CN108129584A - It is a kind of to realize pectin and flavones while the method for extraction in citrus peel residue - Google Patents
It is a kind of to realize pectin and flavones while the method for extraction in citrus peel residue Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
- C08B37/0048—Processes of extraction from organic materials
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
Abstract
Pectin and flavones while the method for extraction in citrus peel residue are realized the invention discloses a kind of.This method comprises the following steps：(1) citrus peel residue addition water is extracted, obtains extracting solution；The extracting solution is centrifuged, obtains supernatant and residue；(2) by the supernatant ultrafiltration, efflux and trapped fluid are obtained；The efflux is evaporated, obtains flavone glycoside；By the trapped fluid alcohol precipitation, precipitated；By the precipitation drying, pectin is obtained；(3) residue addition organic solvent is extracted, obtains extracting solution；The extracting solution is centrifuged, supernatant is collected, is evaporated, obtains fat-soluble flavones.The method of the present invention can realize pectin and flavones while high efficiency extraction in citrus peel residue, environmental pollution caused by effectively solving the problems, such as skin slag waste and waste, realize the comprehensive utilization of citrus peel residue, the exploitation also for pectin and flavones Related product provides important raw material sources simultaneously, has huge economic benefit and social benefit.
Description
Technical field
Pectin and flavones while the method for extraction in citrus peel residue are realized the present invention relates to a kind of, belong to agricultural byproducts processing
Technical field.
Background technology
Citrus is that the fruit of cultivated area and yield maximum, the yield of wherein China's citrus occupy first place in the world in the world, year
Equal output is up to 35,000,000 tons.At present, citrus industry can generate a large amount of skin slag by-product mainly based on juice processed, and China is every
The citrus peel residue that year generates due to processing is more than 7,000,000 tons.Multiple efficacies ingredient is rich in these by-products, development prospect is wide
It is wealthy.But these by-products often do as rubbish and are burned or abandoned at present, not only cause environmental pollution and huge
The wasting of resources.Therefore there is an urgent need for developing the effect of effective processing technology is extracted in citrus peel residue ingredient, its added value is improved.
The highest functional component of content is pectin in citrus peel residue, and content is the 10%~30% and 2% of orange peel dry weight
Left and right.Citrus is the productive first-elected pectin source of tool.Natural citrus pectin is used generally as food additives, is had very
It is good be gelled, stablize, emulsifying, thickening, suspension function.Pectin is also that pure natural aqueous soluble dietary without any side effects is fine
Dimension can promote enterogastric peristalsis, promote nutrient absorption.Pectin can also be combined with the heavy metal in blood and then it is promoted to discharge body
Outside.In addition, the substance can also increase immune function and adjust immunologic derangement, cholesterol prevention of arterial atherosis is reduced, drops blood
Fat, blood glucose treat and prevent endomorphy type fatty liver, treat kinds cancer.Therefore, citrus pectin can be widely used in preparation enhancing
Drug, food and the health products of immune function.At present in industrialized production, mainly extracted using sour water, although simple for process,
But equipment is corroded greatly, and largely discarded sour water can be generated, difficult, there are serious problem of environmental pollutions.Also there is text
It offers and discloses a variety of other extracting methods, such as (1) alkali extraction method, in this method extraction process, pectin demethylation speed is fast, methoxy
Base content is reduced, and easy depolymerization；(2) microbial method, although without heat or acid processing, low energy consumption, pollution is small, to temperature and
The requirement of the conditions such as pH is harsh；(3) enzyme process, same to microbial method, without heat treatment and soda acid processing, but the reaction time is long, enzyme system
Agent dosage is larger, and enzyme is easy to inactivate；(4) other, the common extracting method of pectin also has the methods of microwave radiation technology and excusing from death auxiliary,
Compared with conventional method, although these methods can significantly improve extraction efficiency, shorten extraction time, these method energy consumptions
Greatly, it is of high cost, it is unfavorable for industrialized production.CN 103204954A disclose a kind of utilization microwave continuous adverse current extraction dregs of a decoction fruit
The method of glue, but be also to be extracted using sour water, and need to add in cellulase and cellulose-degrading bacteria, to environmental condition requirement
The use of harshness, easy in inactivation, while microwave increases energy consumption and cost.
