CN107739305A - A kind of method for improving carnosic acid content in rosemary fat-soluble antioxidant - Google Patents
A kind of method for improving carnosic acid content in rosemary fat-soluble antioxidant Download PDFInfo
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- CN107739305A CN107739305A CN201710856154.4A CN201710856154A CN107739305A CN 107739305 A CN107739305 A CN 107739305A CN 201710856154 A CN201710856154 A CN 201710856154A CN 107739305 A CN107739305 A CN 107739305A
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Abstract
A kind of method for improving carnosic acid content in rosemary fat-soluble antioxidant, belongs to technical field of plant extraction.The present invention is using commercially available rosemary leave as raw material, by preparing rosemary extract solution, prepare carnosic acid crude extract, prepare carnosic acid refined liquid, prepare carnosic acid eluent, the step of preparing Rosmarinus officinalis extract highly finished product and preparing regeneration D370R or D315 anion-exchange resin columns, just prepares Rosmarinus officinalis extract highly finished product of the carnosic acid content more than 90%.The present invention uses the big molecular impurity in ceramic membrane separation Rosmarinus officinalis extract, and the carnosic acid of Rosmarinus officinalis extract is isolated and purified with D370R or D315 weak-base anion-exchange resins, and separation selectivity is strong, and separative efficiency is high, and recovery rate is high；The accessory substance such as useless leaf of caused rosemary, has carried out deep processing processing, has realized comprehensive utilization in implementation process, green；Operating condition is gentle, low production cost, and the product prepared can be widely applied to food, health products, medicine and other fields.
Description
First, technical field
The invention belongs to technical field of plant extraction, and in particular to one kind improves rat-tail in rosemary fat-soluble antioxidant
The method of oxalic acid content.
2nd, background technology
Rosmarinus officinalis extract is widely used natural, be widely used in medicine, health products, meat products, tobacco,
The fields such as spices, edible oil and cosmetics, it is generally acknowledged third generation natural.Its dosage increases year by year, market prospects
Well.
The main functional component of rosemary fat-soluble antioxidant is carnosic acid, carnosol.Although national standard is advised
Fixed, it is certified products that carnosic acid and carnosol content, which are more than or equal to 10%, in Rosmarinus officinalis extract, and in the market also occurs
Carnosic acid and carnosol content are respectively the product of the species such as 10%, 20%, 30%.But because impurity content is high, kind
Class is more, seriously affects the value added applications of the product.Therefore, try to reduce impurity content in Rosmarinus officinalis extract, improve
The content of carnosic acid and carnosol, turn into manufacture high-quality rosemary antioxidant and expand the key of its purposes and dosage
Place, receive significant attention.
The existing method for improving carnosic acid in rosemary fat-soluble antioxidant, such as《Chemistry of forest product and industry》Magazine
The summer field paper " carnosic acid isolates and purifies in rosemary leave " write such as beautiful, is described disclosed in the 3rd phases of volume 35 in 2015
The method that carnosic acid is isolated and purified from rosemary leave, the method are solvent with ethanol first using rosemary leave as raw material, ultrasound
Ripple assisted extraction, obtain the rosemary leaf extract that carnosic acid purity is 21.06%；Extracted again through ultrasonic assistant n-hexane
And pH is adjusted, obtain the purified that carnosic acid purity is 79.62%；Finally pass through silica gel column chromatography, prepare carnosic acid
Purity is 95.18% product.The defects of method is：1. solubility of the carnosic acid in n-hexane is low, and the dissolving of lipid
Degree is high, and therefore, lipid content is high in the product of acquisition, and carnosic acid content is low；2. n-hexane low boiling point, peculiar smell is big, in normal temperature
Lower volatilization is fast and inflammable and explosive, dangerous big；3. silica gel column regeneration needs high-temperature process, power consumption is big, pollution weight.
3rd, the content of the invention
The purpose of the present invention is to be directed to the existing weak point for isolating and purifying carnosic acid method, there is provided one kind improves fan and changed
The method of carnosic acid content in face cream soluble antioxidant.Rosmarinus officinalis extract highly finished product are prepared with the inventive method, are prepared
Process condition is gentle, good separating effect, and recovery rate is high, low production cost, non-environmental-pollution, is adapted to industrialized production.
The present invention cardinal principle be：Contain the impurity such as a large amount of polysaccharides, protide, chlorophyll in rosemary crude extract,
At normal temperatures, their solubility in the low-concentration ethanol aqueous solution are low, and useful ceramics film is efficiently separated；Carnosic acid is
Weak acid, containing free carboxy, under optimum conditions, stabilization can be formed with positively charged weak-base anion-exchange resin
Weak acid and mild base salt, so as to which other impurity are disconnected；The weak-base anion-exchange resin of load carnosic acid, in suitable bar
Under part, contacted with weak base eluent, weak base molecule then can carry out anion exchange with carnosic acid thereon, disengage it from setting
Fat, then concentrated, crystallized again, finally just prepare high-purity carnosic acid product.
