CN107987048A - Supercritical carbon dioxide based on the pretreatment of infrared impingement drying extracts Blueberry anthocyanidin technical method - Google Patents
Supercritical carbon dioxide based on the pretreatment of infrared impingement drying extracts Blueberry anthocyanidin technical method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
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- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
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- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention discloses the supercritical carbon dioxide pre-processed based on infrared impingement drying to extract Blueberry anthocyanidin technical method, includes the following steps：1) blueberries are subjected to mechanical compaction, obtain blueberry press cake；2) the blueberry press cake obtained in step 1) is dried using infrared impingement drying method, dry temperature is 60 75 DEG C, and the moisture in dried blueberry press cake is 15% 25%；3) it is polished to dried blueberry press cake in step 2) to use supercritical carbon dioxide extracting method, and extracted using the ethanol of hydrochloric acid acidifying as cosolvent, obtain the extract of anthocyanidin.It is dried using infrared impingement drying method, compared with other drying means, the drying time reached needed for expected drying effect is shorter.Although drying temperature Gao Shihui causes the part of anthocyanidin to damage, under shorter drying time, it is more advantageous to improving the recovery rate of anthocyanidin.
Description
Technical field
The invention belongs to natural active matter extractive technique field, is related to a kind of extracting method of blueberry anthocyanin, specifically
It is related to a kind of supercritical carbon dioxide based on the pretreatment of infrared impingement drying and extracts Blueberry anthocyanidin technical method.
Background technology
Blueberry is shrub, and every clump has result branch 25-30 bars, yields positive results within every 2 years, but yield is smaller, and there have within the 3rd year to be appropriate
Yield, enter within the 5th year high yield period, its service life is 50 years.Anthocyanidin is the nutritional supplement of pure natural anti-aging, research card
Bright is that mankind nowadays find most effective antioxidant, its antioxygenic property is higher by 50 times than vitamin E, compares vitamin C
It is higher by 200 times.Its biological effectiveness to human body is 100%, can just be detected in blood within 20 minutes after taking.Cyanine
Element is referred to as " oral cosmetics for skin ", especially blueberry anthocyanin in Europe, and skin nutrition, strengthens cutaneous immunisation power, reply
Various allergic conditions, are the most effective antioxidant of current nature.It can not only prevent generating ahead of time for wrinkle of skin,
Normal cell connection, the stabilization of blood vessel, the circulation of enhancing fine vascular, the flowing for improving capilary and vein can be also maintained, into
And reach the rapid healing of abnormal skin.Anthocyanidin is natural sunlight overcover, can prevent ultraviolet damage skin, skin
Belong to connective tissue, collagen contained therein and rigid albumen play an important role the total of skin.Anthocyanidin
Collagen can be promoted to be formed appropriately crosslinked, it can prevent skin Du " excessively crosslinking " as a kind of effective free radical scavenger
The generation of this abnormality physiological status, so as to also see the appearance of wrinkle of skin and vesica with regard to prevention, anthocyanidin can also prevent firmly
Property protease generation and suppress its activity and prevent free radical or elastase degradation hardness albumen, be obviously improved skin from inside
The health status of skin.
The content of anthocyanidin is higher than other all fruit and vegetables in blueberries, so, blueberries are good extraction days
The raw material of right anthocyanidin.Blueberry anthocyanin is soluble in acid medium, and the solubility in alcoholic solution is high and water-soluble relatively low, at present
It is to be studied in terms of extraction early period and later separation purify two mostly, extracting solution is mostly methanol.Ethanol and water it is mixed
Liquid is closed, there are the defects of organic solvent usage amount is big, technical process is more, extraction time is long, production is of high cost for this kind of method.
Method also is after blueberries are beaten, and is extracted using the ethanol solution of tartaric acid, lactic acid or acidified with citric acid.This kind
Although the time of method extraction is short, the recovery rate of anthocyanidin is relatively low in blueberry.
The preprocess method research of blueberry anthocyanin extraction is also seldom, especially effectively lifts the skill of anthocyanidin recovery rate
Art method is short of very much.