Another high-content functional component is flavones in citrus peel residue, accounts for 2% or so of orange peel dry weight.Numerous researchs
Show that flavones has the nutrient healths work(such as significant anticancer, anti-inflammatory, anti-oxidant, anti-platelet aggregation, norcholesterol and antibacterial
Can, in consideration of it, tangeritin can be widely used in the exploitation of functional food, market prospects are considerable.Flavonoid at present
The extraction generally use solvent extraction of object, common extracting method have Microwave Extraction and ultrasonic wave extraction, and extraction time is short, extraction
It is efficient, but such method energy consumption is of high cost greatly；Although Enzymatic Extraction mild condition, stringent controlling reaction temperature is needed
And pH value, equipment requirement are high.This three classes method pollutes environment and there are residue problems usually with organic solvent simultaneously.It is in addition, super
Critical carbon dioxide is also used for the extraction of flavones, and this method is simple for process, recovery rate is high, organic solvent-free residual, but molten
Agent range of choice is narrow, and equipment requirement is higher, and cost of investment is high.
Meanwhile the extraction of single component is often confined to for the extraction of citrus functional component at present, in residual residue still
Containing a large amount of functional component, the great wasting of resources is still caused.CN 106188183A disclose one kind and join from pomelo peel
The method for closing extraction naringin and pectin, but this method needs strong acid and strong base, equipment is corroded greatly, waste water is difficult, exists
Serious problem of environmental pollution, and it is complex for operation step, time-consuming (being up to 43 hours), is not suitable for industrialized production；CN
105754014A discloses a kind of method of pectin and polyphenol in sub-critical extraction orange peel, and this method needs high pressure, and energy consumption is big,
And equipment is expensive, it is of high cost；CN 105669800A disclose it is a kind of by enzymolysis, it is strong-acid cation-exchange resin, ultrafiltration, cold
Be lyophilized dry, macroreticular resin and etc. from citrus the method for combined extracting essential oil, pectin, aurantiamarin, synephrine and limonin,
This method is also to extract pectin, and complex steps with sour water, is unsuitable for industrialized production.
Invention content
Pectin and flavones while the method for extraction, this method institute in citrus peel residue are realized the object of the present invention is to provide a kind of
It is conventional equipment with equipment, working condition is mildly easily achieved, and is effectively solved in current citrus industry, and skin slag waste draws
The Heavy environmental pollution and waste problem risen, realizes the comprehensive utilization of citrus peel residue.
It is provided by the invention a kind of to extract pectin and flavones (flavone glycoside and fat-soluble flavones) in citrus peel residue simultaneously
Method includes the following steps：
(1) citrus peel residue addition water is extracted, obtains extracting solution；The extracting solution is centrifuged, obtain supernatant and
Residue；
(2) by the supernatant ultrafiltration, efflux and trapped fluid are obtained；The efflux is evaporated, obtains flavone glycoside；
By the trapped fluid alcohol precipitation, precipitated；By the precipitation drying, pectin is obtained；
(3) residue addition organic solvent is extracted, obtains extracting solution；The extracting solution is centrifuged, in collection
Clear liquid is evaporated, and obtains fat-soluble flavones.
In above-mentioned preparation method, in step (1), the citrus peel residue can be orange peel or citrus peel meal；
The citrus peel residue is citrus peel meal；The method may also include by orange peel freeze before the extraction and do
It is dry and be crushed to the step of citrus peel meal is made in 100~150 mesh (such as 100 mesh).
In above-mentioned preparation method, in step (1), the method may also include before the extraction to citrus peel residue into
The step of row destroy the enzyme treatment.The step of destroy the enzyme treatment, can be as follows：The citrus peel residue is placed in boiling water and is handled, is obtained
Citrus peel residue after to enzyme deactivation.The ratio of the citrus peel residue and the boiling water can be 1g：(1~3) mL, concretely 1g：
1mL；Processing time can be 10~20min, concretely 15min.
