CN110200021A - A kind of preparation method of ginkgo biloba leaf total organic salt - Google Patents
A kind of preparation method of ginkgo biloba leaf total organic salt Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of ginkgo biloba leaf total organic salt, mainly prepare ginkgo leaf organic salt by Soxhlet extraction, saponification, extraction, semi-permeable membrane filtering, concentrated spray drying steps.Preparation method of the invention is simple, and yield is high, good impurity removing effect, product particle particle diameter distribution is uniform, and quality is stablized, which can make full use of ginko leaves flavone, lactone extract production and processing waste, production cost is low, and environmental protection is suitable for the factorial production.
Description
Technical field
The present invention relates to a kind of preparation methods of ginkgo biloba leaf total organic salt, belong to biomedicine field.
Background technique
Ginkgo leaf is the leaf of Ginkgoaceae Ginkgo plant Ginkgo biloba (Ginkgo biloba L.), and ginkgo biloba leaf total organic salt is main
Being separating Ginkgo phenolic acids in ginkgo leaf, fatty acid, chlorophyll etc. passes through saponification institute containing compounds such as phenolic hydroxyl group, carboxyls
?；Ginkgo biloba leaf total organic salt has good antibacterial action, may be used as biological bactericide.Ginko leaves flavone, lactone extract
It produces and processes containing substances such as a large amount of ginkgo leaf phenolic acid, fatty acid, chlorophyll in waste, these direct waste discharges can be made
At environmental pollution, while the physical wastes such as ginkgo leaf phenolic acid, fatty acid, chlorophyll are caused, therefore the system of ginkgo biloba leaf total organic salt
Standby utilize is that very it is necessary to call on and making full use of ginko leaves flavone, lactone extract production and processing waste, make resource most
Bigization.
Summary of the invention
In view of the above existing problems in the prior art, the present invention provides a kind of preparation methods of ginkgo biloba leaf total organic salt, lead to
Soxhlet extraction, saponification, extraction, semi-permeable membrane filtering, concentrated spray drying and other steps are crossed by separating Ginkgo phenolic acids, fatty acid in ginkgo leaf
Class, chlorophyll etc. extract containing compounds such as phenolic hydroxyl group, carboxyls, are saponified obtained ginkgo leaf organic salt, obtain ginkgo leaf organic salt
Rate is high, high-quality.
To achieve the goals above, the present invention adopts the following technical scheme: a kind of preparation method of ginkgo biloba leaf total organic salt,
Specifically includes the following steps:
1) raw material is ground: the ginkgo leaf waste material after choosing flavones, lactone extraction, crushed after being dried, grain diameter are less than
5mm obtains ginkgo leaf powder；
(2) Soxhlet extraction: be added into ginkgo leaf powder obtained in above-mentioned steps (1) I Soxhlet extraction 1 of organic solvent~
10h repeats to extract 2~5 times, combined extract；
(3) it prepares ointment: combined extract being evaporated under reduced pressure recycling organic solvent I, ginkgo leaf is obtained and extracts ointment；
(4) it is saponified: lye is slowly added dropwise to the extraction ointment of ginkgo leaf obtained in above-mentioned steps (3) and low whipping speed is
It is stirred continuously under conditions of 50~500r/min, heat reflux saponification, saponification temperature is 40~65 DEG C, and saponification time is 1~8h, is obtained
To saponification liquor；
(5) it extracts: organic solvent II is added to saponification liquor obtained in above-mentioned steps (4), rock uniformly mixed, standing,
Layering is gradually appeared until layering no longer changes, and collection lower aqueous solution obtains thick organic slat solution, repeats extraction 2~4 times；
(6) semi-permeable membrane filtering and impurity removing: being slowly added dropwise dilute hydrochloric acid to thick organic slat solution obtained in above-mentioned steps (5), adjusts
Then the pH value of thick organic slat solution filters, the impurity such as removal inorganic salts, small-molecule substance obtain total to neutrality through semi-permeable membrane
Organic slat solution；
(7) concentrated spray is dry: by above-mentioned organic slat solution distillation and concentration obtained in above-mentioned steps (6), admittedly contained
The concentrate that amount is 30%~40%, concentrate are pumped into spray drying tower through wriggling, are sprayed into tiny mist by high speed atomisation device
Drop, carries out contacting rapid dry forming with hot wind in Ta Nei, becomes powdered granule, then cooling by air-introduced machine by tower bottom,
Wind send collection, obtains ginkgo biloba leaf total organic salt.
Preferably, the organic solvent I in the step (2) selects any one of ethyl acetate, acetone or dehydrated alcohol,
And dosage when extracting every time is that 5~10L is added in every kilogram of ginkgo leaf powder.
Preferably, the Extracting temperature in the step (2) is 40~65 DEG C.
Preferably, lye in the step (4) select 5~20%NaOH ethanol solution, 5~20%KOH ethanol solution,
5~20%NaOH methanol solution or 5~20%KOH methanol solution, the dosage of the lye are that every kilogram of ginkgo leaf extracts ointment
1~20L is added.