The object of the present invention is achieved like this：It is a kind of to improve carnosic acid content in rosemary fat-soluble antioxidant
Method, using commercially available rosemary leave as raw material, by preparing rosemary extract solution, carnosic acid crude extract is prepared, prepares rat-tail
Oxalic acid refined liquid, prepare carnosic acid eluent, prepare Rosmarinus officinalis extract highly finished product and prepare regeneration D370R or D315 the moon from
The step of sub-exchange resin post, just prepare Rosmarinus officinalis extract highly finished product of the carnosic acid content more than 90%.Its is specific
Processing step is as follows：
(1) rosemary extract solution is prepared
According to the ratio that the ratio between rosemary leave quality and tank volume are 1: 10~13 (kg/L), rosemary leave is loaded and carried
In the stainless steel extractor of condenser.Condenser UNICOM valve is opened after closed extractor, then be passed through gauge pressure for 0.1~
0.25MPa, the saturated vapor that temperature is 100~130 DEG C, 40~120min of distillation essential oil.Steam off after the completion of distillation essential oil
Valve and condenser UNICOM valve, distillation condensate liquid and distillation slag are collected respectively.To the distillation condensate liquid of collection, for preparing
Rosemary Oil and alcohol dew.It is 1: 5~8 according to the ratio between rosemary leave quality and ethanol water volume to the distillation slag of collection
(kg/L) ratio, the ethanol water is added, the concentration expressed in percentage by volume of the ethanol water is 85~95%.Add the ethanol
After the aqueous solution, steam valve is opened, gauge pressure≤0.2MPa saturated vapor is passed through to extractor interlayer, is warming up to 65~85 DEG C,
First time extraction is carried out under agitation, and extraction time is 50~70min.After the completion of extracting for the first time, carried out in extractor thick
Filtering, collects the liquid filtered out and the filter residue being trapped respectively.To the liquid filtered out of collection, as carnosic acid carries for the first time
Liquid is taken, for preparing carnosic acid separating liquid；To the filter residue being trapped of collection, add ethanol water and carried for the second time
Take, add the concentration of alcohol of ethanol water, volume, extraction conditions with extract for the first time it is identical.After the completion of second is extracted,
Coarse filtration is carried out in extractor, collects the liquid filtered out and the filter residue being trapped respectively.To the liquid filtered out of collection, it is
Second of extract solution of carnosic acid, it is merged with carnosic acid first time extract solution, that is, prepares rosemary extract solution, is used for
Lower step prepares carnosic acid crude extract；To the filter residue being trapped of collection, for preparing Rosmarinic acid and bio-feritlizer.
(2) carnosic acid crude extract is prepared
After the completion of (1) step, the rosemary extract solution that (1) step is prepared is pumped into vacuum decker, is in gauge pressure
It is concentrated in vacuo under conditions of 0.05~0.08MPa, is stopped when in concentrate without ethanol.Concentrate and concentration are collected respectively
Condensate liquid, to the concentration condensate liquid of collection, adjust its ethanol concentration expressed in percentage by volume with absolute ethyl alcohol and reach 85~95%, can be used for
Lower batch prepares rosemary extract solution；To the concentrate of collection, carried out with the butterfly centrifugal machine that rotating speed is 3000~6000r/min
Centrifuge.Centrifugation slag and centrifugal clear liquid are collected respectively, to the centrifugal clear liquid of collection, for preparing Rosmarinic acid；To collection
Slag is centrifuged, is sent into vacuum drier, vacuum is carried out under conditions of temperature is 50~60 DEG C, gauge pressure is 0.06~0.09MPa
5~8h is dried, carnosic acid crude extract is just prepared, carnosic acid refined liquid is prepared for lower step.
(3) carnosic acid refined liquid is prepared
After the completion of (2) step, carnosic acid crude extract prepared by (2) step is sent into dissolving tank, is pumped into volume hundred
Point concentration is 50~60% ethanol waters, 15~30min of stirring and dissolving.Carnosic acid crude extract quality and concentration expressed in percentage by volume
It is 1: 10~20 (kg/L) for the ratio between 50~60% ethanol water volumes, dissolves 2 times altogether, every time dissolving ethanol water used
The volume and concentration of solution are consistent.Filtered every time after the completion of dissolving, collect filter residue and filtrate respectively, for collecting
Filter residue, predominantly polysaccharose substance, for preparing culture medium of edible fungus；To the filtrate of collection, it is 10~100nm to be pumped into aperture
Ceramic membrane filter machine in, gauge pressure be 0.2~0.6MPa under conditions of filtered, respectively collect filtered solution and filtering after
Ceramic membrane.To the filtered solution of collection, as carnosic acid refined liquid, carnosic acid eluent is prepared for lower step.To collection
Ceramic membrane after filtering, absolute ethyl alcohol is pumped into, is cleaned repeatedly, after the completion of cleaning, collect the second after cleaning ceramic film respectively
Ceramic membrane after alcohol solution and cleaning.To the ethanol water after the cleaning ceramic film of collection, for reclaiming ethanol；To collecting
Cleaning after ceramic membrane, for lower batch filter carnosic acid lysate.
(4) carnosic acid eluent is prepared
After the completion of (3) step, carnosic acid refined liquid prepared by (3) step is pumped into cloudy equipped with activation D370R or D315
In the resin column of ion exchange resin, it is 1~5 times of resin volume (BV)/h to control and be pumped into the flow velocity of liquid, ion exchange resin body
The ratio between product and the carnosic acid refined liquid volume are 1: 10~30 (L/L).It is pumped into after the completion of carnosic acid refined liquid, collects respectively
Crossing post efflux and load has the resin column of carnosic acid.Post efflux is crossed to collection, for reclaiming ethanol；To the lotus of collection
The resin column of carnosic acid is loaded with, then is pumped into the ethanol water that ethanol concentration expressed in percentage by volume is 15~35% and is washed, should
The temperature of ethanol water is 30~40 DEG C, and it is 2~4BV to be pumped into volume, and it is 1~4BV/h to be pumped into flow velocity.After the completion of washing, point
Shou Ji not cleaning solution and the resin column after washing.To the cleaning solution of collection, for reclaiming ethanol；To the resin after the washing of collection
Post, then the eluent that ethanol concentration expressed in percentage by volume is 80~95%, pH value is 9.0~10.5, volume is 4~6BV is pumped into, with 2
~4BV/h flow velocity is eluted, untill elution liquid pump is complete.1~2BV, 2.1~4.0BV and the 4.1st are collected respectively
~6.0BV eluent and the anion-exchange resin column of unloading carnosic acid.To the anion of the unloading carnosic acid of collection
Exchange resin column, regeneration D370R or D315 anion-exchange resin columns are prepared for (6) step；1~2BV to collection,
4.1~6.0BV eluent, for reclaiming ethanol；To 2.1~4.0BV of collection eluent, that is, prepare carnosic acid
Eluent, Rosmarinus officinalis extract highly finished product are prepared for lower step.