The extraction can be that adverse current is extracted, and concretely continuous dynamic countercurrent extracts.In the extraction step, the citrus
The ratio of skin slag and water can be 1g：(10~30) mL (such as 1g：15mL、1g：30mL、1g：15~30mL), Extracting temperature can be 25
~50 DEG C (such as 35~50 DEG C, 35 DEG C or 50 DEG C), extraction time can be 30~90min (such as 30~40min, 30min or
40min)。
The rotating speed of the centrifugation can be 8000~15000r/min, concretely 5000r/min；Time can be 6~
20min, concretely 10min.
Above-mentioned preparation method, in step (2), in the ultrafiltration step, ultrafiltration membrane is ceramic membrane；The retention of ultrafiltration membrane point
Sub- amount >=5KDa, concretely 5~10KDa, 5KDa or 10KDa；The volume ratio of efflux and trapped fluid can be (3~10)：1,
Concretely (6~10)：1、6：1 or 10：1.
In the alcohol precipitation step, the volume ratio of the trapped fluid and ethyl alcohol can be 1：(1~8), concretely 1：(2~8),
1：2 or 1：8.
The drying can be drying；The temperature of the drying is 30~45 DEG C, and concretely 35 DEG C, the time is 3~8h, is had
Body can 3~5h, 3h or 5h.
The method it is described be evaporated in step further include recycle-water and described in step (1) in extraction step it is again sharp
The step of using；
The method further included in the alcohol precipitation step recycling ethyl alcohol and described in step (3) in extraction step again
The step of utilization.
Above-mentioned preparation method, in step (3), the extraction can be that adverse current is extracted, and concretely continuous dynamic countercurrent carries
It takes, can countercurrently extract described in step (1) and be extracted in extractor used.The organic solvent is ethyl alcohol.It is described to carry
It takes in step, the ratio of the residue and the organic solvent is 1g：(10~15) mL (such as 1g：10mL or 1g：15mL), it extracts
Temperature is 15~30 DEG C (such as 25 DEG C), and extraction time is 30~60min, concretely 30min.
The rotating speed of the centrifugation can be 8000~15000r/min, concretely 5000r/min；Time can be 6~
20min, concretely 10min.
The method it is described be evaporated in step further include recycling ethyl alcohol and in step (2) and/or step (3) it is again sharp
The step of using.
The method of pectin and flavones while high efficiency extraction in citrus peel residue can be realized the invention discloses a kind of.Due to not
Same kind, the place of production, maturity orange peel in, pectin content difference is very big, and therefore, it is difficult to be compared with the result reported
Compared with, identical raw material of the invention, the method common in design document, yield is higher is carried out at the same time experiment, with more different
The extraction efficiency of method.The result shows that being extracted with common high temperature sour water and Ultrasonic Heating, method therefor of the present invention is in extraction time
On the basis of shortening 40%, the recovery rate of pectin can significantly improve 16.9%~39.4%；The recovery rate of flavone glycoside improves
1.2~6.8 times；The recovery rate of lipophilicity flavones is suitable with Ultrasonic Heating extraction, even higher, is that common high temperature sour water extracts
1.1~6.4 times.This method can also realize the grading extraction of flavones in citrus peel residue.In addition, the advantage of this method also resides in nothing
Acid-base condition is needed, it is small to equipment corrosion；Normal temperature and pressure, energy consumption are small；It is simple for process, it is easy to operate；Solvent only has water and ethyl alcohol,
Pollution-free, solvent is recyclable, recycles, at low cost, suitable for industrialized production.Orange peel can be realized by the method
Pectin and flavones while high efficiency extraction, greatly improve its added value, effectively solve in current citrus industry, skin slag is discarded in slag
Heavy environmental pollution caused by object and waste problem realize the comprehensive utilization of citrus peel residue, while also related to flavones for pectin
The exploitation of product provides important raw material sources, has huge economic benefit and social benefit.
Description of the drawings
Fig. 1 is pectin and flavones while the process flow chart of extraction in citrus peel residue of the present invention.
Fig. 2 is the HPLC analysis charts of flavone glycoside, wherein, Fig. 2 (A) is the standard curve (range of linearity 0.125 of orange peel mandarin orange
~2.0mg/mL)；Fig. 2 (B) is flavone glycoside HPLC analysis charts under the red tangerine various extracting conditions in ten thousand states.
