CN110272507A - A method of extracting high viscosity pectin from leaf category biomass - Google Patents
A method of extracting high viscosity pectin from leaf category biomass Download PDFInfo
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- CN110272507A CN110272507A CN201910679925.6A CN201910679925A CN110272507A CN 110272507 A CN110272507 A CN 110272507A CN 201910679925 A CN201910679925 A CN 201910679925A CN 110272507 A CN110272507 A CN 110272507A
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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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Abstract
The method that the present invention provides a kind of to extract high viscosity pectin from leaf category biomass, specific method includes following characteristics step: by pretreatment of raw material, the lye for regulating pH being added in Ye Fenzhong, a kind of mixture is obtained after reaction；Mixture is separated, the extracting solution containing pectin is obtained；Pectin precipitating reagent is added in extracting solution, is separated after mixing, obtains pectin and precipitates and redissolve the precipitating with water, or extracting solution is subjected to ultra-filtration and separation；Solution after redissolution is centrifuged, the pectin in supernatant is dried, obtains a kind of pectin product in aqueous solvent with high viscosity degree.This method extracts the applied widely of high viscosity pectin, can be used for the high viscosity pectin extraction of most of leaf category biomass, and the recovery rate of pectin is high, and the pectin viscosity of acquisition is high.Pectin after extraction can be used as gelling agent, crosslinking agent, stabilizer and thickener etc. applied in the relevant industries products such as food.
Description
Technical field
The invention belongs to technical field of polysaccharide extraction, are more particularly to a kind of extracting method of leaf category class high viscosity pectin.
Background technique
Pectin is that one kind is widely present in the primary wall of plant cell wall and the heteroglycan of cell middle sheet, in food work
It is widely used in industry.Pectin is usually as food additives, and such as thickener, stabilizer and gelling agent, can also be used as crosslinking agent makes
With.The production of business pectin at present mainly using citrus and apple as raw material, also have it is a small number of with lemon peel, banana skin, pineapple peel and
Sunflower plate etc. is that raw material is produced, still, more rare as the report of raw material production pectin using leaf biolobic material.Therefore add
By force to the development and application of leaf class pectin, the comprehensive utilization ratio of living resources can be improved, but the extractive technique of leaf class pectin still has
Many deficiencies limit its application in food and medicine field.
The extracting method of pectin mainly has classical acid formulation, salting out method, enzyme process, microbial method, microwave assisting method, surpasses at present
Sound wave assisted extraction method, but all there is its shortcoming in these methods.By taking salting out method as an example, using free carboxy in pectin with
Salt ion opposite charge in salting liquid generates precipitating by neutralization, although precipitated metal can remove free neutral sugar,
Also partially protein can be removed, but obtained pectin product ash content is high.Although Enzymatic Extraction pectin can keep the day of pectin
Right configuration, but enzyme is expensive, and the yield obtained is lower, is not suitable for a large amount of industrialized productions.
In order to make pectin application in the food industry, " Food Chemistry product code " regulation, pectin is in moisture and ash-free condition
There should be the galacturonic acid content not less than 65% down.Therefore it one kind is provided can produce galacturonic acid content and be greater than
The method of the high viscosity pectin of 65wt% is particularly significant applied to food service industry.
Summary of the invention
Present invention aims at: provide it is a kind of be readily produced, safe and simple high viscosity leaf class pectin extraction method so that
The pectin being extracted keeps highly viscous state.
The purpose of the present invention includes: the galacturonic with minimum 65wt% for providing and being obtained by claimed method
The food-grade pectin of sour (GA) is used to stablize beverage (such as acidified milk or diluted fruit juice), the dairy products of construction acidification or as cream
Dietary fiber, gelling agent, stabilizer in sweet food processed and/or as albumen complexing agent.
To achieve the above object, technical solution provided by the invention is as follows: one kind extracting high viscosity from leaf category biomass
The method of pectin, the step include:
(a): the pretreatment of leaf category biomass material: rejecting undesirable leaf class, crush cured leaf after cleaning up；
(b): extracting: alkaline solution being added in the leaf powder that step (a) obtains, obtains a kind of mixture after heating reaction；
(c): separation: the isolated extracting solution containing pectin of the mixture that step (b) is obtained；
(d): purifying: pectin precipitating reagent is added in the extracting solution that step (c) is obtained, and separates after mixing, and acquisition pectin, which precipitates, to be used in combination
Water redissolves precipitating；
(e): dry: the pectin in supernatant obtained by step (d) being dried, a kind of leaf class high viscosity pectin finished product is obtained.