Preferably, the extraction in the step (4) selects n-hexane or petroleum ether, each extraction with organic solvent II
The volume ratio of agent organic solvent II and saponification liquor is 1~10:1.
Beneficial effects of the present invention:
1, the present invention utilizes the organic salt powder of ginkgo biloba leaf total of spray drying process, compares condensing crystallizing, reduces auxiliary
Raw material shortens the production time, improves production efficiency, reduces loss of material, and product particle particle diameter distribution is uniform, and quality is stablized.
2, the present invention selects cellulose acetate semi-permeable membrane, aromatic polyamide semi-permeable membrane, and hydrophily is strong, during applicable pH value is
Property solution, it is high to the substances such as inorganic salts, small-molecule substance removal rates.
3, the present invention selects ethyl acetate, acetone or dehydrated alcohol as organic solvent I, can be by ginkgol in ginkgo leaf
The extraction containing compounds such as phenolic hydroxyl group, carboxyls such as acids, fatty acid, chlorophyll, and recovery rate is higher, makes phenol in ginkgo leaf
The compounds such as hydroxyl, carboxyl are using sufficiently.
4, the present invention using ginkgo leaf as raw material, sufficiently to the substances such as ginkgo leaf phenolic acid, fatty acid, chlorophyll in ginkgo leaf into
Row extraction and application, resource are rationally utilized, and waste discharge is avoided to pollute, and reduce production cost, improve product competitiveness, are improved
Economic benefit.
5, preparation method of the present invention is simple, and yield is high, and good impurity removing effect, product particle particle diameter distribution is uniform, and quality is stablized,
The preparation method can make full use of ginko leaves flavone, lactone extract production and processing waste, and production cost is low, environmental protection,
Suitable for the factorial production.
Specific embodiment
Illustrate the present invention with specific embodiment below, but is not the limitation to invention.
Embodiment 1
In the present embodiment, a kind of preparation method of the ginkgo biloba leaf total organic salt provided, specifically includes the following steps:
(1) raw material is ground: the ginkgo leaf waste material after choosing flavones, lactone extraction, crushed after being dried, grain diameter are less than
5mm obtains ginkgo leaf powder；
(2) Soxhlet extraction: taking ginkgo leaf powder 1kg obtained in above-mentioned steps (1), ethyl acetate 5L is added to it, in temperature
Degree is Soxhlet extraction 2h at 60 DEG C, repeats to extract 3 times, combined extract；
(3) it prepares ointment: combined extract being evaporated under reduced pressure recycling organic solvent I, residue is ginkgo biloba p.e, is obtained
Ointment 50.1g is extracted to ginkgo leaf；
(4) it is saponified: extracting ointment to ginkgo leaf obtained in above-mentioned steps (3) and be slowly added dropwise into 10%NaOH ethanol solution
0.5L and low whipping speed are stirred continuously under conditions of being 100r/min, and heat reflux saponification, saponification temperature is 60 DEG C, saponification time
For 2h, saponification liquor is obtained；
(5) it extracts: petroleum ether 1L is added to saponification liquor obtained in above-mentioned steps (4), rock uniformly mixed, standing, by
Gradually there is layering until layering no longer changes, collection lower aqueous solution obtains thick organic slat solution, repeats extraction 3 times；
(6) semi-permeable membrane filters: concentration is slowly added dropwise less than 10% in thick organic slat solution obtained in above-mentioned steps (5)
Dilute hydrochloric acid adjusts the pH value of thick organic slat solution to neutrality, then filters through aromatic polyamide semi-permeable membrane, remove inorganic salts and divide
Son measures small substance, obtains organic slat solution；
(7) concentrated spray is dry: by above-mentioned organic slat solution distillation and concentration obtained in above-mentioned steps (6), admittedly contained
Amount be 33% concentrate, concentrate through the wriggling that speed is 15rpm be pumped into inlet air temperature be 200 DEG C, leaving air temp 100
DEG C spray drying tower, by atomization frequency be 250Hz high speed atomisation device be sprayed into fine mist, connect in Ta Nei and hot wind
Rapid dry forming is touched, powdered granule is become, then cooling, wind send collection by air-introduced machine by tower bottom, obtains ginkgo biloba leaf total
Organic salt 40.1g, the Particle Size Analyzer through model SALD-2300 measure analysis, and analysis finds that grain diameter is micron order,
Grain is evenly distributed.
Nonaquepous tration is used to the ginkgo biloba leaf total organic salt in upper the present embodiment, ginkgo biloba leaf total organic salt 100mg is taken to be dissolved in
In the glacial acetic acid of 60ml, then plus the anhydrous of 30ml 0.1mol cross chloric acid titer, the 2 anhydrous gentian violet indicator of drop, stir and evenly mix,
With the anhydrous sodium acetate titer of 0.1mol with constant-current titration, after measured, the purity of ginkgo biloba leaf total organic salt is 89.1%.