(5) Rosmarinus officinalis extract highly finished product are prepared
After the completion of (4) step, first by carnosic acid eluent prepared by (4) step with watery hydrochloric acid adjust pH value to 4~
4.5, then be pumped into vacuum concentrator, it is dense that vacuum is carried out under conditions of gauge pressure is 0.06~0.09MPa, temperature is 40~50 DEG C
Contracting, stop concentration when without ethanol.Concentration condensate and concentrate are collected respectively, to the concentration condensate of collection, containing highly concentrated
Ethanol is spent, is 50~60% ethanol waters for allocating ethanol concentration expressed in percentage by volume；To the concentrate of collection, 0~8 DEG C is placed in
Refrigerator in cool down 4~10h, refilter.Filter residue and filtrate are collected respectively, to the filtrate of collection, are pumped into wastewater disposal basin and are carried out biochemistry
Processing, discharged after up to standard；To the filter residue of collection, be sent into vacuum drier, in temperature be 50~60 DEG C, gauge pressure be 0.06~
5~8h of vacuum drying is carried out under conditions of 0.09MPa, just prepares Rosmarinus officinalis extract highly finished product.Rosmarinus officinalis extract refines
The content of carnosic acid is 90~95% in product, and carnosol content is 5~1%.The highly finished product recovery rate is that rosemary slightly carries
Take the 20~25% of amount of substance.
(6) regeneration D370R or D315 anion-exchange resin columns are prepared
After the completion of (4) step, it is pumped into the anion-exchange resin column for the unloading carnosic acid first collected to (4) step dilute
Hydrochloric acid solution, under conditions of flow velocity is pumped into as 1~4BV/h, handle 0.5~1h, HCl quality hundred wherein in dilute hydrochloric acid solution
It is 2~4% to divide concentration.After the completion of processing, the resin column after the dilute hydrochloric acid solution for flowing out the resin column and processing is collected respectively.It is right
Resin column after the processing of collection, namely regenerated D370R or D315 anion-exchange resin columns, rat-tail is prepared available for lower batch
Oxalic acid eluent；To collection outflow the resin column dilute hydrochloric acid solution, after allotment can be used for lower batch prepare regeneration D370R or
D315 anion-exchange resin columns.
The present invention is after adopting the above technical scheme, mainly have the following effects：
1st, good separating effect, recovery rate are high.The present invention uses the big molecular impurity in ceramic membrane separation Rosmarinus officinalis extract,
Separation accuracy is high；The carnosic acid of Rosmarinus officinalis extract is isolated and purified with D370R or D315 weak-base anion-exchange resins, point
Strong from selectivity, exchange capacity is more than 10 times of macroporous absorbent resin and silica gel, and separative efficiency is high；Rat-tail in the product of acquisition
Oxalic acid content is more than 90%, good separating effect；Carnosic acid recovery rate is up to more than 85%, and recovery rate is high；
2nd, comprehensive utilization is realized, it is green.In implementation process of the present invention, give up the accessory substances such as leaf to caused rosemary,
Deep processing processing has been carried out respectively, realizes comprehensive utilization；The solution type used is only ethanol water and dilute hydrochloric acid solution,
Nontoxic and peculiar smell is low, and the waste liquid after reuses after processing；Caused a small amount of waste water, the qualified discharge after biochemical treatment.
Therefore environmental pollution of the present invention is small.
3rd, the inventive method operating condition is gentle, using standardization equipment, working specification, low production cost, prepares
The product gone out can be widely applied to food, health products, medicine and other fields, and there is huge society and economy to be worth.
4th, embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment 1
A kind of method for improving carnosic acid content in rosemary fat-soluble antioxidant, its concrete technology step are as follows：
(1) rosemary extract solution is prepared
According to the ratio that the ratio between rosemary leave quality and tank volume are 1: 10 (kg/L), rosemary leave is loaded with condensation
In the stainless steel extractor of device.Condenser UNICOM valve is opened after closed extractor, then be passed through gauge pressure be 0.1MPa, temperature be
100 DEG C of saturated vapor, distillation essential oil 40min.Steam off valve and condenser UNICOM valve after the completion of distillation essential oil, respectively
Collect distillation condensate liquid and distillation slag.To the distillation condensate liquid of collection, for preparing Rosemary Oil and alcohol dew.To collection
Distillation slag, according to the ratio that the ratio between rosemary leave quality and ethanol water volume are 1: 5 (kg/L), it is water-soluble to add the ethanol
Liquid, the concentration expressed in percentage by volume of the ethanol water is 85%.After adding the ethanol water, steam valve is opened, to extractor
Interlayer is passed through the saturated vapor that gauge pressure is 0.2MPa, is warming up to 65 DEG C, carries out first time extraction under agitation, extraction time is
50min.After the completion of extracting for the first time, coarse filtration is carried out in extractor, collects the liquid filtered out and the filter residue being trapped respectively.
To the liquid filtered out of collection, as carnosic acid first time extract solution, for preparing carnosic acid separating liquid；To the quilt of collection
The filter residue of retention, add ethanol water and carry out second of extraction, add concentration of alcohol, volume, the extraction bar of ethanol water
Part with extract for the first time it is identical.After the completion of second is extracted, coarse filtration is carried out in extractor, collects the liquid filtered out respectively
With the filter residue being trapped.To the liquid filtered out of collection, as second of extract solution of carnosic acid, by itself and carnosic acid first
Secondary extract solution merges, that is, prepares rosemary extract solution, carnosic acid crude extract is prepared for lower step；Collection is trapped
Filter residue, for preparing Rosmarinic acid and bio-feritlizer.
(2) carnosic acid crude extract is prepared
After the completion of (1) step, the rosemary extract solution that (1) step is prepared is pumped into vacuum decker, is in gauge pressure
It is concentrated in vacuo under conditions of 0.05MPa, is stopped when in concentrate without ethanol.Concentrate is collected respectively and concentration condenses
Liquid, to the concentration condensate liquid of collection, adjust its ethanol concentration expressed in percentage by volume with absolute ethyl alcohol and reach 85%, available for lower batch system
Standby rosemary extract solution；To the concentrate of collection, the butterfly centrifugal machine for being 3000r/min with rotating speed is centrifuged.Respectively
Centrifugation slag and centrifugal clear liquid are collected, to the centrifugal clear liquid of collection, for preparing Rosmarinic acid；To the centrifugation slag of collection, it is sent into true
In empty drying machine, vacuum drying 5h is carried out under conditions of temperature is 50 DEG C, gauge pressure is 0.06MPa, just prepares carnosic acid
Crude extract, carnosic acid refined liquid is prepared for lower step.