Fig. 3 is catechin canonical plotting used in Determination of Total Flavonoids.
Fig. 4 is the standard curve of pectin content.
Fig. 5 is the fat-soluble flavones HPLC analyses (the red tangerine in ten thousand states) of Different Extraction Method.
Specific embodiment
Following embodiment is intended to further illustrate the present invention rather than limitation of the present invention, all are based on institute of the present invention
The improvement made is all within the scope of the present invention.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
The method that flavone glycoside is measured using HPLC methods, is as follows：From the flavone glycoside (being denoted as Mmg) of extraction
In, it weighs certain flavone glycoside crude product and (is denoted as mIt is to be measuredMg), it is made into the methanol solution (being denoted as V mL) of 1.5mg/mL, stationary phase
For C18 columns, mobile phase forms (B), elution requirement by 1 ‰ sour water (A) and acetonitrile：0~2min, 90%A；5min, 80%A；
15min, 65%A；25min, 5%A；26min, 5%A；26.1~30min, 90%A.The calculating of the recovery rate of general flavone glucosides
Formula is as follows：V*M* (peak area -419.54)/[mIt is to be measured* 12037* citrus peel residues quality * (1- moisture content)].
The content of pectin is measured using ultraviolet spectrophotometer method, is as follows：A certain amount of pectin is weighed (to be denoted as
mIt is to be measuredMg it) is placed in 100mL volumetric flasks, adds in 5.0mL sodium hydroxide solutions (1.0mol/L), scale is settled to deionized water
Line, mixing at least prevent 15min, and sway frequently, and filtering retains filtrate, for colorimetric estimation.Pipette 1.0mL pectin samples
Liquid is in 25mL teat glass；It is another pipette each concentration of 1.0mL respectively galacturonic acid standard serial solution (20.0mg/L,
40.0mg/L, 60.0mg/L, 80.0mg/L, 100.0mg/L) in teat glass.It is respectively added in sample and standard solution
0.1% carbazole of 0.25mL-ethanol solution generates white flock precipitate, constantly shakes test tube, then rapidly join 5.0mL
Test tube is put into 85 DEG C of water bath chaders heats 20min at once by sulfuric acid, is put into after taking-up in originally water-bath and is allowed to rapid cold
But, its absorbance is measured at 525nm wavelength with spectrophotometer within the 1.5h times, drafting standard curve is relatively more quantitative (to be pressed
The above method does blank test simultaneously, with blank tune 0).The calculation formula of the recovery rate of pectin is as follows：100*M(APectin+
0.0176)/[0.001*mIt is to be measured* citrus peel residue quality * (1- moisture content)].
By the content of the fat-soluble general flavone of alchlor colorimetric method for determining, it is as follows：From general flavone crude product (note
For m1G) m is weighed in2Mg adds in suitable 80% methanol water dissolution (V mL), after suitably diluting certain multiple, 1mL is taken to be added to
In test tube with cover, add in 4mL distilled water and be uniformly mixed, then add in 0.3mL 5%NaNO2Solution, 0.3mL 10%AlCl3It is molten
Liquid, mixing.6min is stood, the NaOH solution of 2mL 1mol/L is added in, 10mL is settled to distilled water, measures and inhales at 510nm
Luminosity.Above-mentioned sample equivalent is changed into the catechin of various concentration (0,5,100,150,200,250,300 and 350mg/L),
Its operating procedure is identical, using 80% methanol aqueous solution as blank control, draws standard curve.The recovery rate of fat-soluble general flavone
Calculation formula is as follows：(absorbance+0.0003) * V*m1* extension rate/[0.0003*m2* (1- is aqueous by citrus peel residue quality *
Rate)].