Embodiment 2
In the present embodiment, a kind of preparation method of the ginkgo biloba leaf total organic salt provided, specifically includes the following steps:
(1) raw material is ground: the ginkgo leaf waste material after choosing flavones, lactone extraction, crushed after being dried, grain diameter are less than
5mm obtains ginkgo leaf powder；
(2) Soxhlet extraction: taking ginkgo leaf powder 6kg obtained in above-mentioned steps (1), ethyl acetate 30L is added to it, in temperature
Degree is Soxhlet extraction 3h at 65 DEG C, repeats to extract 3 times, combined extract；
(3) it prepares ointment: extracting solution obtained in above-mentioned steps (2) is mixed, then vacuum distillation recycling organic solvent
I, residue is ginkgo biloba p.e, obtains ginkgo leaf and extracts ointment 300g；
(4) it is saponified: extracting ointment to ginkgo leaf obtained in above-mentioned steps (3) and be slowly added dropwise into 20%NaOH ethanol solution
1.5L and low whipping speed are stirred continuously under conditions of being 400r/min, and heat reflux saponification, saponification temperature is 65 DEG C, saponification time
For 2h, saponification liquor is obtained；
(5) it extracts: n-hexane 4L is added to saponification liquor obtained in above-mentioned steps (4), rock uniformly mixed, standing, by
Gradually there is layering until layering no longer changes, collection lower aqueous solution obtains thick organic slat solution, repeats extraction 3 times；
(6) semi-permeable membrane filters: concentration is slowly added dropwise less than 10% in thick organic slat solution obtained in above-mentioned steps (5)
Dilute hydrochloric acid adjusts the pH value of thick organic slat solution to neutrality, then filters through aromatic polyamide semi-permeable membrane, remove inorganic salts and divide
Son measures small substance, obtains organic slat solution；
(7) concentrated spray is dry: by above-mentioned organic slat solution distillation and concentration obtained in above-mentioned steps (6), admittedly contained
Amount be 35% concentrate, concentrate through the wriggling that speed is 20rpm be pumped into inlet air temperature be 220 DEG C, leaving air temp 105
DEG C spray drying tower, by atomization frequency be 350Hz high speed atomisation device be sprayed into fine mist, connect in Ta Nei and hot wind
Rapid dry forming is touched, powdered granule is become, then cooling, wind send collection by air-introduced machine by tower bottom, obtains ginkgo biloba leaf total
Organic salt 240.3g, the Particle Size Analyzer through model SALD-2300 measure analysis, and analysis finds that grain diameter is micron order,
Even particle distribution.
Nonaquepous tration is used to the ginkgo biloba leaf total organic salt in upper the present embodiment, ginkgo biloba leaf total organic salt 100mg is taken to be dissolved in
In the glacial acetic acid of 60ml, then plus the anhydrous of 30ml 0.1mol cross chloric acid titer, the 2 anhydrous gentian violet indicator of drop, stir and evenly mix,
With the anhydrous sodium acetate titer of 0.1mol with constant-current titration, after measured, the purity of ginkgo biloba leaf total organic salt is 88.4%.
Embodiment 3
In the present embodiment, a kind of preparation method of the ginkgo biloba leaf total organic salt provided, specifically includes the following steps:
(1) raw material is ground: the ginkgo leaf waste material after choosing flavones, lactone extraction, crushed after being dried, grain diameter are less than
5mm obtains ginkgo leaf powder；
(2) Soxhlet extraction: taking ginkgo leaf powder 10kg obtained in above-mentioned steps (1), and ethyl acetate 50L is added to it,
Temperature is Soxhlet extraction 5h at 60 DEG C, repeats to extract 3 times, combined extract；
(3) it prepares ointment: extracting solution obtained in above-mentioned steps (2) is mixed, then vacuum distillation recycling organic solvent
I, residue is ginkgo biloba p.e, obtains ginkgo leaf and extracts ointment 499.6g；
(4) it is saponified: extracting ointment to ginkgo leaf obtained in above-mentioned steps (3) and be slowly added dropwise into 10%NaOH ethanol solution
5L and low whipping speed are stirred continuously under conditions of being 100r/min, and heat reflux saponification, saponification temperature is 60 DEG C, and saponification time is
5h obtains saponification liquor；
(5) it extracts: n-hexane 10L is added to saponification liquor obtained in above-mentioned steps (4), rock uniformly mixed, standing, by
Gradually there is layering until layering no longer changes, collection lower aqueous solution obtains thick organic slat solution, repeats extraction 3 times；
(6) semi-permeable membrane filters: concentration is slowly added dropwise less than 10% in thick organic slat solution obtained in above-mentioned steps (5)
Dilute hydrochloric acid adjusts the pH value of thick organic slat solution to neutrality, then filters through aromatic polyamide semi-permeable membrane, remove inorganic salts and divide
Son measures small substance, obtains organic slat solution；
(7) concentrated spray is dry: by above-mentioned organic slat solution distillation and concentration obtained in above-mentioned steps (6), admittedly contained
Amount be 33% concentrate, concentrate through the wriggling that speed is 15rpm be pumped into inlet air temperature be 230 DEG C, leaving air temp 110
DEG C spray drying tower, by atomization frequency be 350Hz high speed atomisation device be sprayed into fine mist, connect in Ta Nei and hot wind
Rapid dry forming is touched, powdered granule is become, then cooling, wind send collection by air-introduced machine by tower bottom, obtains ginkgo biloba leaf total
Organic salt 399.8g, the Particle Size Analyzer through model SALD-2300 measure analysis, and analysis finds that grain diameter is micron order,
Even particle distribution.