(3) carnosic acid refined liquid is prepared
After the completion of (2) step, carnosic acid crude extract prepared by (2) step is sent into dissolving tank, is pumped into volume hundred
Point concentration is 50% ethanol water, stirring and dissolving 15min.Carnosic acid crude extract quality and concentration expressed in percentage by volume are 50% second
The ratio between alcohol solution volume is 1: 10 (kg/L), is dissolved 2 times altogether, every time the volume and concentration of dissolving ethanol water used
It is consistent.Filtered every time after the completion of dissolving, collect filter residue and filtrate respectively, it is predominantly more for the filter residue of collection
Glucide, for preparing culture medium of edible fungus；To the filtrate of collection, it is pumped into the ceramic membrane filter machine that aperture is 10nm,
Gauge pressure is filtered under conditions of being 0.2MPa, collects the ceramic membrane after filtered solution and filtering respectively.To the filtered solution of collection, i.e.,
For carnosic acid refined liquid, carnosic acid eluent is prepared for lower step.To the ceramic membrane after the filtering of collection, anhydrous second is pumped into
Alcohol, cleaned repeatedly, after the completion of cleaning, collect the ethanol water after cleaning ceramic film and the ceramic membrane after cleaning respectively.
To the ethanol water after the cleaning ceramic film of collection, for reclaiming ethanol；To the ceramic membrane after the cleaning of collection, for lower batch
Secondary filtering carnosic acid lysate.
(4) carnosic acid eluent is prepared
After the completion of (3) step, carnosic acid refined liquid prepared by (3) step is pumped into and handed over equipped with activation D370R anion
Change in the resin column of resin, it is 1 times of resin volume (BV)/h to control and be pumped into the flow velocity of liquid, ion exchange resin volume and the rat-tail
The ratio between oxalic acid refined liquid volume is 1: 10 (L/L).It is pumped into after the completion of carnosic acid refined liquid, collected post efflux and lotus respectively
It is loaded with the resin column of carnosic acid.Post efflux is crossed to collection, for reclaiming ethanol：There is carnosic acid to the load of collection
Resin column, then be pumped into the ethanol water that ethanol concentration expressed in percentage by volume is 15% and washed, the temperature of the ethanol water is
30 DEG C, it is 2BV to be pumped into volume, and it is 1BV/h to be pumped into flow velocity.After the completion of washing, the resin column after cleaning solution and washing is collected respectively.
To the cleaning solution of collection, for reclaiming ethanol；To the resin column after the washing of collection, then it is pumped into ethanol concentration expressed in percentage by volume and is
80%th, the eluent that pH value 9.0, volume are 4BV, eluted with 2BV/h flow velocity, untill elution liquid pump is complete.Point
Not Shou Ji 1~2BV, 2.1~4.0BV and 4.1~6.0BV eluent and unload carnosic acid anion exchange tree
Fat post.To the anion-exchange resin column of the unloading carnosic acid of collection, prepare regeneration D370R anion for (6) step and hand over
Change resin column；The eluent of 1~2BV, 4.1~6.0BV to collection, for reclaiming ethanol；To the 2.1st of collection~
4.0BV eluent, that is, carnosic acid eluent is prepared, Rosmarinus officinalis extract highly finished product are prepared for lower step.
(5) Rosmarinus officinalis extract highly finished product are prepared
After the completion of (4) step, carnosic acid eluent prepared by (4) step is first adjusted into pH value to 4, then pump with watery hydrochloric acid
Enter in vacuum concentrator, be concentrated in vacuo under conditions of gauge pressure is 0.06MPa, temperature is 40 DEG C, stopped when without ethanol
Only concentrate.Concentration condensate and concentrate are collected respectively, to the concentration condensate of collection, containing high concentration ethanol, for allocating second
Alcohol concentration expressed in percentage by volume is 50% ethanol water；To the concentrate of collection, it is placed in 0~8 DEG C of refrigerator and cools down 4h, after
Filter.Filter residue and filtrate are collected respectively, to the filtrate of collection, are pumped into wastewater disposal basin and are carried out biochemical treatment, discharged after up to standard；To collection
Filter residue, it is sent into vacuum drier, vacuum drying 5h is carried out under conditions of temperature is 50 DEG C, gauge pressure is 0.06MPa, just prepares
Go out Rosmarinus officinalis extract highly finished product.The content of carnosic acid is 90~95% in Rosmarinus officinalis extract highly finished product, and carnosol contains
Measure as 5~1%.The highly finished product recovery rate is the 20~25% of rosemary crude extract quality.
(6) regeneration D370R anion-exchange resin columns are prepared
After the completion of (4) step, it is pumped into the anion-exchange resin column for the unloading carnosic acid first collected to (4) step dilute
Hydrochloric acid solution, under conditions of flow velocity is pumped into as 1BV/h, handle 0.5h, HCl mass percentage concentration wherein in dilute hydrochloric acid solution
For 2%.After the completion of processing, the resin column after the dilute hydrochloric acid solution for flowing out the resin column and processing is collected respectively.To the place of collection
Resin column after reason, namely regenerated D370R anion-exchange resin columns, carnosic acid eluent is prepared available for lower batch；It is right
The dilute hydrochloric acid solution of the outflow of the collection resin column, can be used for lower batch to prepare regeneration D370R anion exchange resin after allotment
Post.
Embodiment 2
A kind of method for improving carnosic acid content in rosemary fat-soluble antioxidant, its concrete technology step are as follows：
(1) rosemary extract solution is prepared
According to the ratio that the ratio between rosemary leave quality and tank volume are 1: 12 (kg/L), rosemary leave is loaded with condensation
In the stainless steel extractor of device.Condenser UNICOM valve is opened after closed extractor, then be passed through gauge pressure be 0.2MPa, temperature be
115 DEG C of saturated vapor, distillation essential oil 80min.Steam off valve and condenser UNICOM valve after the completion of distillation essential oil, respectively
Collect distillation condensate liquid and distillation slag.To the distillation condensate liquid of collection, for preparing Rosemary Oil and alcohol dew.To collection
Distillation slag, according to the ratio that the ratio between rosemary leave quality and ethanol water volume are 1: 6 (kg/L), it is water-soluble to add the ethanol
Liquid, the concentration expressed in percentage by volume of the ethanol water is 90%.After adding the ethanol water, steam valve is opened, to extractor
Interlayer is passed through the saturated vapor that gauge pressure is 0.2MPa, is warming up to 75 DEG C, carries out first time extraction under agitation, extraction time is
60min.After the completion of extracting for the first time, coarse filtration is carried out in extractor, collects the liquid filtered out and the filter residue being trapped respectively.