In embodiment 1, the red tangerine orange peel in ten thousand states pectin and (continuous dynamic countercurrent extraction) is extracted while flavones
Pectin and flavones in the red tangerine orange peel in ten thousand states are extracted simultaneously according to flow chart shown in Fig. 1, are as follows：
(1) the fresh red tangerine orange peel (moisture content 71%) in ten thousand states is freeze-dried and is crushed, it is new to obtain 100 purposes
Fresh orange peel ground-slag；After the fresh orange peel ground-slags of 1000kg are boiled 15min progress destroy the enzyme treatments in 1000L boiling water, input
Into continuous dynamic countercurrent extractor, with solid-liquid ratio 1：15 (1g orange peel ground-slags：15mL water) distilled water is inversely inputted, and keep carrying
The temperature for taking pipe is 35 DEG C, extracts 90min, obtains orange peel extracting solution；Obtained orange peel extracting solution is transported in centrifugal device,
10min is centrifuged with the speed of 5000r/min, obtains supernatant and orange peel residue；
(2) supernatant that step (1) obtains is conveyed into ultrafiltration apparatus, using the filter membrane (ceramic membrane) of 10kDa, to centrifugation
Liquid carries out 6 times of ultrafiltration, and (volume ratio of efflux and trapped fluid is 6：1) trapped fluid and efflux, are obtained；By efflux using rotation
Turn evaporimeter to be evaporated to solid, obtain flavone glycoside crude product, recycle-water extracts for next batch；Trapped fluid is added in into 2 times of volumes
Ethanol precipitation, and washed with the ethyl alcohol of 2 times of volumes and be precipitated to white, separation of solid and liquid is realized in centrifugation, will be deposited at 35 DEG C and is dried
Dry 3h obtains pectin；Meanwhile ethyl alcohol recycling is spare；
(3) the orange peel residue that step (1) obtains is transmitted back to adverse current extraction element again, the second that step (2) is recycled
Alcohol is inversely input in adverse current extraction element, using solid-liquid ratio as 1：15 (1g orange peel residues：15mL ethyl alcohol), room temperature (25 DEG C) carries
30min is taken, obtains extracting solution；Extracting solution is input in centrifugal device, the condition of same step (1), centrifuged, using rotary evaporation
Centrifugate is evaporated to solid by instrument, obtains fat-soluble general flavone, and recycling ethyl alcohol is used for the operation of next batch.
According to said determination method measure respectively pectin, flavone glycoside and fat-soluble general flavone content and calculate extraction
Rate.Fig. 2 is the HPLC analysis charts of flavone glycoside, wherein.Fig. 2 (A) be orange peel mandarin orange standard curve (range of linearity 0.125~
2.0mg/mL)；Fig. 2 (B) is flavone glycoside HPLC analysis charts under the red tangerine various extracting conditions in ten thousand states.Fig. 3 is Determination of Total Flavonoids institute
With catechin canonical plotting.Fig. 4 is the standard curve of pectin content.Fig. 5 is Different Extraction Method under Detection wavelength 340nm
The HPLC analyses (the red tangerine in ten thousand states) of fat-soluble flavones.Pectin, flavone glycoside and the fat-soluble general flavone that the present embodiment extracts
Recovery rate be shown in Table 1.
In reference examples 1-1, the red tangerine orange peel in ten thousand states pectin and (extraction of high temperature sour water) is extracted while flavones
(1) the fresh red tangerine orange peel (moisture content 71%) in ten thousand states is freeze-dried and is crushed, it is new to obtain 100 purposes
Fresh orange peel ground-slag；After the fresh orange peel ground-slags of 200g are boiled 15min progress destroy the enzyme treatments in 200mL boiling water, with feed liquid
Than 1：15 add in the aqueous solution of salt acid for adjusting pH 2.0, and at 80 DEG C, stirring extraction 50min obtains orange peel extracting solution；By what is obtained
Orange peel extracting solution is transported in centrifugal device, is centrifuged 10min with the speed of 5000r/min, is obtained supernatant and orange peel residue；
(2) with embodiment 1.
(3) residue for obtaining step (1) is with solid-liquid ratio 1g：15mL adds in ethyl alcohol, and 35 DEG C, 50min, ethyl alcohol are extracted in stirring
It is evaporated, obtains fat-soluble general flavone crude product.
