CN107652372A - A kind of orange peel pectin without alcohol extracting method - Google Patents
A kind of orange peel pectin without alcohol extracting method Download PDFInfo
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- CN107652372A CN107652372A CN201711015743.6A CN201711015743A CN107652372A CN 107652372 A CN107652372 A CN 107652372A CN 201711015743 A CN201711015743 A CN 201711015743A CN 107652372 A CN107652372 A CN 107652372A
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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
- 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
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
What it is the invention discloses a kind of orange peel pectin is without alcohol extracting method, step：A, orange peel pre-processes：After cleaning up plus boiling is boiled, and is dried, is crushed, obtain citrus peel meal；B, extract：Citrus peel meal is placed in beaker, with salt acid for adjusting pH, beaker is placed in thermostat water bath and heated, and stirring, obtains mixture；C, centrifuge：Mixture is centrifuged, obtains the extract solution containing pectin；D, purify：Caseinic acid is added according to the volume ratio of extract solution and casein sodium to receive, is centrifuged, and obtains the sediment of pectin and casein sodium；E, purify；Sediment is transferred in distilled water, after adding sodium chloride, the pH value of solution is adjusted, pectin is obtained in supernatant；F, drying：Pectin is subjected to vacuum freeze drying, obtains orange peel pectin.Energy consumption is big, production cost is high, product colour is deep, the quality problems such as peculiar smell be present when solving in traditional handicraft big ethanol consumption, recovery, and easy to implement the method, easy to operate, working condition is gentle, product purity height.
Description
Technical field
The invention belongs to fruit-vegetable food processing technique field, be more particularly to a kind of orange peel pectin without alcohol extracting method.
Background technology
Pectin is the part of plant cell wall, is a kind of plant polyose of abundance, generally extract from apple and
Orange peel, it is often used as food industry thickener, stabilizer, gelling agent, emulsifying agent, drug delivery vehicle.Generally, pectin by
300 to 1000 monosaccharide molecule compositions, form the monose of pectin based on galacturonic acid, additionally contain arabinose, Portugal
Other monose such as grape sugar, galactolipin, rhamnose, it is a kind of heteroglycan.
The method of extraction purification pectin mainly includes alcohol precipitation, dialysis, salt precipitation and membrane separation process.Alcohol precipitation
Separate pectin, be the characteristics of not dissolving in alcohols solvent using pectin, and some dissociate neutral oligosaccharides and polysaccharide it is molten in alcohol
Solution degree is poor, can be with pectin co-precipitation in alcohol.Salting out method purifying pectin makees precipitating reagent frequently with aluminium salt or high price molysite etc.,
Using free carboxy in pectin with the characteristic with the salt ion opposite charges in salting liquid, precipitation is produced by neutralization.
Precipitated metal can remove free neutral sugar, can also remove partially protein.But obtained pectin product ash content is high, dissolving
Property is poor, and color and luster is deeper, and process conditions are difficult to control.UF membrane has energy consumption low, and operating procedure is simple, and alternative removes fruit
Sugar and oligomer in glue extract solution, so as to improve the quality of glue.But film is difficult to cleaning and easily blocked, price is also more
Costliness, membrane separation technique is set to be difficult to popularize.The purification process generally used still needs further improvement.
The interaction of protein-pectin is usually used to as emulsion stabilizer, as natural full fat food substitute or
Half substitute, as meat products analog, edibility film and medicine bioengineering prosthese, protein purification etc..Casein sodium is pure
Change pectin mainly due to the electrostatic interaction between both polymer.Compound action between casein sodium and pectin
Rely on and the pH and ionic strength in reaction medium.By probing into influence of the various factors to reaction, to obtain optimal purifying fruit
The condition of glue.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, is to be the provision of one kind for above-mentioned problem
Caseinic acid receive purifying pectin method, it is easy to implement the method, it is easy to operate, using casein sodium purify pectin, solve tradition
Ethanol consumption is big in technique, recovery when energy consumption is big, production cost is high, product colour is deep, the technical problems such as peculiar smell be present, production bar
Part is gentle, and product purity is high, in addition, the casein sodium used has good functional characteristic and very high nutritive value.
To achieve these goals, the present invention uses following technical measures：
The present invention adopts the following technical scheme that the purification process is divided into two steps, and the first step is to obtain pectin and caseinic acid
The sediment of sodium, second step be by the way that sediment is redissolved after, the isoelectric point received to caseinic acid of regulation pH value so that casein
Acid receives precipitation, and pectin is present in supernatant, it is achieved thereby that caseinic acid receives the dissociation with pectin.