Nonaquepous tration is used to the ginkgo biloba leaf total organic salt in upper the present embodiment, ginkgo biloba leaf total organic salt 100mg is taken to be dissolved in
In the glacial acetic acid of 60ml, then plus the anhydrous of 30ml 0.1mol cross chloric acid titer, the 2 anhydrous gentian violet indicator of drop, stir and evenly mix,
With the anhydrous sodium acetate titer of 0.1mol with constant-current titration, after measured, the purity of ginkgo biloba leaf total organic salt is 90.7%.
Comparative example
Compared with Example 1, this comparative example difference is step (7):
(7) be concentrated and dried: by above-mentioned organic slat solution distillation and concentration obtained in above-mentioned steps (6), obtaining solid content is
33% concentrate distillation and concentration and is stirred continuously, mixing speed 300rpm, until solid content is at being then 95 DEG C in temperature
90%, it is cooled to distillation and concentration at 40 DEG C and is stirred continuously, mixing speed 200rpm, and spray 95% ethanol solution 100ml, directly
To being completely dried, particle is formed, obtains ginkgo leaf organic salt 39.4g, particle has agglomeration.
Nonaquepous tration is used to the ginkgo biloba leaf total organic salt in upper comparative example, ginkgo biloba leaf total organic salt 100mg is taken to be dissolved in
In the glacial acetic acid of 60ml, then plus the anhydrous of 30ml 0.1mol cross chloric acid titer, the 2 anhydrous gentian violet indicator of drop, stir and evenly mix,
With the anhydrous sodium acetate titer of 0.1mol with constant-current titration, after measured, the purity of ginkgo biloba leaf total organic salt is 84.9%.
Through above-described embodiment 1, embodiment 2, embodiment 3, comparative example 1, discovery utilizes the ginkgo leaf of spray drying process
Total organic salt powder, loss of material is few, and particle size distribution is uniform, soilless sticking phenomenon, and quality is stablized, and the production time is short.
Embodiment 4
In the present embodiment, a kind of preparation method of the ginkgo biloba leaf total organic salt provided, specifically includes the following steps:
(1) raw material is ground: the ginkgo leaf waste material after choosing flavones, lactone extraction, crushed after being dried, grain diameter are less than
5mm obtains ginkgo leaf powder；
(2) Soxhlet extraction: taking ginkgo leaf powder 1.5kg obtained in above-mentioned steps (1), acetone 10.5L is added to it, in temperature
Degree is Soxhlet extraction 3h at 45 DEG C, repeats to extract 3 times, combined extract；
(3) it prepares ointment: extracting solution obtained in above-mentioned steps (2) is mixed, then vacuum distillation recycling organic solvent
I, residue is ginkgo biloba p.e, obtains ginkgo leaf and extracts ointment 87.5g；
(4) it is saponified: extracting ointment to ginkgo leaf obtained in above-mentioned steps (3) and be slowly added dropwise into 5%NaOH ethanol solution
1.5L and low whipping speed are stirred continuously under conditions of being 50r/min, and heat reflux saponification, saponification temperature is 55 DEG C, saponification time
For 2.5h, saponification liquor is obtained；
(5) it extracts: petroleum ether 4L is added to saponification liquor obtained in above-mentioned steps (4), rock uniformly mixed, standing, by
Gradually there is layering until layering no longer changes, collection lower aqueous solution obtains thick organic slat solution, repeats extraction 3 times；
(6) semi-permeable membrane filters: concentration is slowly added dropwise less than 10% in thick organic slat solution obtained in above-mentioned steps (5)
Dilute hydrochloric acid adjusts the pH value of thick organic slat solution to neutrality, then filters through cellulose acetate semi-permeable membrane, remove inorganic salts and molecule
Small substance is measured, organic slat solution is obtained；
(7) concentrated spray is dry: by above-mentioned organic slat solution distillation and concentration obtained in above-mentioned steps (6), admittedly contained
Amount be 35% concentrate, concentrate through the wriggling that speed is 17rpm be pumped into inlet air temperature be 200 DEG C, leaving air temp 100
DEG C spray drying tower, by atomization frequency be 300Hz high speed atomisation device be sprayed into fine mist, connect in Ta Nei and hot wind
Rapid dry forming is touched, powdered granule is become, then cooling, wind send collection by air-introduced machine by tower bottom, obtains ginkgo biloba leaf total
Organic salt 58.3g, the Particle Size Analyzer through model SALD-2300 measure analysis, and analysis finds that grain diameter is micron order,
Grain is evenly distributed.