The content of the invention
For above-mentioned technical problem existing in the prior art, the object of the present invention is to provide a kind of infrared impingement drying side
The method that method promotes supercritical carbon dioxide extraction Blueberry anthocyanidin, this method pass through the indigo plant after controlling infrared impingement drying
The moisture of the certain kind of berries and the parameter of supercritical carbon dioxide, substantially increase the recovery rate of anthocyanidin in Blueberry.
In order to solve problem above, the technical scheme is that：
The method that infrared impingement drying method promotes supercritical carbon dioxide extraction Blueberry anthocyanidin, including following step
Suddenly：
1) blueberries are subjected to mechanical compaction, obtain blueberry press cake；
2) the blueberry press cake obtained in step 1) is dried using infrared impingement drying method, dry temperature is
60-75 DEG C, the moisture in dried blueberry press cake is 15%-25%；
3) it is polished to dried blueberry press cake in step 2) to use supercritical carbon dioxide extracting method, and adopt
The ethanol being acidified by the use of hydrochloric acid is extracted as cosolvent, obtains the extract of anthocyanidin.
The blueberry press cake that blueberry progress mechanical compaction obtains is more conducive to follow-up drying, is conducive to improve the equal of drying
Even property, and then be conducive to improve the recovery rate of anthocyanidin in blueberries.
It is dried using infrared impingement drying method, compared with other drying means, reaches expected drying effect institute
The drying time needed is shorter.Experiment finds that drying time seriously affects the recovery rate of anthocyanidin in blueberries, when the dry time
For 60-75 DEG C, the drying temperature compared to 40 DEG C, more can shorten drying time.Although drying temperature Gao Shihui causes anthocyanidin
Part infringement, but under shorter drying time, be more advantageous to improving the recovery rate of anthocyanidin.Experiment also found, dry
The moisture in blueberry press cake afterwards can equally influence the recovery rate of anthocyanidin, the water in dried blueberry press cake
When being divided into 15%-25%, be conducive to improve the recovery rate of anthocyanidin.
Preferably, in step 1), blueberry is stored in -20 DEG C of dark, when use thaws in 8 DEG C of dark, solves
Blueberry after jelly carries out mechanical compaction.In order to retain the anthocyanidin in blueberry to greatest extent.
It is further preferred that in step 1), pressed blueberry press cake is placed in polybag, and it is black at -20 DEG C
Preserve in the dark, until experiment is dried, by black undercover defrosting of the blueberry press cake at 8 DEG C before drying.
Preferably, in step 2), the temperature of infrared impingement drying is 65-75 DEG C, is preferably 68-72 DEG C, further preferably
For 70 DEG C.
It is further preferred that in step 2), the moisture in dried blueberry press cake is 17%-22%, preferably
For 20%.
Preferably, in step 2), 6 near-infrared radiations are housed in the oven for the infrared dryer that infrared impingement drying uses
Device, near-infrared radiator are located at the top of sample disc, and are 300mm with the distance between sample disc, and radiator is under total power
1.2 μm are produced, 2100 DEG C of peak value radiation.
Preferably, in step 3), the granularity of the polished powder of blueberry press cake is 100-300 mesh.
Preferably, in step 3), during extraction, the powder after the grinding of blueberry press cake is mixed with bead.It can prevent sample
Product lump, and can be conducive to being smoothed out for anthocyanidin extraction to avoid channelling.
Preferably, in step 3), the temperature of means of supercritical extraction is 45-55 DEG C, and the time of extraction is 45-55min, is preferably
The temperature of extraction is 50 DEG C, and the time of extraction is 50min.
It is further preferred that in step 3), when extraction, includes static extraction and Dynamic Extraction, static state extraction and Dynamic Extraction
Time ratio be 1:4, the flow velocity of cosolvent during Dynamic Extraction is 2ml/min.
Preferably, in step 3), the volume ratio of absolute ethyl alcohol, water and 37% concentrated hydrochloric acid is 50 in the cosolvent:50:1.