To the liquid filtered out of collection, as carnosic acid first time extract solution, for preparing carnosic acid separating liquid；To the quilt of collection
The filter residue of retention, add ethanol water and carry out second of extraction, add concentration of alcohol, volume, the extraction bar of ethanol water
Part with extract for the first time it is identical.After the completion of second is extracted, coarse filtration is carried out in extractor, collects the liquid filtered out respectively
With the filter residue being trapped.To the liquid filtered out of collection, as second of extract solution of carnosic acid, by itself and carnosic acid first
Secondary extract solution merges, that is, prepares rosemary extract solution, carnosic acid crude extract is prepared for lower step；Collection is trapped
Filter residue, for preparing Rosmarinic acid and bio-feritlizer.
(2) carnosic acid crude extract is prepared
After the completion of (1) step, the rosemary extract solution that (1) step is prepared is pumped into vacuum decker, is in gauge pressure
It is concentrated in vacuo under conditions of 0.06MPa, is stopped when in concentrate without ethanol.Concentrate is collected respectively and concentration condenses
Liquid, to the concentration condensate liquid of collection, adjust its ethanol concentration expressed in percentage by volume with absolute ethyl alcohol and reach 90%, available for lower batch system
Standby rosemary extract solution；To the concentrate of collection, the butterfly centrifugal machine for being 5000r/min with rotating speed is centrifuged.Respectively
Centrifugation slag and centrifugal clear liquid are collected, to the centrifugal clear liquid of collection, for preparing Rosmarinic acid；To the centrifugation slag of collection, it is sent into true
In empty drying machine, vacuum drying 6h is carried out under conditions of temperature is 55 DEG C, gauge pressure is 0.08MPa, just prepares carnosic acid
Crude extract, carnosic acid refined liquid is prepared for lower step.
(3) carnosic acid refined liquid is prepared
After the completion of (2) step, carnosic acid crude extract prepared by (2) step is sent into dissolving tank, is pumped into volume hundred
Point concentration is 55% ethanol water, stirring and dissolving 25min.Carnosic acid crude extract quality and concentration expressed in percentage by volume are 55% second
The ratio between alcohol solution volume is 1: 15 (kg/L), is dissolved 2 times altogether, every time the volume and concentration of dissolving ethanol water used
It is consistent.Filtered every time after the completion of dissolving, collect filter residue and filtrate respectively, it is predominantly more for the filter residue of collection
Glucide, for preparing culture medium of edible fungus；To the filtrate of collection, it is pumped into the ceramic membrane filter machine that aperture is 50nm,
Gauge pressure is filtered under conditions of being 0.4MPa, collects the ceramic membrane after filtered solution and filtering respectively.To the filtered solution of collection, i.e.,
For carnosic acid refined liquid, carnosic acid eluent is prepared for lower step.To the ceramic membrane after the filtering of collection, anhydrous second is pumped into
Alcohol, cleaned repeatedly, after the completion of cleaning, collect the ethanol water after cleaning ceramic film and the ceramic membrane after cleaning respectively.
To the ethanol water after the cleaning ceramic film of collection, for reclaiming ethanol；To the ceramic membrane after the cleaning of collection, for lower batch
Secondary filtering carnosic acid lysate.
(4) carnosic acid eluent is prepared
After the completion of (3) step, carnosic acid refined liquid prepared by (3) step is pumped into equipped with activation D315 anion exchanges
In the resin column of resin, it is 3 times of resin volume (BV)/h to control and be pumped into the flow velocity of liquid, ion exchange resin volume and the Salvia japonica
The ratio between acid treating liquid product is 1: 20 (L/L).It is pumped into after the completion of carnosic acid refined liquid, collected post efflux and load respectively
There is the resin column of carnosic acid.Post efflux is crossed to collection, for reclaiming ethanol；There is the tree of carnosic acid to the load of collection
Fat post, then be pumped into the ethanol water that ethanol concentration expressed in percentage by volume is 25% and washed, the temperature of the ethanol water is 35
DEG C, it is 3BV to be pumped into volume, and it is 3BV/h to be pumped into flow velocity.After the completion of washing, the resin column after cleaning solution and washing is collected respectively.It is right
The cleaning solution of collection, for reclaiming ethanol；To the resin column after the washing of collection, then it is pumped into ethanol concentration expressed in percentage by volume and is
90%th, the eluent that pH value 10, volume are 5BV, eluted with 3BV/h flow velocity, untill elution liquid pump is complete.Respectively
Collect 1~2BV, 2.1~4.0BV and 4.1~6.0BV eluent and unloading carnosic acid anion exchange resin
Post.To the anion-exchange resin column of the unloading carnosic acid of collection, regeneration D315 anion exchange trees are prepared for (6) step
Fat post；The eluent of 1~2BV, 4.1~6.0BV to collection, for reclaiming ethanol；To 2.1~4.0BV of collection
Eluent, that is, prepare carnosic acid eluent, Rosmarinus officinalis extract highly finished product prepared for lower step.
(5) Rosmarinus officinalis extract highly finished product are prepared
After the completion of (4) step, carnosic acid eluent prepared by (4) step is first adjusted into pH value to 4.2 with watery hydrochloric acid, then
It is pumped into vacuum concentrator, is concentrated in vacuo under conditions of gauge pressure is 0.08MPa, temperature is 45 DEG C, when without ethanol
Stop concentration.Concentration condensate and concentrate are collected respectively, to the concentration condensate of collection, containing high concentration ethanol, for allocating
Ethanol concentration expressed in percentage by volume is 55% ethanol water；To the concentrate of collection, it is placed in 0~8 DEG C of refrigerator and cools down 7h, after
Filter.Filter residue and filtrate are collected respectively, to the filtrate of collection, are pumped into wastewater disposal basin and are carried out biochemical treatment, discharged after up to standard；To collection
Filter residue, it is sent into vacuum drier, vacuum drying 6h is carried out under conditions of temperature is 55 DEG C, gauge pressure is 0.08MPa, just prepares
Go out Rosmarinus officinalis extract highly finished product.The content of carnosic acid is 90~95% in Rosmarinus officinalis extract highly finished product, and carnosol contains
Measure as 5~1%.The highly finished product recovery rate is the 20~25% of rosemary crude extract quality.