Nonaquepous tration is used to the ginkgo biloba leaf total organic salt in upper the present embodiment, ginkgo biloba leaf total organic salt 100mg is taken to be dissolved in
In the glacial acetic acid of 60ml, then plus the anhydrous of 30ml 0.1mol cross chloric acid titer, the 2 anhydrous gentian violet indicator of drop, stir and evenly mix,
With the anhydrous sodium acetate titer of 0.1mol with constant-current titration, after measured, the purity of ginkgo biloba leaf total organic salt is 87.2%.
Embodiment 5
In the present embodiment, a kind of preparation method of the ginkgo biloba leaf total organic salt provided, specifically includes the following steps:
(1) raw material is ground: the ginkgo leaf waste material after choosing flavones, lactone extraction, crushed after being dried, grain diameter are less than
5mm obtains ginkgo leaf powder；
(2) Soxhlet extraction: taking ginkgo leaf powder 2kg obtained in above-mentioned steps (1), dehydrated alcohol 16L is added to it, in temperature
Degree is Soxhlet extraction 4h at 55 DEG C, repeats to extract 3 times, combined extract；
(3) it prepares ointment: extracting solution obtained in above-mentioned steps (2) is mixed, then vacuum distillation recycling organic solvent
I, residue is ginkgo biloba p.e, obtains ginkgo leaf and extracts ointment 123.7g；
(4) it is saponified: extracting ointment to ginkgo leaf obtained in above-mentioned steps (3) and be slowly added dropwise into 15%NaOH ethanol solution
0.7L and low whipping speed are stirred continuously under conditions of being 250r/min, and heat reflux saponification, saponification temperature is 55 DEG C, saponification time
For 2h, saponification liquor is obtained；
(5) it extracts: petroleum ether 1.5L is added to saponification liquor obtained in above-mentioned steps (4), rock uniformly mixed, standing,
Layering is gradually appeared until layering no longer changes, and collection lower aqueous solution obtains thick organic slat solution, repeats extraction 3 times；
(6) semi-permeable membrane filters: concentration is slowly added dropwise less than 10% in thick organic slat solution obtained in above-mentioned steps (5)
Dilute hydrochloric acid adjusts the pH value of thick organic slat solution to neutrality, then filters, go through cellulose acetate or aromatic polyamide semi-permeable membrane
Except inorganic salts and the small substance of molecular weight, organic slat solution is obtained；
(7) concentrated spray is dry: by above-mentioned organic slat solution distillation and concentration obtained in above-mentioned steps (6), admittedly contained
Amount be 40% concentrate, concentrate through the wriggling that speed is 25rpm be pumped into inlet air temperature be 230 DEG C, leaving air temp 110
DEG C spray drying tower, by atomization frequency be 400Hz high speed atomisation device be sprayed into fine mist, connect in Ta Nei and hot wind
Rapid dry forming is touched, powdered granule is become, then cooling, wind send collection by air-introduced machine by tower bottom, obtains ginkgo biloba leaf total
Organic salt 79.5g, the Particle Size Analyzer through model SALD-2300 measure analysis, and analysis finds that grain diameter is micron order,
Grain is evenly distributed.
Nonaquepous tration is used to the ginkgo biloba leaf total organic salt in upper the present embodiment, ginkgo biloba leaf total organic salt 100mg is taken to be dissolved in
In the glacial acetic acid of 60ml, then plus the anhydrous of 30ml 0.1mol cross chloric acid titer, the 2 anhydrous gentian violet indicator of drop, stir and evenly mix,
With the anhydrous sodium acetate titer of 0.1mol with constant-current titration, after measured, the purity of ginkgo biloba leaf total organic salt is 88.4%.
Embodiment 6
In the present embodiment, a kind of preparation method of the ginkgo biloba leaf total organic salt provided, specifically includes the following steps:
(1) raw material is ground: the ginkgo leaf waste material after choosing flavones, lactone extraction, crushed after being dried, grain diameter are less than
5mm obtains ginkgo leaf powder；
(2) Soxhlet extraction: taking ginkgo leaf powder 1kg obtained in above-mentioned steps (1), n-hexane 6L is added to it, in temperature
It is Soxhlet extraction 2.5h at 65 DEG C, repeats to extract 3 times, combined extract；
(3) it prepares ointment: extracting solution obtained in above-mentioned steps (2) is mixed, then vacuum distillation recycling organic solvent
I, residue is ginkgo biloba p.e, obtains ginkgo leaf and extracts ointment 46.7g；
(4) it is saponified: extracting ointment to ginkgo leaf obtained in above-mentioned steps (3) and be slowly added dropwise into 10%NaOH ethanol solution
0.5L and low whipping speed are stirred continuously under conditions of being 100r/min, and heat reflux saponification, saponification temperature is 65 DEG C, saponification time
For 2h, saponification liquor is obtained；
(5) it extracts: petroleum ether 1L is added to saponification liquor obtained in above-mentioned steps (4), rock uniformly mixed, standing, by
Gradually there is layering until layering no longer changes, collection lower aqueous solution obtains thick organic slat solution, repeats extraction 3 times；
(6) semi-permeable membrane filters: concentration is slowly added dropwise less than 10% in thick organic slat solution obtained in above-mentioned steps (5)
Dilute hydrochloric acid adjusts the pH value of thick organic slat solution to neutrality, then filters through aromatic polyamide semi-permeable membrane, remove inorganic salts and divide
Son measures small substance, obtains organic slat solution；
(7) concentrated spray is dry: by above-mentioned organic slat solution distillation and concentration obtained in above-mentioned steps (6), admittedly contained
Amount be 33% concentrate, concentrate through the wriggling that speed is 15rpm be pumped into inlet air temperature be 200 DEG C, leaving air temp 100
DEG C spray drying tower, by atomization frequency be 250Hz high speed atomisation device be sprayed into fine mist, connect in Ta Nei and hot wind
Rapid dry forming is touched, powdered granule is become, then cooling, wind send collection by air-introduced machine by tower bottom, obtains ginkgo biloba leaf total
Organic salt 35.8g, the Particle Size Analyzer through model SALD-2300 measure analysis, and analysis finds that grain diameter is micron order
Grain, is evenly distributed.