Beneficial effects of the present invention are：
1) it is dried using infrared impingement drying method, compared with other drying means, reaches expected drying effect
Required drying time is shorter.Experiment finds that drying time seriously affects the recovery rate of anthocyanidin in blueberries, when dry
Between be 60-75 DEG C, the drying temperature compared to 40 DEG C, more can shorten drying time.Although drying temperature Gao Shihui causes cyanine
The part infringement of element, but under shorter drying time, it is more advantageous to improving the recovery rate of anthocyanidin.Experiment also found, do
The moisture in blueberry press cake after dry can equally influence the recovery rate of anthocyanidin, when in dried blueberry press cake
When moisture is 15%-25%, be conducive to improve the recovery rate of anthocyanidin.
2) in the case where ethanol is as cosolvent, blueberry press cake is pre-processed before supercritical carbon dioxide extracting
The selection of dry technology and processing conditions has significant impact to the measurer of the anthocyanidin of extraction.Infrared impingement drying method is faced with super
When boundary's carbon dioxide abstraction coordinates, be conducive to improve the quality of the recovery rate of anthocyanidin and the anthocyanidin of extraction in blueberries.
Embodiment
It is noted that described further below is all illustrative, it is intended to provides further instruction to the application.It is unless another
Indicate, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
Embodiment 1
1 material
Moisture is the blueberry of 82-88%.
Blueberry is stored in -20 DEG C of dark.The blueberry of freezing thaws overnight in 8 DEG C of dark.By the slurry of defrosting
Fruit mechanical compaction, produces the blueberry press cake that moisture is 75% ± 1%.By filter cake be put into the polybag of sealing and-
Preserved in 20 DEG C of dark, until experiment is dried.Filter cake is thawed to 8 DEG C in the dark before the drying overnight.
2 methods
The pretreatment of blueberry press cake
Blueberry press cake is carried out under the conditions of 70 DEG C to infrared impingement drying makes its final water content be 20%, when dry
Between be 80-120min.By monitoring along dry weight loss and determining that the theoretical moisture of material contains according to this estimate
Measure to determine to reach the drying time of target moisture content.When reaching required weight loss, after drying and being cooled to room temperature,
Blueberry press cake is ground 30 seconds in knife grinding machine.Powder is placed in 50ml containers and is stored at -20 DEG C to 2 days until carrying
Take into.
The method of infrared impingement drying, includes the following steps：
1) culture dish and defrosting filter cake are placed in the centre of infrared baking oven.
2) the squeezing blueberry cake being put into two T-shaped thermocouples in each culture dish.
3) infrared dryer is used, and adding, there is gap nozzle to be connected to external fan.
4) impact is applied, air is distributed in the sample top in baking oven with the speed of 9m/s by gap nozzle.
5) 8kW/m is initially applied2Heat flux heat sample to required treatment temperature.
6) heat flux is adjusted according to the temperature monitored manually.
6 near-infrared radiators are housed in oven, above sample disc.Radiator produces 1.2 μm under total power
The peak value radiation of (2100 DEG C).The distance between the source of infrared radiation and sample disc are 300mm.
Supercritical carbon dioxide method for extracting and relevant parameter are as follows：
Coolant is water/ethanol (95%, v/v) solution (1：1).By the blueberry press cake powder that about 1g is ground and pre-processes
Weigh and mixed with bead (3mm) to prevent sample from luming and avoid channelling in 10ml extracts pond in end.Filled with bead
Extract the remaining void volume in pond.
Extraction conditions are：Pressure 350Pa, 50 DEG C of Extracting temperature are extracted, cosolvent is the ethanol solution of hydrochloric acid acidifying, its
In, the volume ratio of absolute ethyl alcohol, water and 37% concentrated hydrochloric acid is 50:50:1.
Each extraction operation carries out 50 minutes (10 minutes static, dynamic 40 minutes), 2 ml/min of flow velocity.All extractions
Current limiter temperature be all 50 DEG C.Before analysis, extract is collected in 50ml Falcon pipes, and is protected in -20 DEG C of lucifuges
Deposit.