According to said determination method measure respectively pectin, flavone glycoside and fat-soluble general flavone content and calculate extraction
Rate.Fig. 2 is the HPLC analysis charts of flavone glycoside, wherein.Fig. 2 (A) be orange peel mandarin orange standard curve (range of linearity 0.125~
2.0mg/mL)；Fig. 2 (B) is flavone glycoside HPLC analysis charts under the red tangerine various extracting conditions in ten thousand states.Fig. 3 is Determination of Total Flavonoids institute
With catechin canonical plotting.Fig. 4 is the standard curve of pectin content.Fig. 5 is Different Extraction Method under Detection wavelength 340nm
The HPLC analyses (the red tangerine in ten thousand states) of fat-soluble flavones.Pectin, flavone glycoside and the fat-soluble general flavone that this reference examples is extracted
Recovery rate be shown in Table 1.
In reference examples 1-2, the red tangerine orange peel in ten thousand states pectin and (Ultrasonic Heating extraction) is extracted while flavones
(1) the fresh red tangerine orange peel (moisture content 71%) in ten thousand states is freeze-dried and is crushed, it is new to obtain 100 purposes
Fresh orange peel ground-slag；After the fresh orange peel ground-slags of 200g are boiled 15min progress destroy the enzyme treatments in 200mL boiling water, with feed liquid
Than 1：30 add in distilled water, and 75 DEG C, ultrasonic extraction 30min under 45kHz obtains orange peel extracting solution；The orange peel extracting solution that will be obtained
It is transported in centrifugal device, 10min is centrifuged with the speed of 5000r/min, obtains supernatant and orange peel residue；
(2) with embodiment 1.
(3) the orange peel residue for obtaining step (1) is with solid-liquid ratio 1g：15mL adds in ethyl alcohol, 35 DEG C, ultrasonic under 45kHz
50min is extracted, ethyl alcohol is evaporated, and obtains fat-soluble general flavone crude product.
According to said determination method measure respectively pectin, flavone glycoside and fat-soluble general flavone content and calculate extraction
Rate.Fig. 2 is the HPLC analysis charts of flavone glycoside, wherein.Fig. 2 (A) be orange peel mandarin orange standard curve (range of linearity 0.125~
2.0mg/mL)；Fig. 2 (B) is flavone glycoside HPLC analysis charts under the red tangerine various extracting conditions in ten thousand states.Fig. 3 is Determination of Total Flavonoids institute
With catechin canonical plotting.Fig. 4 is the standard curve of pectin content.Fig. 5 is Different Extraction Method under Detection wavelength 340nm
The HPLC analyses (the red tangerine in ten thousand states) of fat-soluble flavones.Pectin, flavone glycoside and the fat-soluble general flavone that this reference examples is extracted
Recovery rate be shown in Table 1.
Table 1 statistics indicate that, continuous dynamic countercurrent extraction, high temperature sour water extraction and Ultrasonic Heating extraction in pectin recovery rate
Respectively 19.8%, 12.0% and 17.2% (shorten 40%), continuous dynamic countercurrent extracting method within the relatively short time
The recovery rate of pectin can be significantly improved 39.4% and 15.1%.
HPLC analysis results (Fig. 2) show in flavone glycoside that (ten thousand state used is red in terms of dry weight mainly based on orange peel mandarin orange
The moisture content of tangerine is that 72%), during adverse current is extracted, the recovery rate of orange peel mandarin orange is 10.8mg/g, and common high temperature sour water extracts and super
The recovery rate of acoustic heating only has 1.6mg/g and 5.4mg/g respectively, is 6.8 times of the latter and 2.0 times (tables 2).
When HPLC analysis results (Fig. 4) show flavones fat-soluble as solvent extraction using ethyl alcohol, in terms of dry weight, adverse current is extracted
Recovery rate it is suitable with the recovery rate that Ultrasonic Heating extracts, respectively 68.2mg/g and 69.3mg/g, be high temperature sour water extraction
6.4~6.5 times of (10.6mg/g).In addition, using the characteristic absorption peak 340nm of flavones as Detection wavelength, to carried flavones crude product
Carry out HPLC analyses, the results showed that, fat-soluble flavones is substantially free of flavonoid glycoside, mainly yellow with the longer lipophilicity of retention time
Based on ketone.