Nonaquepous tration is used to the ginkgo biloba leaf total organic salt in upper the present embodiment, ginkgo biloba leaf total organic salt 100mg is taken to be dissolved in
In the glacial acetic acid of 60ml, then plus the anhydrous of 30ml 0.1mol cross chloric acid titer, the 2 anhydrous gentian violet indicator of drop, stir and evenly mix,
With the anhydrous sodium acetate titer of 0.1mol with constant-current titration, after measured, the purity of ginkgo biloba leaf total organic salt is 82.4%.
Embodiment 7
In the present embodiment, a kind of preparation method of the ginkgo biloba leaf total organic salt provided, specifically includes the following steps:
(1) raw material is ground: the ginkgo leaf waste material after choosing flavones, lactone extraction, crushed after being dried, grain diameter are less than
5mm obtains ginkgo leaf powder；
(2) Soxhlet extraction: taking ginkgo leaf powder 1kg obtained in above-mentioned steps (1), petroleum ether 6L is added to it, in temperature
It is Soxhlet extraction 2.5h at 65 DEG C, repeats to extract 3 times, combined extract；
(3) it prepares ointment: extracting solution obtained in above-mentioned steps (2) is mixed, then vacuum distillation recycling organic solvent
I, residue is ginkgo biloba p.e, obtains ginkgo leaf and extracts ointment 46.3g；
(4) it is saponified: extracting ointment to ginkgo leaf obtained in above-mentioned steps (3) and be slowly added dropwise into 10%NaOH ethanol solution
0.5L and low whipping speed are stirred continuously under conditions of being 100r/min, and heat reflux saponification, saponification temperature is 65 DEG C, saponification time
For 2h, saponification liquor is obtained；
(5) it extracts: petroleum ether 1L is added to saponification liquor obtained in above-mentioned steps (4), rock uniformly mixed, standing, by
Gradually there is layering until layering no longer changes, collection lower aqueous solution obtains thick organic slat solution, repeats extraction 3 times；
(6) semi-permeable membrane filters: concentration is slowly added dropwise less than 10% in thick organic slat solution obtained in above-mentioned steps (5)
Dilute hydrochloric acid adjusts the pH value of thick organic slat solution to neutrality, then filters through aromatic polyamide semi-permeable membrane, remove inorganic salts and divide
Son measures small substance, obtains organic slat solution；
(7) concentrated spray is dry: by above-mentioned organic slat solution distillation and concentration obtained in above-mentioned steps (6), admittedly contained
Amount be 33% concentrate, concentrate through the wriggling that speed is 15rpm be pumped into inlet air temperature be 200 DEG C, leaving air temp 100
DEG C spray drying tower, by atomization frequency be 250Hz high speed atomisation device be sprayed into fine mist, connect in Ta Nei and hot wind
Rapid dry forming is touched, powdered granule is become, then cooling, wind send collection by air-introduced machine by tower bottom, obtains ginkgo biloba leaf total
Organic salt 33.6g, the Particle Size Analyzer through model SALD-2300 measure analysis, and analysis finds that grain diameter is micron order
Grain, is evenly distributed.
Nonaquepous tration is used to the ginkgo biloba leaf total organic salt in upper the present embodiment, ginkgo biloba leaf total organic salt 100mg is taken to be dissolved in
In the glacial acetic acid of 60ml, then plus the anhydrous of 30ml 0.1mol cross chloric acid titer, the 2 anhydrous gentian violet indicator of drop, stir and evenly mix,
With the anhydrous sodium acetate titer of 0.1mol with constant-current titration, after measured, the purity of ginkgo biloba leaf total organic salt is 81.1%.
Through above-described embodiment 1, embodiment 4, embodiment 5, embodiment 6, embodiment 7, ethyl acetate, acetone, anhydrous is found
For ethyl alcohol as organic solvent I, the ointment yield of preparation is higher, keep the obtained ginkgo biloba leaf total organic salt yield of spray drying higher and
Purity is greater than 85%.