The recovery rate of anthocyanidin is 0.6%.
Comparative example 1
With being distinguished as embodiment 1, blueberry press cake is carried out infrared impingement drying under the conditions of 70 DEG C makes it finally contain
Water is 7%.The recovery rate of anthocyanidin is 0.45%.
Comparative example 2
With being distinguished as embodiment 1, blueberry press cake is carried out infrared impingement drying under the conditions of 40 DEG C makes it finally contain
Water is 20%.The recovery rate of anthocyanidin is 0.46%.
Comparative example 3
With being distinguished as embodiment 1, blueberry press cake is carried out infra-red drying under the conditions of 70 DEG C makes its final water content
For 20%.The recovery rate of anthocyanidin is 0.4%.
Blueberry press cake is carried out infra-red drying under the conditions of 70 DEG C makes its final water content be 7%.The extraction of anthocyanidin
Rate is 0.35%.
Blueberry press cake is carried out infra-red drying under the conditions of 40 DEG C makes its final water content be 20%.The extraction of anthocyanidin
Rate is 0.36%.
Blueberry press cake is carried out infra-red drying under the conditions of 40 DEG C makes its final water content be 6%.The extraction of anthocyanidin
Rate is 0.33%.
Comparative example 4
With being distinguished as embodiment 1, blueberry press cake is dried using microwave radiation technology air drying methods, work ginseng
Number is 1000W, 200Hz, and it is 20% to make its final water content, and drying time is more than 120min.The recovery rate of anthocyanidin is
0.45%.
Blueberry press cake is dried using microwave radiation technology air drying methods, it is 7% to make its final water content.Cyanine
The recovery rate of element is 0.45%.
Comparative example 5
With being distinguished as embodiment 1, blueberry press cake is dried using freeze-drying method, makes its final water content
For 20%, the dry time is 300-900min.The recovery rate of anthocyanidin is 0.4%.
Blueberry press cake is dried using freeze-drying method, it is 7% to make its final water content.The extraction of anthocyanidin
Rate is 0.15%.
Conclusion
This result of study shows, in the case where ethanol is as cosolvent, locates in advance before supercritical carbon dioxide extracting
The selection for managing the dry technology and processing conditions of blueberry press cake has significant impact to the measurer of the anthocyanidin of extraction.In extraction
Before, drying temperature and moisture depending on filter cake.Near-infrared impingement drying is at 70 DEG C, the blueberry of 20% water content pretreatment
The anthocyanidin yield highest extracted in press cake, illustrates that the novel dried technology such as near-infrared impingement drying may be successfully used to surpass
Critical carbon dioxide extracts.Regardless of dry technology, when dry blueberry press cake water content reaches 20%, anthocyanidin yield
Content during higher than drying to 7% water content.In addition, compared with the drying at 40 DEG C, cause the flower of extract in 70 DEG C of dryings
Blue or green element yield higher.Although heat-labile compound can be preserved, vacuum freeze-drying and the novel dried skill in present invention research
Art (near-infrared impingement drying) compares the anthocyanidin yield for not showing higher.Make full use of supercritical carbon dioxide extracting
Benefit, dry pre-treatment step needs to make to measure, to ensure the extract of efficient yield and high-quality.
The advantages of infrared impingement drying：
1. infrared impingement drying is 70 DEG C in drying temperature, carried in the blueberry press cake that 20% water content pre-processes after drying
The anthocyanidin yield highest taken.
2. compared with microwave radiation technology heated-air drying, the quantity of material needed for infrared impingement drying every batch of is smaller.With infrared impact
Drying is compared, and the longer time is needed using microwave radiation technology hot-air drying technology.
3. compared with vacuum freeze drying, infrared impingement drying has higher anthocyanidin yield, and extract has efficient
Yield and high-quality.Consumed energy is few, saves the time, improves efficiency.Infrared impingement drying rapid heating technology, does with traditional
Dry Vacuum Freezing ＆ Drying Technology is compared, and greatly reduces process time.