A kind of orange peel pectin it is as follows without alcohol extracting method, its step：
A, orange peel pre-processes：The orange peel to rot is rejected, the fritter of a cm is cut into after cleaning up, is added
Boiling boiling 9-11min enzyme deactivations are lived, and are put into 64-66 DEG C of baking oven and are dried after rinsing (3-6 times) repeatedly with 48-52 DEG C of hot water,
Orange peel is crushed with common pulverizer, 50-70 mesh sieves are crossed after crushing, obtain a kind of citrus peel meal, it is stand-by；
B, extract：Weigh the citrus peel meal that step (A) obtains to be placed in beaker, according to citrus peel meal and the ratio 1 of distilled water：
25-1：40(g:ML distilled water) is added, it is 1-2 to adjust pH value with 1M hydrochloric acid (HCl).Beaker is placed in 80-95 DEG C of constant temperature
60-90min is heated in water-bath, and is stirred continuously, obtains a kind of mixture；
C, centrifuge：By the mixture that step (B) obtains in 5000r/min, 18-22min is centrifuged, is obtained containing pectin
Extract solution；
D, the first step is purified：The extract solution and caseinic acid that step (C) is obtained receive the pH value of solution and are adjusted to 3.2-3.7；
Extract solution 10mL is taken, is 1-15 (1 according to the volume ratio of extract solution and casein sodium:2,1:3,1:4,1:5,1:6,1:10,
1:15) add caseinic acid to receive, it was observed that being centrifuged (7000rt/min, 28-32min) after precipitation, obtain pectin and junket egg
The sediment of white acid sodium；
E, second step is purified；(D) sediment obtained is transferred in 30mL distilled water, by adding 1M sodium hydroxides
(NaOH) pH of the system is gradually increased to pH6.6-7, after precipitation dissolves, adds sodium chloride (NaCl) 10-250mM
(10mM, 30mM, 50mM, 100Mm, 200mM, 250mM), adjusting the pH value of solution makes caseinic acid receive precipitation to 4.4-4.8,
28-32min is centrifuged in 9000rt/min, pectin is obtained in supernatant；
F, drying：By the pectin in supernatant obtained by step (E), pre-freeze 18-24h in -10 DEG C to -20 DEG C refrigerator-freezers is placed in,
Then it is -50 DEG C to -70 DEG C in condenser temperature, vacuum is vacuum freeze drying 36-48h under conditions of 0.65-0.85mbar,
Obtain a kind of orange peel pectin.
As a kind of preferred scheme, by citrus peel meal according to 1 in the step (B)：35 add distilled water, and regulation pH value is
1.5, heat 70min in 85 DEG C of water-bath.
As a kind of preferred scheme, in the step (D) according to the volume ratio of extract solution and casein sodium be 1：15 add
Enter caseinic acid to receive.
As a kind of preferred scheme, the concentration of the sodium chloride (NaCl) added in the step (E) is 200mM.
What the present invention proposed a kind of orange peel pectin is mainly based upon two kinds of polymer without alcohol extracting method, the purification process
Between electrostatic interaction, the sediment of pectin and caseinic acid is obtained under pH3.5, regulation pH answers sediment to 6.8
After molten, the isoelectric points 4.6 received to caseinic acid of regulation pH so that caseinic acid receives precipitation, obtains pectin.Pectin in the present invention
Recovery rate can reach 89.5%, and the rate of deposition of casein sodium can reach 98.3%.Ethanol purification pectin is used with conventional method
Compare, do not cause the co-precipitation of other compounds and pectin, obtain the higher pectin of purity, while casein sodium is reversible
Protein, can be reclaimed and recycling at the end of the process, cost-effective.
The present invention compared with prior art, has the following advantages that and effect：
(1) compared with traditional handicraft, the inventive method solves second in traditional handicraft using casein sodium purifying pectin
Alcohol dosage is big, and energy consumption is big during recovery, and production cost is higher, product colour is deep, the problem of peculiar smell be present.
(2) casein sodium used in the inventive method has good functional characteristic and very high nutritive value, both
It is protein fortifier, is emulsifying agent, stabilizer and thickener again, is a kind of green and healthy, energy-efficient extraction pectin
Method.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to specific embodiment to this
The method of invention is described in further detail, but embodiment described herein is not used to limit only to explain the present invention
The fixed present invention.
Embodiment 1：
It is a kind of using caseinic acid receive purifying pectin method, including pretreatment of raw material, extraction, centrifugation, purifying the first step,
Purify second step, freeze-drying；Comprise the following steps that：
1st, material：Sodium hydroxide, sodium chloride, citrus are purchased from Zigui of Hubei, Sigma (Steinheim, Germany) junket
Protein acid sodium (C-8654).