Embodiment 8
In the present embodiment, a kind of preparation method of the ginkgo biloba leaf total organic salt provided, specifically includes the following steps:
(1) raw material is ground: the ginkgo leaf waste material after choosing flavones, lactone extraction, crushed after being dried, grain diameter are less than
5mm obtains ginkgo leaf powder；
(2) Soxhlet extraction: taking ginkgo leaf powder 1kg obtained in above-mentioned steps (1), ethyl acetate 5L is added to it, in temperature
Degree is Soxhlet extraction 2h at 65 DEG C, repeats to extract 3 times, combined extract；
(3) it prepares ointment: extracting solution obtained in above-mentioned steps (2) is mixed, then vacuum distillation recycling organic solvent
I, residue is ginkgo biloba p.e, obtains ginkgo leaf and extracts ointment 49.7g；
(4) it is saponified: extracting ointment to ginkgo leaf obtained in above-mentioned steps (3) and be slowly added dropwise into 10%NaOH ethanol solution
0.5L and low whipping speed are stirred continuously under conditions of being 100r/min, and heat reflux saponification, saponification temperature is 65 DEG C, saponification time
For 2h, saponification liquor is obtained；
(5) it extracts: petroleum ether 1L is added to saponification liquor obtained in above-mentioned steps (4), rock uniformly mixed, standing, by
Gradually there is layering until layering no longer changes, collection lower aqueous solution obtains thick organic slat solution, repeats extraction 3 times；
(6) semi-permeable membrane filters: concentration is slowly added dropwise less than 10% in thick organic slat solution obtained in above-mentioned steps (5)
Dilute hydrochloric acid adjusts the pH value of thick organic slat solution to neutrality, then filters through nylon semi-permeable membrane, remove inorganic salts and molecular weight is small
Substance obtains organic slat solution；
(7) concentrated spray is dry: by above-mentioned organic slat solution distillation and concentration obtained in above-mentioned steps (6), admittedly contained
Amount be 33% concentrate, concentrate through the wriggling that speed is 15rpm be pumped into inlet air temperature be 200 DEG C, leaving air temp 100
DEG C spray drying tower, by atomization frequency be 250Hz high speed atomisation device be sprayed into fine mist, connect in Ta Nei and hot wind
Rapid dry forming is touched, powdered granule is become, then cooling, wind send collection by air-introduced machine by tower bottom, obtains ginkgo biloba leaf total
Organic salt 42.5g, the Particle Size Analyzer through model SALD-2300 measure analysis, and analysis finds that grain diameter is micron order,
Grain is evenly distributed.
Nonaquepous tration is used to the ginkgo biloba leaf total organic salt in upper the present embodiment, ginkgo biloba leaf total organic salt 100mg is taken to be dissolved in
In the glacial acetic acid of 60ml, then plus the anhydrous of 30ml 0.1mol cross chloric acid titer, the 2 anhydrous gentian violet indicator of drop, stir and evenly mix,
With the anhydrous sodium acetate titer of 0.1mol with constant-current titration, after measured, the purity of ginkgo biloba leaf total organic salt is 78.2%.
Through ginkgo biloba leaf total organic salt made from above-described embodiment 1, embodiment 4, embodiment 8, pass through potentiometric determination
It is lower than 80% it was found that filtering using nylon semi-permeable membrane and the organic purity salt of ginkgo biloba leaf total being made, containing inorganic salts sodium chloride, acetic acid is fine
It is high to the substances such as inorganic salts, small-molecule substance removal rate to tie up plain semi-permeable membrane, aromatic polyamide semi-permeable membrane, it is obtained to obtain ginkgo leaf
Total organic purity salt is greater than 85%.
Finally it should be noted that the above embodiments are only used to illustrate and not limit the technical solutions of the present invention, although reference
Above-described embodiment describes the invention in detail, it will be appreciated by those skilled in the art that can still carry out to the present invention
Modification or equivalent replacement should all cover without departing from the spirit or scope of the invention, or any substitutions
In scope of the presently claimed invention.
Claims (7)
1. a kind of preparation method of ginkgo biloba leaf total organic salt, which is characterized in that specifically includes the following steps:
(1) raw material is ground: the ginkgo leaf waste material after choosing flavones, lactone extraction, crushed after being dried, grain diameter are less than 5mm, obtain
To ginkgo leaf powder；
(2) I 1~10h of Soxhlet extraction of organic solvent, weight Soxhlet extraction: are added into ginkgo leaf powder obtained in above-mentioned steps (1)
It extracts 2~5 times again, combined extract；
(3) it prepares ointment: combined extract being evaporated under reduced pressure recycling organic solvent I, ginkgo leaf is obtained and extracts ointment；
(4) be saponified: to ginkgo leaf obtained in above-mentioned steps (3) extract ointment be slowly added dropwise lye and low whipping speed be 50~
It is stirred continuously under conditions of 500r/min, heat reflux saponification, saponification temperature is 40~65 DEG C, and saponification time is 1~8h, obtains soap
Change liquid；
(5) it extracts: organic solvent II is added to saponification liquor obtained in above-mentioned steps (4), rock uniformly mixed, standing, gradually
There is layering until layering no longer changes, collection lower aqueous solution obtains thick organic slat solution, repeats extraction 2~4 times；
(6) semi-permeable membrane filtering and impurity removing: dilute hydrochloric acid is slowly added dropwise to thick organic slat solution obtained in above-mentioned steps (5), tune slightly has
Then the pH value of machine salting liquid filters, the impurity such as removal inorganic salts, small-molecule substance obtain total organic to neutrality through semi-permeable membrane
Salting liquid；
(7) concentrated spray is dry: by above-mentioned organic slat solution distillation and concentration obtained in above-mentioned steps (6), obtaining solid content is
30%~40% concentrate, concentrate are pumped into spray drying tower through wriggling, are sprayed into fine mist by high speed atomisation device,
It carries out contacting rapid dry forming with hot wind in tower, becomes powdered granule, then cooling, wind send receipts by air-introduced machine by tower bottom
Collection, obtains ginkgo biloba leaf total organic salt.