4. in relatively infra-red drying and infrared impingement drying, 20% water content, infrared impingement drying are issued at 70 DEG C
Drying time be infra-red drying drying time half.
Influence factor
1. temperature
When the water content of considerable moisture content 7% and 20%, drying temperature are different, 70 DEG C of dryings compared with 40 DEG C of dryings,
Infrared impingement drying anthocyanidin yield higher under 70 DEG C of drying conditions.When shorter drying time is than drying longer at low temperature
Between it is more effective.
2. water content and drying time
Regardless of dry technology, blueberry press cake is done into moisture control 20%, its extract anthocyanidin obtains
Rate content squeezes the anthocyanidin yield of biscuit higher than moisture for 7% blueberry.Reason this be probably due to reaching compared with High water cut
Amount needs shorter drying time.Compared with traditional dry technology vacuum freeze drying, infrared impingement drying reduces processing
Time, it is clear that reduce drying time.The anthocyanidin that drying time and final moisture content pre-process vacuum freeze drying obtains
Rate has an impact.
The foregoing is merely the preferred embodiment of the application, the application is not limited to, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. the supercritical carbon dioxide based on the pretreatment of infrared impingement drying extracts Blueberry anthocyanidin technical method, its feature
It is：Include the following steps：
1) blueberries are subjected to mechanical compaction, obtain blueberry press cake；
2) the blueberry press cake obtained in step 1) is dried using infrared impingement drying method, dry temperature is 60-
75 DEG C, the moisture in dried blueberry press cake is 15%-25%；
3) it is polished to dried blueberry press cake in step 2) to use supercritical carbon dioxide extracting method, and use salt
The ethanol of acid acidifying is extracted as cosolvent, obtains the extract of anthocyanidin.
2. according to the method described in claim 1, it is characterized in that：In step 1), blueberry is stored in -20 DEG C of dark,
Thaw during use in 8 DEG C of dark, the blueberry after defrosting carries out mechanical compaction.
3. according to the method described in claim 2, it is characterized in that：In step 1), pressed blueberry press cake is placed on modeling
In material bag, and preserved in -20 DEG C of dark, until experiment is dried, by dark of the blueberry press cake at 8 DEG C before drying
In thaw.
4. according to the method described in claim 1, it is characterized in that：In step 2), the temperature of infrared impingement drying is 65-75
DEG C, it is preferably 68-72 DEG C, more preferably 70 DEG C.
5. according to the method described in claim 4, it is characterized in that：In step 2), the moisture in dried blueberry press cake
Content is 17%-22%, is preferably 20%.
6. according to the method described in claim 1, it is characterized in that：In step 2), infra-red drying that infrared impingement drying uses
6 near-infrared radiators are housed in the oven of device, near-infrared radiator is located at the top of sample disc, and between sample disc away from
1.2 μm are produced under total power from for 300mm, radiator, 2100 DEG C of peak value radiation.
7. according to the method described in claim 1, it is characterized in that：In step 3), the polished powder of blueberry press cake
Granularity is 100-300 mesh.
8. according to the method described in claim 7, it is characterized in that：In step 3), during extraction, the powder after the grinding of blueberry press cake
End is mixed with bead.
9. according to the method described in claim 1, it is characterized in that：In step 3), the temperature of means of supercritical extraction is 45-55 DEG C,
The time of extraction is 45-55min, and the temperature preferably extracted is 50 DEG C, and the time of extraction is 50min.
10. according to the method described in claim 1, it is characterized in that：In step 3), absolute ethyl alcohol in the cosolvent, water and
The volume ratio of 37% concentrated hydrochloric acid is 50:50:1.
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| CN111437226A (en) * | 2020-04-26 | 2020-07-24 | 合肥工业大学 | Preparation method of multi-source low-temperature extracted anthocyanin beautifying essence |
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| CN111437226A (en) * | 2020-04-26 | 2020-07-24 | 合肥工业大学 | Preparation method of multi-source low-temperature extracted anthocyanin beautifying essence |
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