 3 times with 95% ethyl alcohol,
It is freeze-dried to obtain flavones finished product.
Through detecting, the quality of gained flavones is the 1.4% of sugarcane butt quality.
The preparation of B carotenoid
B1) evaporation removes the solvent ether in the chloroplast pigment clarified solution, and residue is washed 3 times with dehydrated alcohol,
This step is repeated, spiral shell centrifuge separation of crouching obtains filter residue two and filtrate two, and filter residue two is carotenoid.
B2) filter residue two repeats to wash using removing solvent petroleum ether, residue petroleum ether after petroleum ether dissolution, is evaporated in vacuo
It washs 3 times, the petroleum ether solution of carotenoid is obtained after this step of repetition.
B3) petroleum ether solution of the carotenoid using fibre column chromatography be separated into alpha-carotene, beta carotene,
Three kinds of pigments of gamma carotene, are eluted with ethyl alcohol-petroleum ether mixed solvent, ethyl alcohol-petroleum ether in the mixed solvent ethyl alcohol with
The volume ratio of petroleum ether is 2:8, and 3 kinds of pigments are collected separately in eluent in different time periods.
B4 it) is evaporated in vacuo the vehicle of ethanol-petroleum ether mixed solvent for removing three kinds of eluents, residue second respectively
Alcohol-petroleum ether mixed solvent washes repeatedly 3 times, repeats this step, washes away impurity, chilled freeze-drying obtain alpha-carotene,
Beta carotene, gamma carotene finished product.
Through detecting, the quality of gained carotenoid is the 1.9% of sugarcane butt quality.
The preparation of C chloroplast pigment
C1) vaporization removal step B1) gained filtrate two in solvent, residue with 95% ethyl alcohol wash repeatedly 3 times after, weigh
Duplicate step, washes away impurity, obtains the ethanol solution of chloroplast pigment.
C2) ethanol solution of the chloroplast pigment is separated into chlorophyll a, chlorophyll b, leaf Huang using fibre column chromatography
Element is eluted with ethyl alcohol-petroleum ether mixed solvent, and the volume ratio of ethyl alcohol-petroleum ether in the mixed solvent ethyl alcohol and petroleum ether is
4:6,3 kinds of pigments are collected separately in eluent in different time periods.
C3) vehicle of ethanol-petroleum ether mixed solvent of evaporation removing three kinds of eluents, residue are used respectively respectively
95% ethyl alcohol washes repeatedly 3 times, repeats this step, washes away impurity, it is freeze-dried obtain chlorophyll a, chlorophyll b, lutein at
Product.
Through detecting, the quality of gained chlorophyll is the 1.2% of sugarcane butt quality, and the quality of lutein is sugarcane butt matter
The 0.7% of amount.
Claims (10)
1. a kind of method for extracting stalk pigment using steam explosion technology, which comprises the following steps:
The extraction of A flavones
A1) stalk segment is placed in steam-explosion jar, is passed through after inert gas empties air in tank and is sealed into the steam-explosion jar；
Then it is forced into 1-5 MPa, pressure maintaining is spurted after 20-120 minutes, obtains stalk slurry；
A2) the stalk slurry is placed in steam-explosion jar, ether is added, inert gas is passed through into the steam-explosion jar will be in tank
Air seals after emptying；Then inert gas is intermittently passed through into tank, to maintain pressure inside the tank for 1-5 MPa, temperature is
16-20 DEG C, pressure maintaining is spurted after 20-180 minutes；
A3 it) is separated by solid-liquid separation, obtains filter residue one and filtrate one；Filter residue one is washed using ether, the ether solution and filtrate one after washing close
And obtain amalgamation liquid one；
A4 the solid phase particles in amalgamation liquid one) are removed, the amalgamation liquid one after removing solid phase particles successively passes through ultrafiltration, reverse osmosis membrane
Separation obtains the chloroplaset color that molecular weight is greater than 1000 dalton between the flavones clarified solution and molecular weight of 300-1000 dalton
Plain clarified solution；
A5) evaporation removes the solvent ether in the flavones clarified solution, and residue is washed repeatedly with ethyl alcohol, through dry flavones at
Product；
The preparation of B carotenoid
B1) evaporation removes the solvent ether in the chloroplast pigment clarified solution, solid-liquid point after residue is washed repeatedly with ethyl alcohol