2nd, technological process：
(1) orange peel pre-processes：The orange peel to rot is rejected, the fritter of 1 cm is cut into after cleaning up, is added
Boiling boiling 10min enzyme deactivations are lived, and are put into 65 DEG C of baking ovens and are dried after being rinsed repeatedly with 50 DEG C of hot water, 60 mesh sieves are crossed after crushing, are obtained
A kind of citrus peel meal, it is stand-by；
(2) extract：Weigh the citrus peel meal that 5g steps (1) obtain to be placed in beaker, according to citrus peel meal and distilled water
Than 1：40 (g/mL) add distilled water, are 1.5 with 1M hydrochloric acid (HCl) regulation pH value.Beaker is placed in 85 DEG C of water bath with thermostatic control
70min is heated in pot, and is stirred continuously；
(3) centrifuge：By the mixture that step (2) obtains in 5000r/min, 20min is centrifuged, obtains the extraction containing pectin
Liquid；
(4) first step is purified：The extract solution and caseinic acid that (3) are obtained receive the pH value of solution and are adjusted to 3.5；Take extract solution
10mL, it is 1 according to the mass ratio of extract solution and casein sodium：15 addition caseinic acids are received, it was observed that being centrifuged after precipitation
(7000rt/min, 30min), obtain the sediment of pectin and casein sodium；
(5) second step is purified；The precipitation that (4) obtain is transferred in 30mL distilled water, by adding 1M NaOH by this point
The pH of granular media is gradually increased to pH6.8, and after precipitation dissolves, addition NaCl concentration is 200mM, and adjusting the pH value of solution makes to 4.6
Caseinic acid receives precipitation, centrifuges 30min in 9000rt/min, pectin is obtained in supernatant；
(6) dry：By the pectin in supernatant obtained by step (5), it is placed in -10 or -14 or -18 or -20 DEG C of refrigerator-freezers pre-
18 or 20 or 22 or 24h of jelly, is then -50 DEG C in condenser temperature or -55 or -60 or -64 or -67 or -70 DEG C, vacuum are
Vacuum freeze drying 36 or 40 or 44 or 48h under conditions of 0.65 or 0.7 or 0.75 or 0.85mbar, obtain a kind of orange peel fruit
Glue.
Obtained pectin extraction rate is 89.5%, and the rate of deposition of casein sodium is 98.3%.
Embodiment 2：
It is a kind of using caseinic acid receive purifying pectin method, including pretreatment of raw material, extraction, centrifugation, purifying the first step,
Purify second step, freeze-drying；It is specific as follows：
1st, material：Sodium hydroxide, sodium chloride, citrus are purchased from Zigui of Hubei, Sigma (Steinheim, Germany) junket
Protein acid sodium (C-8654)
2nd, technological process：
(1) orange peel pre-processes：The orange peel to rot is rejected, 1 centimetre of fritter is cut into after cleaning up, adds boiling
Boil 11min enzyme deactivations to live, be put into 64 DEG C of baking ovens and dry after being rinsed repeatedly with 52 DEG C of hot water, 60 mesh sieves are crossed after crushing, obtain one kind
Citrus peel meal, it is stand-by；
(2) extract：Weigh the citrus peel meal that 5g steps (1) obtain to be placed in beaker, according to citrus peel meal and distilled water
Than 1：35 (g/mL) add distilled water, are 1.5 with 1M hydrochloric acid (HCl) regulation pH value.Beaker is placed in 90 DEG C of water bath with thermostatic control
80min is heated in pot, and is stirred continuously；
(3) centrifuge：By the mixture that step (2) obtains in 5000r/min, 18min is centrifuged, obtains the extraction containing pectin
Liquid；
(4) first step is purified：The extract solution and caseinic acid that (3) are obtained receive the pH value of solution and are adjusted to 3.4；Take extract solution
10mL, the mass ratio received according to extract solution and caseinic acid are 1：10 addition caseinic acids are received, it was observed that being centrifuged after precipitation
(7000rt/min, 28min), obtain the sediment of pectin and casein sodium；
(5) second step is purified；The precipitation that (4) obtain is transferred in 30mL distilled water, by adding 1M NaOH by this point
The pH of granular media is gradually increased to pH7.0, and after precipitation dissolves, addition NaCl concentration is 200mM, and adjusting the pH value of solution makes to 4.5
Caseinic acid receives precipitation, centrifuges 28min in 9000rt/min, pectin is obtained in supernatant；
(6) dry：By the pectin in supernatant obtained by step (5), it is placed in -10 or -13 or -17 or -20 DEG C of refrigerator-freezers pre-
Freeze 18 or 21 or 24h, be then -50 DEG C or -54 or -58 or -62 or -68 or -70 DEG C in condenser temperature, vacuum for 0.65 or
Vacuum freeze drying 36 or 41 or 45 or 48h under conditions of 0.69 or 0.74 or 0.85mbar, obtain a kind of orange peel pectin.