In embodiment 2, south jiangxi navel orange orange peel pectin and (continuous dynamic countercurrent extraction) is extracted while flavones
Pectin and flavones in south jiangxi navel orange orange peel are extracted simultaneously according to flow chart shown in Fig. 1, are as follows：
(1) the fresh south jiangxi navel orange orange peels (moisture content 75%) of 1000kg are boiled 15min in 1000L boiling water to go out
It after enzymatic treatment, is input in continuous dynamic countercurrent extractor, with solid-liquid ratio 1：30 (1g orange peel slags：30mL water) inversely input distillation
Water, and it is 50 DEG C to keep the temperature of extraction tube, extracts 30min, obtains orange peel extracting solution；Obtained orange peel extracting solution is transported to
In centrifugal device, 10min is centrifuged with the speed of 5000r/min, obtains supernatant and orange peel residue；
(2) supernatant that step (1) obtains is conveyed into ultrafiltration apparatus, using the filter membrane (ceramic membrane) of 5kDa, to centrifugation
Liquid carries out 10 times of ultrafiltration, and (volume ratio of efflux and trapped fluid is 10：1) trapped fluid and efflux, are obtained；Efflux is used
Rotary Evaporators are evaporated to solid, obtain flavone glycoside crude product, and recycle-water extracts for next batch；Trapped fluid is added in into 8 times of bodies
Long-pending ethanol precipitation, and washed with the ethyl alcohol of 2 times of volumes and be precipitated to white, separation of solid and liquid is realized in centrifugation, will be deposited at 35 DEG C
Drying 3h obtains pectin；Meanwhile ethyl alcohol recycling is spare；
(3) the orange peel residue that step (1) obtains is transmitted back to adverse current extraction element again, the second that step (2) is recycled
Alcohol is inversely input in adverse current extraction element, using solid-liquid ratio as 1：10 (1g orange peel residues：10mL ethyl alcohol), room temperature (25 DEG C) carries
30min is taken, obtains extracting solution；Extracting solution is input in centrifugal device, the condition of same step (1), centrifuged, using rotary evaporation
Centrifugate is evaporated to solid by instrument, obtains fat-soluble general flavone, and recycling ethyl alcohol is used for the operation of next batch.
The recovery rate of pectin, flavone glycoside and fat-soluble general flavone that the present embodiment extracts is shown in Table 1.
In reference examples 2-1, south jiangxi navel orange orange peel pectin and (extraction of high temperature sour water) is extracted while flavones
The red tangerine in ten thousand states in reference examples 1-1 is only replaced with south jiangxi navel orange by experimental procedure with reference examples 1-1.
The recovery rate of pectin, flavone glycoside and fat-soluble general flavone that this reference examples is extracted is shown in Table 1.
In reference examples 2-2, south jiangxi navel orange orange peel pectin and (Ultrasonic Heating extraction) is extracted while flavones
The red tangerine in ten thousand states in reference examples 1-2 is only replaced with south jiangxi navel orange by experimental procedure with reference examples 1-2.
The recovery rate of pectin, flavone glycoside and fat-soluble general flavone that this reference examples is extracted is shown in Table 1.
The result shows that the recovery rate of pectin divides in continuous dynamic countercurrent extraction, the extraction of high temperature sour water and Ultrasonic Heating extraction
Not Wei 15.9%, 8.2% and 13.6%, compared to common extraction, (shorten 40%) within the relatively short time, continuous dynamic
The recovery rate of pectin can be significantly improved 93.9% and 16.9% by countercurrent extraction method.
HPLC analysis results show in flavone glycoside mainly based on orange peel mandarin orange, and (south jiangxi navel orange used contains in terms of dry weight
Water rate is 75%), during adverse current is extracted, the recovery rate of orange peel mandarin orange is 10.6mg/g, and common high temperature sour water extraction and Ultrasonic Heating
Recovery rate there was only 7.8mg/g and 9.2mg/g respectively, be 1.4 times of the latter and 1.2 times (tables 1).