(6) regeneration D315 anion-exchange resin columns are prepared
After the completion of (4) step, it is pumped into the anion-exchange resin column for the unloading carnosic acid first collected to (4) step dilute
Hydrochloric acid solution, under conditions of flow velocity is pumped into as 2BV/h, handle 0.5h, HCl mass percentage concentration wherein in dilute hydrochloric acid solution
For 3%.After the completion of processing, the resin column after the dilute hydrochloric acid solution for flowing out the resin column and processing is collected respectively.To the place of collection
Resin column after reason, namely regenerated D315 anion-exchange resin columns, carnosic acid eluent is prepared available for lower batch；To receiving
The dilute hydrochloric acid solution of the outflow of the collection resin column, can be used for lower batch to prepare regeneration D315 anion-exchange resin columns after allotment.
Embodiment 3
A kind of method for improving carnosic acid content in rosemary fat-soluble antioxidant, its concrete technology step are as follows：
(1) rosemary extract solution is prepared
According to the ratio that the ratio between rosemary leave quality and tank volume are 1: 13 (kg/L), rosemary leave is loaded with condensation
In the stainless steel extractor of device.Condenser UNICOM valve is opened after closed extractor, then be passed through gauge pressure be 0.25MPa, temperature be
130 DEG C of saturated vapor, distillation essential oil 120min.Steam off valve and condenser UNICOM valve after the completion of distillation essential oil, point
Condensate liquid and distillation slag Shou Ji not distilled.To the distillation condensate liquid of collection, for preparing Rosemary Oil and alcohol dew.To collecting
Distillation slag, according to the ratio between rosemary leave quality and ethanol water volume be 1: 8 (kg/L) ratio, it is water-soluble to add the ethanol
Liquid, the concentration expressed in percentage by volume of the ethanol water is 95%.After adding the ethanol water, steam valve is opened, to extractor
Interlayer is passed through the saturated vapor that gauge pressure is 0.2MPa, is warming up to 85 DEG C, carries out first time extraction under agitation, extraction time is
70min.After the completion of extracting for the first time, coarse filtration is carried out in extractor, collects the liquid filtered out and the filter residue being trapped respectively.
To the liquid filtered out of collection, as carnosic acid first time extract solution, for preparing carnosic acid separating liquid；To the quilt of collection
The filter residue of retention, add ethanol water and carry out second of extraction, add concentration of alcohol, volume, the extraction bar of ethanol water
Part with extract for the first time it is identical.After the completion of second is extracted, coarse filtration is carried out in extractor, collects the liquid filtered out respectively
With the filter residue being trapped.To the liquid filtered out of collection, as second of extract solution of carnosic acid, by itself and carnosic acid first
Secondary extract solution merges, that is, prepares rosemary extract solution, carnosic acid crude extract is prepared for lower step；Collection is trapped
Filter residue, for preparing Rosmarinic acid and bio-feritlizer.
(2) carnosic acid crude extract is prepared
After the completion of (1) step, the rosemary extract solution that (1) step is prepared is pumped into vacuum decker, is in gauge pressure
It is concentrated in vacuo under conditions of 0.08MPa, is stopped when in concentrate without ethanol.Concentrate is collected respectively and concentration condenses
Liquid, to the concentration condensate liquid of collection, adjust its ethanol concentration expressed in percentage by volume with absolute ethyl alcohol and reach 95%, available for lower batch system
Standby rosemary extract solution；To the concentrate of collection, the butterfly centrifugal machine for being 6000r/min with rotating speed is centrifuged.Respectively
Centrifugation slag and centrifugal clear liquid are collected, to the centrifugal clear liquid of collection, for preparing Rosmarinic acid；To the centrifugation slag of collection, it is sent into true
In empty drying machine, vacuum drying 8h is carried out under conditions of temperature is 60 DEG C, gauge pressure is 0.09MPa, just prepares carnosic acid
Crude extract, carnosic acid refined liquid is prepared for lower step.
(3) carnosic acid refined liquid is prepared
After the completion of (2) step, carnosic acid crude extract prepared by (2) step is sent into dissolving tank, is pumped into volume hundred
Point concentration is 60% ethanol water, stirring and dissolving 30min.Carnosic acid crude extract quality and concentration expressed in percentage by volume are 60% second
The ratio between alcohol solution volume is 1: 20 (kg/L), is dissolved 2 times altogether, every time the volume and concentration of dissolving ethanol water used
It is consistent.Filtered every time after the completion of dissolving, collect filter residue and filtrate respectively, it is predominantly more for the filter residue of collection
Glucide, for preparing culture medium of edible fungus；To the filtrate of collection, it is pumped into the ceramic membrane filter machine that aperture is 100nm,
Gauge pressure is filtered under conditions of being 0.6MPa, collects the ceramic membrane after filtered solution and filtering respectively.To the filtered solution of collection, i.e.,
For carnosic acid refined liquid, carnosic acid eluent is prepared for lower step.To the ceramic membrane after the filtering of collection, anhydrous second is pumped into
Alcohol, cleaned repeatedly, after the completion of cleaning, collect the ethanol water after cleaning ceramic film and the ceramic membrane after cleaning respectively.
To the ethanol water after the cleaning ceramic film of collection, for reclaiming ethanol；To the ceramic membrane after the cleaning of collection, for lower batch
Secondary filtering carnosic acid lysate.
(4) carnosic acid eluent is prepared
After the completion of (3) step, carnosic acid refined liquid prepared by (3) step is pumped into and handed over equipped with activation D370R anion
Change in the resin column of resin, it is 5 times of resin volume (BV)/h to control and be pumped into the flow velocity of liquid, ion exchange resin volume and the rat-tail
The ratio between oxalic acid refined liquid volume is 1: 30 (L/L).It is pumped into after the completion of carnosic acid refined liquid, collected post efflux and lotus respectively
It is loaded with the resin column of carnosic acid.Post efflux is crossed to collection, for reclaiming ethanol；There is carnosic acid to the load of collection
Resin column, then be pumped into the ethanol water that ethanol concentration expressed in percentage by volume is 35% and washed, the temperature of the ethanol water is
40 DEG C, it is 4BV to be pumped into volume, and it is 4BV/h to be pumped into flow velocity.After the completion of washing, the resin column after cleaning solution and washing is collected respectively.