Obtained pectin extraction rate is 82.1%, and the rate of deposition of casein sodium is 96.2%.
Embodiment 3：
It is a kind of using caseinic acid receive purifying pectin method, including pretreatment of raw material, extraction, centrifugation, purifying the first step,
Purify second step, freeze-drying；It is specific as follows：
1st, material：Sodium hydroxide, sodium chloride, citrus are purchased from Zigui of Hubei, Sigma (Steinheim, Germany) junket
Protein acid sodium (C-8654).
2nd, technological process：
(1) orange peel pre-processes：The orange peel to rot is rejected, 1 centimetre of fritter is cut into after cleaning up, adds boiling
Boil 9min enzyme deactivations to live, be put into 66 DEG C of baking ovens and dry after being rinsed repeatedly with 48 DEG C of hot water, 60 mesh sieves are crossed after crushing, obtain a kind of mandarin orange
Orange peel powder, it is stand-by；
(2) extract：Weigh the citrus peel meal that 5g steps (1) obtain to be placed in beaker, according to solid-liquid ratio 1：40 add distillation
Water, it is 2 with 1M hydrochloric acid (HCl) regulation pH value.Beaker is placed in 90 DEG C of thermostat water bath and heats 90min, and is constantly stirred
Mix；
(3) centrifuge：By the mixture that step (2) obtains in 5000r/min, 22min is centrifuged, obtains the extraction containing pectin
Liquid；
(4) first step is purified：The extract solution and caseinic acid that (3) are obtained receive the pH value of solution and are adjusted to 3.6；Take extract solution
10mL, it is 1 according to the mass ratio of extract solution and albumen：15 addition caseinic acids are received, it was observed that being centrifuged after precipitation
(7000rt/min, 32min), obtain the sediment of pectin and casein sodium；
(5) second step is purified；The precipitation that (4) obtain is transferred in 30mL distilled water, by adding 1M NaOH by this point
The pH of granular media is gradually increased to pH6.9, and after precipitation dissolves, addition NaCl concentration is 200mM, and adjusting the pH value of solution makes to 4.7
Caseinic acid receives precipitation, centrifuges 32min in 9000rt/min, pectin is obtained in supernatant；
(6) dry：By the pectin in supernatant obtained by step (5), -10 DEG C or -13 or -16 or -18 or -20 DEG C of ice are placed in
Pre-freeze 18 or 22 or 24h in cabinet, it is then -50 DEG C or -57 or -64 or -70 DEG C in condenser temperature, vacuum is 0.65 or 0.68
Or vacuum freeze drying 36 or 41 or 48h under conditions of 072 or 0.8 or 0.85mbar, obtain a kind of orange peel pectin.
Obtained pectin extraction rate is 81.3%, and the rate of deposition of casein sodium is 94.8%.
Experimental example 1：Nacl adds the determination of concentration
NaCl has a great impact to the electrostatic interaction between pectin and casein sodium and its compatibility, and salt is in fruit
Played an important role in the separation of glue and caseinate, when NaCl is added in mixture, Na+With casein sodium just
Charge bonded site competition combination polysaccharide chain.Meanwhile Cl-Also with the negative electrical charge binding site competition binding caseinic acid of pectin
Sodium, receives the chance combined with pectin it reduce caseinic acid.
1st, NaCl adds concentration experiment result
Table 1：Nacl adds influence of the concentration to pectin extraction rate
Pectin (PE) recovery rate=a/ (a+b) * 100%
Casein sodium (SC) recovery rate=c/ (c+d) * 100%
2nd, interpretation of result
Table 1 is given under the NaCl of various concentrations, in supernatant and precipitation the content received of pectin and caseinic acid and
Pectin extraction rate and caseinic acid receive rate of deposition.When no addition salt, only 38.4% albumen is deposited, and in supernatant
Pectin content be 49.6%, the pectin of more than half is separated in not received from caseinic acid；With NaCl addition, on
Pectin content in clear liquid is continuously increased, and the rate of deposition that caseinic acid is received also constantly increases.When salinity increases to 250mM,
The rate of deposition of albumen has reached 96.6%.And the percentage composition of the pectin in supernatant also brings up to 90.2% from 49.6%.