Fat-soluble determination of total flavonoids the result shows that, it is inverse in terms of dry weight during flavones fat-soluble as solvent extraction using ethyl alcohol
The recovery rate highest of extraction is flowed, is 35.8mg/g, is high temperature sour water extraction (24.3mg/g) and Ultrasonic Heating extraction respectively
1.5 and 1.1 times of (31.9mg/g).HPLC analysis results show that fat-soluble flavones is substantially free of flavonoid glycoside, mainly to retain when
Between based on longer lipophilicity flavones.
Under table 1, Different Extraction Method, the recovery rate of pectin and flavones in the red tangerine in ten thousand states and south jiangxi navel orange
Claims (10)
1. method that is a kind of while extracting pectin in citrus peel residue, flavone glycoside and fat-soluble flavones, includes the following steps：
(1) citrus peel residue addition water is extracted, obtains extracting solution；The extracting solution is centrifuged, obtains supernatant and residue；
(2) by the supernatant ultrafiltration, efflux and trapped fluid are obtained；The efflux is evaporated, obtains flavone glycoside；By institute
Trapped fluid alcohol precipitation is stated, is precipitated；By the precipitation drying, pectin is obtained；
(3) residue addition organic solvent is extracted, obtains extracting solution；The extracting solution is centrifuged, collects supernatant,
It is evaporated, obtains fat-soluble flavones.
2. according to the method described in claim 1, it is characterized in that：In step (1), the citrus peel residue is orange peel or mandarin orange
Orange peel powder；
The citrus peel residue is citrus peel meal；The method further includes before the extraction and is freeze-dried orange peel simultaneously
It is crushed to the step of citrus peel meal is made in 100~150 mesh.
3. method according to claim 1 or 2, it is characterised in that：In step (1), the method is before the extraction
Further include the step of destroy the enzyme treatment is carried out to the citrus peel residue；And/or
The step of destroy the enzyme treatment, is as follows：The citrus peel residue is placed in boiling water and is handled, obtains the citrus after enzyme deactivation
Skin slag；And/or
The ratio of the citrus peel residue and the boiling water is 1g：(1~3) mL, processing time are 10~20min.
4. method according to any one of claim 1-3, it is characterised in that：In step (1), the adverse current that is extracted as carries
It takes；And/or
The adverse current is extracted as continuous dynamic countercurrent extraction；And/or
In the extraction step, the ratio of the citrus peel residue and water is 1g：(10~30) mL, Extracting temperature are 25~50 DEG C,
Extraction time is 30~90min.
5. according to the described method of any one of claim 1-4, it is characterised in that：In step (1), the rotating speed of the centrifugation is
8000~15000r/min, time are 6~20min.
6. method according to any one of claims 1-5, it is characterised in that：In step (2), in the ultrafiltration step,
Ultrafiltration membrane is ceramic membrane；Molecular cut off >=5KDa of ultrafiltration membrane；The volume ratio of efflux and trapped fluid is (3~10)：1.
7. according to the method described in any one of claim 1-6, it is characterised in that：In step (2), in the alcohol precipitation step,
The volume ratio of the trapped fluid and ethyl alcohol is 1：(1~8)；And/or
The drying is drying；The temperature of the drying is 30~45 DEG C, and the time is 3~8h.
8. according to the described method of any one of claim 1-7, it is characterised in that：In step (2), the method is in the steaming
The step of recycle-water being further included in dry step and being re-used in extraction step described in step (1)；
The method further includes recycling ethyl alcohol in the alcohol precipitation step and is re-used in extraction step described in step (3)
The step of.
9. according to the method described in any one of claim 1-8, it is characterised in that：In step (3), the adverse current that is extracted as carries
It takes；And/or
The adverse current is extracted as continuous dynamic countercurrent extraction；And/or
The organic solvent is ethyl alcohol；And/or
In the extraction step, the ratio of the residue and the organic solvent is 1g：(10~15) mL, Extracting temperature for 15~
30 DEG C, extraction time is 30~60min.
10. according to the method described in any one of claim 1-9, it is characterised in that：In step (3), the rotating speed of the centrifugation
For 8000~15000r/min；Time is 6~20min；And/or
The method is evaporated recycling ethyl alcohol is further included in step and is re-used in step (2) and/or step (3) described
Step.
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