To the cleaning solution of collection, for reclaiming ethanol；To the resin column after the washing of collection, then it is pumped into ethanol concentration expressed in percentage by volume and is
95%th, the eluent that pH value 10.5, volume are 6BV, eluted with 4BV/h flow velocity, untill elution liquid pump is complete.Point
Not Shou Ji 1~2BV, 2.1~4.0BV and 4.1~6.0BV eluent and unload carnosic acid anion exchange tree
Fat post.To the anion-exchange resin column of the unloading carnosic acid of collection, prepare regeneration D370R anion for (6) step and hand over
Change resin column；The eluent of 1~2BV, 4.1~6.0BV to collection, for reclaiming ethanol；To the 2.1st of collection~
4.0BV eluent, that is, carnosic acid eluent is prepared, Rosmarinus officinalis extract highly finished product are prepared for lower step.
(5) Rosmarinus officinalis extract highly finished product are prepared
After the completion of (4) step, carnosic acid eluent prepared by (4) step is first adjusted into pH value to 4.5 with watery hydrochloric acid, then
It is pumped into vacuum concentrator, is concentrated in vacuo under conditions of gauge pressure is 0.09MPa, temperature is 50 DEG C, when without ethanol
Stop concentration.Concentration condensate and concentrate are collected respectively, to the concentration condensate of collection, containing high concentration ethanol, for allocating
Ethanol concentration expressed in percentage by volume is 60% ethanol water；To the concentrate of collection, it is placed in 0~8 DEG C of refrigerator and cools down 10h, then
Filtering.Filter residue and filtrate are collected respectively, to the filtrate of collection, are pumped into wastewater disposal basin and are carried out biochemical treatment, discharged after up to standard；To collecting
Filter residue, be sent into vacuum drier in, carry out vacuum drying 8h under conditions of temperature is 60 DEG C, gauge pressure is 0.09MPa, just make
It is standby go out Rosmarinus officinalis extract highly finished product.The content of carnosic acid is 90~95% in Rosmarinus officinalis extract highly finished product, carnosol
Content is 5~1%.The highly finished product recovery rate is the 20~25% of rosemary crude extract quality.
(6) regeneration D370R anion-exchange resin columns are prepared
After the completion of (4) step, it is pumped into the anion-exchange resin column for the unloading carnosic acid first collected to (4) step dilute
Hydrochloric acid solution, under conditions of flow velocity is pumped into as 4BV/h, 1h is handled, wherein HCl mass percentage concentration is in dilute hydrochloric acid solution
4%.After the completion of processing, the resin column after the dilute hydrochloric acid solution for flowing out the resin column and processing is collected respectively.Processing to collection
Resin column afterwards, namely regenerated D370R anion-exchange resin columns, carnosic acid eluent is prepared available for lower batch；To receiving
The dilute hydrochloric acid solution of the outflow of the collection resin column, can be used for lower batch to prepare regeneration D370R anion-exchange resin columns after allotment.
Claims (1)
- A kind of 1. method for improving carnosic acid content in rosemary fat-soluble antioxidant, it is characterised in that specific technique step It is rapid as follows：(1) rosemary extract solution is preparedAccording to the ratio that the ratio between rosemary leave quality and tank volume are 1: 10~13 (kg/L), rosemary leave is loaded with condensation Condenser UNICOM valve is opened in the stainless steel extractor of device, after closed extractor, then is passed through gauge pressure as 0.1~0.25MPa, temperature The saturated vapor for 100~130 DEG C is spent, distills 40~120min of essential oil, distills steam off valve and condensation after the completion of essential oil Device UNICOM valve, distillation condensate liquid and distillation slag is collected respectively, to the distillation condensate liquid of collection, for preparing Rosemary Oil Reveal with alcohol, to the distillation slag of collection, according to the ratio that the ratio between rosemary leave quality and ethanol water volume are 1: 5~8 (kg/L) Example, the ethanol water being added, the concentration expressed in percentage by volume of the ethanol water is 85~95%, after adding the ethanol water, Steam valve is opened, gauge pressure≤0.2MPa saturated vapor is passed through to extractor interlayer, 65~85 DEG C is warming up to, enters under agitation Row extracts for the first time, and extraction time is 50~70min, after the completion of extracting for the first time, coarse filtration is carried out in extractor, is received respectively Collect the liquid filtered out and the filter residue being trapped, to the liquid filtered out of collection, as carnosic acid first time extract solution, for making Standby carnosic acid separating liquid；To the filter residue being trapped of collection, add ethanol water and carry out second of extraction, add ethanol water The concentration of alcohol of solution, volume, extraction conditions with extracting for the first time identical, after the completion of second is extracted, enter in extractor Row coarse filtration, the liquid filtered out and the filter residue being trapped are collected respectively, to the liquid filtered out of collection, as carnosic acid second Secondary extract solution, it is merged with carnosic acid first time extract solution, that is, prepares rosemary extract solution, rat-tail is prepared for lower step Oxalic acid crude extract；To the filter residue being trapped of collection, for preparing Rosmarinic acid and bio-feritlizer；(2) carnosic acid crude extract is preparedAfter the completion of (1) step, the rosemary extract solution that (1) step is prepared is pumped into vacuum decker, is 0.05 in gauge pressure It is concentrated in vacuo under conditions of~0.08MPa, is stopped when in concentrate without ethanol, is collected concentrate respectively and concentration condenses Liquid, to the concentration condensate liquid of collection, adjust its ethanol concentration expressed in percentage by volume with absolute ethyl alcohol and reach 85~95%, available for lower batch It is secondary to prepare rosemary extract solution；To the concentrate of collection, centrifuged with the butterfly centrifugal machine that rotating speed is 3000~6000r/min Separation, centrifugation slag and centrifugal clear liquid is collected respectively, to the centrifugal clear liquid of collection, for preparing Rosmarinic acid；Centrifugation to collection Slag, it is sent into vacuum drier, vacuum drying 5 is carried out under conditions of temperature is 50~60 DEG