Experimental example 2：Pectin/caseinic acid receives the determination of mass ratio
The stoichiometry of biopolymer is the significant variable that compound is formed, when with polysaccharide compound action occurs for albumen,
Tend to be formed the compound of electroneutral；Low proteoglycan mass ratio means that proteic charge is not enough to neutralizing polysaccharide carrying just
Electric charge, it is therefore desirable to add more casein sodiums.The concentration for adding NaCl is 200mM, by comparing the recovery rate of pectin,
Obtain optimal pectin/caseinic acid and receive mass ratio.
Table 2：Pectin/caseinic acid receives influence of the mass ratio to pectin extraction rate
Table 2 shows that different pectin/caseinic acids receive the recovery rate of pectin under the conditions of mass ratio.When pectin/caseinic acid
Mass ratio is received from 1:15 are gradually reduced to 1:When 2, the recovery rate of pectin is down to 44.6% by 89.5%.Illustrate with caseinic acid
Receive the increase of addition, more pectin can be combined to improve the recovery rate of pectin.
Note：The recovery rate of pectin in the present invention is calculated with the content of galacturonic acid.
Claims (4)
1. a kind of orange peel pectin is without alcohol extracting method, its step：
A, orange peel pre-processes：The orange peel to rot is rejected, one centimetre of fritter is cut into after cleaning up, adds boiling to boil
9-11min enzyme deactivations are lived, and are put into 64-66 DEG C of baking oven and are dried after being rinsed repeatedly with 48-52 DEG C of hot water, orange peel is carried out into powder
It is broken, 50-70 mesh sieves are crossed after crushing, obtain a kind of citrus peel meal, it is stand-by；
B, extract：Weigh step（A）Obtained citrus peel meal is placed in beaker, according to citrus peel meal and the ratio 1 of distilled water：25-
1：40g:ML adds distilled water, is 1-2 with 1M salt acid for adjusting pH value, beaker is placed in 80-95 DEG C of thermostat water bath and added
Hot 60-90min, is stirred continuously, and obtains a kind of mixture；
C, centrifuge：By step（B）Obtained mixture centrifuges 18-22min, obtains the extraction containing pectin in 5000r/min
Liquid；
D, the first step is purified：By step（C）Obtained extract solution and caseinic acid receives the pH value of solution and is adjusted to 3.2-3.7；Take and carry
Liquid 10mL is taken, is that 1-15 addition caseinic acids are received according to the volume ratio of extract solution and casein sodium, it was observed that being carried out after precipitation
7000rt/min, 28-32min are centrifuged, obtains the sediment of pectin and casein sodium；
E, second step is purified；By step（D）The sediment of acquisition is transferred in 30mL distilled water, by adding 1M sodium hydroxides
The pH of dispersion is gradually increased to pH6.6-7, after precipitation dissolves, sodium chloride 10-250mM is added, adjusts the pH value of solution
Caseinic acid is received precipitation to 4.4-4.8, centrifuge 28-32min in 9000rt/min, pectin is obtained in supernatant；
F, drying：By step（E）Pectin in gained supernatant, pre-freeze 18-24h in -10 DEG C to -20 DEG C refrigerator-freezers is placed in, then
It it is -50 DEG C to -70 DEG C in condenser temperature, vacuum is vacuum freeze drying 36-48h under conditions of 0.65-0.85mbar, is obtained
A kind of orange peel pectin.
2. a kind of orange peel pectin according to claim 1 without alcohol extracting method, it is characterised in that：The step（B）In
By citrus peel meal according to 1：35 add distilled water, and regulation pH value is 1.5, and 70min is heated in 85 DEG C of water-bath.
3. a kind of orange peel pectin according to claim 1 without alcohol extracting method, it is characterised in that：The step（D）In
It is 1 according to the volume ratio of extract solution and casein sodium：15 addition caseinic acids are received.
4. a kind of orange peel pectin according to claim 1 without alcohol extracting method, it is characterised in that：The step（E）In
The concentration of the sodium chloride of addition is 200mM.
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| CN108641012A (en) * | 2018-03-12 | 2018-10-12 | 湖北大学知行学院 | A method of extracting pectin by raw material of wild elephant skin mandarin orange |
| CN115584133A (en) * | 2021-07-06 | 2023-01-10 | 宋悠洋 | Thermoplastic composition based on degradable biopolymer and preparation method and application thereof |
| CN115584133B (en) * | 2021-07-06 | 2023-12-15 | 深圳市朴飞生物科技有限公司 | Thermoplastic composition based on degradable biopolymer, preparation method and application thereof |
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Application publication date: 20180202 |