2. a kind of preparation method of ginkgo biloba leaf total organic salt according to claim 1, which is characterized in that the step (7)
In the condition of spray drying be inlet air temperature be 180~230 DEG C, leaving air temp is 90~110 DEG C, charging rate is 10~
25rpm, atomization frequency are 200~400Hz.
3. a kind of preparation method of ginkgo biloba leaf total organic salt according to claim 2, which is characterized in that the step (6)
In semi-permeable membrane select cellulose acetate film or aromatic polyamide film.
4. a kind of preparation method of ginkgo biloba leaf total organic salt according to claim 3, which is characterized in that the step (2)
In organic solvent I select ethyl acetate, acetone or dehydrated alcohol any one, and dosage when extracting every time is every kilogram
5~10L is added in ginkgo leaf powder.
5. a kind of preparation method of ginkgo biloba leaf total organic salt according to claim 4, which is characterized in that the step (2)
In Extracting temperature be 40~65 DEG C.
6. a kind of preparation method of ginkgo biloba leaf total organic salt according to claim 5, which is characterized in that the step (4)
In lye select 5~20%NaOH ethanol solution, 5~20%KOH ethanol solution, 5~20%NaOH methanol solution or 5~
20%KOH methanol solution, the dosage of the lye are that every kilogram of ginkgo leaf extracts 1~20L of ointment addition.
7. a kind of preparation method of ginkgo biloba leaf total organic salt according to claim 6, which is characterized in that the step (4)
In extraction select n-hexane or petroleum ether, the body of each extractant organic solvent II and saponification liquor with organic solvent II
Product is than being 1~10:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115385753A (en) * | 2021-05-22 | 2022-11-25 | 石启田 | Method for preparing organic pesticide fertilizer by using sticky paste-shaped waste residues generated in ginkgo ketone production |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1340574A (en) * | 2000-09-03 | 2002-03-20 | 石启田 | Process for extracting yellow pigment from leftover of ginkgone |
| CN102775414A (en) * | 2012-06-12 | 2012-11-14 | 宁波立华植物提取技术有限公司 | Process for preparing sodium copper chlorophyllin from ginkgo leaf leftovers |
| CN104725387A (en) * | 2015-02-05 | 2015-06-24 | 浙江得乐康食品股份有限公司 | Preparation method for preparing sodium copper chlorophyllin from gingko leaves |
| CN109705127A (en) * | 2018-12-24 | 2019-05-03 | 南京斯拜科生化实业有限公司 | A kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin |
-
2019
- 2019-07-23 CN CN201910664020.1A patent/CN110200021A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1340574A (en) * | 2000-09-03 | 2002-03-20 | 石启田 | Process for extracting yellow pigment from leftover of ginkgone |
| CN102775414A (en) * | 2012-06-12 | 2012-11-14 | 宁波立华植物提取技术有限公司 | Process for preparing sodium copper chlorophyllin from ginkgo leaf leftovers |
| CN104725387A (en) * | 2015-02-05 | 2015-06-24 | 浙江得乐康食品股份有限公司 | Preparation method for preparing sodium copper chlorophyllin from gingko leaves |
| CN109705127A (en) * | 2018-12-24 | 2019-05-03 | 南京斯拜科生化实业有限公司 | A kind of emulsion resistance preparation method of plant source sodium copper chlorophyllin |
Non-Patent Citations (4)
| Title |
|---|
| 冯怡: "《中药固体制剂技术理论与实践》", 31 March 2017, 中国中医药出版社 * |
| 孔令义等: "《中药制药化学》", 30 April 2007, 中国医药科技出版社 * |
| 王成章等: ""银杏叶中脂肪酸的含量及化学组成"", 《林产化工通讯》 * |
| 高坤等: ""银杏叶下脚料制备叶绿素铜钠盐的工艺研究"", 《浙江万里学院学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115385753A (en) * | 2021-05-22 | 2022-11-25 | 石启田 | Method for preparing organic pesticide fertilizer by using sticky paste-shaped waste residues generated in ginkgo ketone production |
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