C, gauge pressure is 0.06~0.09MPa ~8h, carnosic acid crude extract is just prepared, carnosic acid refined liquid is prepared for lower step；(3) carnosic acid refined liquid is preparedAfter the completion of (2) step, carnosic acid crude extract prepared by (2) step is sent into dissolving tank, and it is dense to be pumped into volume basis It is 50 with concentration expressed in percentage by volume to spend for 50~60% ethanol waters, 15~30min of stirring and dissolving, carnosic acid crude extract quality The ratio between~60% ethanol water volume is 1: 10~20 (kg/L), is dissolved 2 times altogether, every time dissolving ethanol water used Volume and concentration be consistent, filtered every time after the completion of dissolving, filter residue and filtrate collected respectively, for the filter of collection Slag, predominantly polysaccharose substance, for preparing culture medium of edible fungus；To the filtrate of collection, the pottery that aperture is 10~100nm is pumped into In porcelain Membrane filtering machine, filtered under conditions of gauge pressure is 0.2~0.6MPa, collect the ceramics after filtered solution and filtering respectively Film, to the filtered solution of collection, as carnosic acid refined liquid, carnosic acid eluent is prepared for lower step, the filtering to collection Ceramic membrane afterwards, absolute ethyl alcohol is pumped into, is cleaned repeatedly, after the completion of cleaning, collect the ethanol water after cleaning ceramic film respectively Ceramic membrane after solution and cleaning, to the ethanol water after the cleaning ceramic film of collection, for reclaiming ethanol；To the clear of collection Ceramic membrane after washing, carnosic acid lysate is filtered for lower batch；(4) carnosic acid eluent is preparedAfter the completion of (3) step, carnosic acid refined liquid prepared by (3) step is pumped into equipped with activation D370R or D315 anion In the resin column of exchanger resin, it is 1~5 times of resin volume (BV)/h to control and be pumped into the flow velocity of liquid, ion exchange resin volume with The ratio between the carnosic acid refined liquid volume is 1: 10~30 (L/L), is pumped into after the completion of carnosic acid refined liquid, collected post respectively Efflux and load have the resin column of carnosic acid, post efflux are crossed to collection, for reclaiming ethanol；Have to the load of collection The resin column of carnosic acid, then be pumped into the ethanol water that ethanol concentration expressed in percentage by volume is 15~35% and washed, the ethanol The temperature of the aqueous solution is 30~40 DEG C, and it is 2~4BV to be pumped into volume, and it is 1~4BV/h to be pumped into flow velocity, after the completion of washing, is received respectively Collect the resin column after cleaning solution and washing, to the cleaning solution of collection, for reclaiming ethanol；To the resin column after the washing of collection, The eluent that ethanol concentration expressed in percentage by volume is 80~95%, pH value is 9.0~10.5, volume is 4~6BV is pumped into again, with 2~ 4BV/h flow velocity is eluted, until elution liquid pump it is complete untill, respectively collect 1~2BV, 2.1~4.0BV and the 4.1st~ 6.0BV eluent and the anion-exchange resin column of unloading carnosic acid, are handed over the anion of the unloading carnosic acid of collection Resin column is changed, regeneration D370R or D315 anion-exchange resin columns are prepared for (6) step；1~2BV to collection, 4.1~6.0BV eluent, for reclaiming ethanol；To 2.1~4.0BV of collection eluent, that is, prepare carnosic acid Eluent, Rosmarinus officinalis extract highly finished product are prepared for lower step；(5) Rosmarinus officinalis extract highly finished product are preparedAfter the completion of (4) step, carnosic acid eluent prepared by (4) step is first adjusted into pH value to 4~4.5 with watery hydrochloric acid, then It is pumped into vacuum concentrator, is concentrated in vacuo under conditions of gauge pressure is 0.06~0.09MPa, temperature is 40~50 DEG C, directly Stop concentration during to without ethanol, collect concentration condensate and concentrate, to the concentration condensate of collection, second containing high concentration respectively Alcohol, it is 50~60% ethanol waters for allocating ethanol concentration expressed in percentage by volume；To the concentrate of collection, 0~8 DEG C of ice is placed in 4~10h is cooled down in case, is refiltered, collects filter residue and filtrate respectively, to the filtrate of collection, wastewater disposal basin is pumped into and carries out biochemical treatment, Discharged after up to standard；To the filter residue of collection, be sent into vacuum drier, in temperature be 50~60 DEG C, gauge pressure be 0.06~0.09MPa Under conditions of carry out 5~8h of vacuum drying, just prepare Rosmarinus officinalis extract highly finished product, rat-tail in Rosmarinus officinalis extract highly finished product The content of oxalic acid is 90~95%, and carnosol content is 5~1%, and the highly finished product recovery rate is rosemary crude extract quality 20~25%；(6) regeneration D370R or D315 anion-exchange resin columns are preparedAfter the completion of (4) step, watery hydrochloric acid is pumped into the anion-exchange resin column for the unloading carnosic acid first collected to (4) step Solution, under conditions of flow velocity is pumped into as 1~4BV/h, 0.5~1h is handled, HCl quality percentage is dense wherein in dilute hydrochloric acid solution Spend for 2~4%, after the completion of processing, the resin column after the dilute hydrochloric acid solution for flowing out the resin column and processing is collected respectively, to collecting Processing after resin column, namely regenerated D370R or D315 anion-exchange resin columns, carnosic acid is prepared available for lower batch Eluent；To the dilute hydrochloric acid solution of the outflow of the collection resin column, lower batch can be used for prepare regeneration D370R or D315 after allotment Anion-exchange resin column.
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| CN114702378A (en) * | 2022-05-10 | 2022-07-05 | 南京泛成生物科技有限公司 | Method for preparing rosemary extract by using two-aqueous-phase extraction method |
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| CN113461518A (en) * | 2021-07-07 | 2021-10-01 | 云南胜天生物科技有限公司 | Method for extracting and preparing high-purity carnosic acid from rosemary by using deep eutectic solvent |
| CN114702378A (en) * | 2022-05-10 | 2022-07-05 | 南京泛成生物科技有限公司 | Method for preparing rosemary extract by using two-aqueous-phase extraction method |
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