From obtaining filter residue two and filtrate two, filter residue two is carotenoid；
B2) for filter residue two using after petroleum ether dissolution, evaporation removes solvent petroleum ether, and residue obtains class after being washed repeatedly with petroleum ether
The petroleum ether solution of carrotene；
B3) petroleum ether solution of the carotenoid is separated into alpha-carotene, beta carotene, γ-Hu using fibre column chromatography
Radish three kinds of pigments of element, are eluted, 3 kinds of pigments are collected separately to be washed in different time periods with ethyl alcohol-petroleum ether mixed solvent
In de- liquid；
B4 vehicle of ethanol-petroleum ether the mixed solvent for removing three kinds of eluents, residue ethyl alcohol-petroleum) are evaporated respectively
Ether mixed solvent repeated washing, is dried to obtain alpha-carotene, beta carotene, gamma carotene finished product；
The preparation of C chloroplast pigment
C1) vaporization removal step B1) solvent in gained filtrate two, residue washed repeatedly with ethyl alcohol after chloroplast pigment
Ethanol solution；
C2) ethanol solution of the chloroplast pigment is separated into chlorophyll a, chlorophyll b, lutein using fibre column chromatography, uses
Ethyl alcohol-petroleum ether mixed solvent is eluted, and 3 kinds of pigments are collected separately in eluent in different time periods；
C3) vehicle of ethanol-petroleum ether mixed solvent of evaporation removing three kinds of eluents, residue ethyl alcohol repeat to wash respectively
It washs, is dried to obtain chlorophyll a, chlorophyll b, lutein finished product.
2. a kind of method for extracting stalk pigment using steam explosion technology according to claim 1, it is characterised in that: step
A1 the obtaining step of stalk segment described in) are as follows: harvest fresh straw goes after sandstone, sundries to be washed with clear water, is cut into 1-3cm
Segment.
3. a kind of method for extracting stalk pigment using steam explosion technology according to claim 1 or 2, it is characterised in that: step
Rapid A1) in stalk segment be added steam-explosion jar in amount be steam explosion tank volume 5-50%.
4. a kind of method for extracting stalk pigment using steam explosion technology according to claim 2, it is characterised in that: step
A1 the process of stalk dissection described in) completely cuts off air.
5. a kind of method for extracting stalk pigment using steam explosion technology according to claim 1, it is characterised in that: step
A2 1-20 times that ether volume is stalk slurry is added in).
6. a kind of method for extracting stalk pigment using steam explosion technology according to claim 1, it is characterised in that: step
A2 temperature is controlled by inert gas in steam-explosion jar in), and the holding vessel of the inert gas is externally provided with interlayer, is full of low temperature in interlayer
Air, it is 16-18 DEG C that Cryogenic air, which controls inert gas temperature in holding vessel,.
7. a kind of method for extracting stalk pigment using steam explosion technology according to claim 1 or 6, it is characterised in that: step
Rapid A2) in be passed through the volume of inert gas in steam-explosion jar be 1-10 times of steam explosion tank volume.
8. a kind of method for extracting stalk pigment using steam explosion technology according to claim 1, it is characterised in that: step
B3 the volume ratio of ethyl alcohol-petroleum ether in the mixed solvent ethyl alcohol and petroleum ether used is (1-3): (1-9) in).
9. a kind of method for extracting stalk pigment using steam explosion technology according to claim 1, it is characterised in that: step
C2 the volume ratio of ethyl alcohol-petroleum ether in the mixed solvent ethyl alcohol and petroleum ether used is (1-7): (1-9) in).
10. a kind of method for extracting stalk pigment using steam explosion technology according to claim 1, it is characterised in that: step
A5), C1), C3) described in ethyl alcohol volume fraction be 95%.
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| CN109463491A (en) * | 2019-01-07 | 2019-03-15 | 刘安军 | A kind of instant green tea and preparation method thereof rich in chlorophillins |
| CN111675923B (en) * | 2020-06-24 | 2021-05-25 | 河南大农联生物工程有限公司 | Method for extracting gardenia pigment through steam explosion and application method of extracted pigment |
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