The mass volume ratio of leaf powder and aqueous slkali is mixed according to g:mL for 1:1-120 in step (b).
The alkaline solution being added in the step (b) is the sodium hydroxide or potassium hydroxide solution of pH range 7-12.
Step (b) reaction temperature is 15 DEG C -100 DEG C, heating time 10min-24h.
Adoptable separation method includes one of centrifugation, ultrafiltration, absorption or various ways in step (c).
Ultrafiltration membrane aperture is less than 150kDa.
Precipitating reagent in step (d) includes one of acid solution or organic solvent；The organic solvent is ethyl alcohol.
The drying proposal method of the step (e) includes oven drying, freeze-drying or spray drying process.
As a preferred embodiment, by the matter of the leaves powder and aqueous slkali such as green tea powder, raspberry leaf, lotus leaf in the step (a)
Volume ratio is measured according to 1:30(g:mL) (the wherein NaOH solution that lye is pH value 9.0) is mixed, in the case where temperature is 15-100 DEG C, add
Thermal response 15min-24h.
As a preferred embodiment, in the step (b) by green tea powder respectively with pH be 9.0 sodium hydroxide solution, go
Hydrochloric acid solution that ionized water, pH are 2, the cellulose-containing carbohydrate composite enzyme solution of packet are 1:30(g by mass volume ratio:
ML it) mixes, in the case where temperature is 15-100 DEG C, heating reaction 15min-24h.
As a preferred embodiment, in the step (b) by the mass volume ratio of leaf powder and aqueous slkali according to 1:30(g:
ML) mixing (the wherein NaOH solution that lye is pH value 7-12), in the case where temperature is 15-100 DEG C, heating reaction 15min-24h.
As a preferred embodiment, in the step (b) by the mass volume ratio of leaf powder and aqueous slkali according to 1:30(g:
ML) mixing (the wherein NaOH solution that lye is pH value 7-12), in the case where temperature is 50-70 DEG C, heating reaction 15min-24h.
As a preferred embodiment, in the step (b) by the mass volume ratio of leaf powder and aqueous slkali according to 1:30(g:
ML) mixing (the wherein NaOH solution that lye is pH value 7-12), in the case where temperature is 50-70 DEG C, heating reaction 15min-6h.
As a preferred embodiment, the separation side for the use that (c) is used in the step is method centrifugation, be can get higher viscous
The pectin product of property.
As a preferred embodiment, for ethyl alcohol, the pectin that can get high viscosity produces the precipitating reagent used in the step (d)
Product.
As a preferred embodiment, the drying means used in the step (e) is vacuum freeze-drying method, can get height
The pectin product of viscosity.
Remarkable advantage of the invention is:
The invention proposes a kind of extracting methods of high viscosity leaf class pectin, compared with prior art, production technology of the invention
Easy to operate, production cost is low, and product quality is high, and the recovery rate of pectin is high, and viscosity is good.
Detailed description of the invention
Fig. 1 is influence of the different pH extraction to pectin viscosity.
Fig. 2 is influence of the different disposal method to pectin viscosity.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in more detail, but is not limited to protection scope of the present invention.
A method of extract high viscosity pectin from leaf category biolobic material, pretreatment, extracting and developing including raw material,
Purifying, drying；Specific step is as follows:
Material: green tea, raspberry leaf, lotus leaf, sodium hydroxide, hydrochloric acid solution, carbohydrate complex enzyme (Viscozyme® L)
Solution, deionized water, dehydrated alcohol.
Embodiment 1
A: the pretreatment of leaf class: three kinds of green tea, raspberry leaf, lotus leaf leaves are respectively put into pulverizer and are crushed, 60 mesh are smashed it through
Sieve, obtain three kinds of sieving leaf powder, for use；
B: extracting: weighing the leaf powder in 100g step (a) respectively, mixed for 1:30 (g:mL) according to the ratio of leaf powder and lye
It closes, the lye is the NaOH solution of pH9.0；It is respectively placed in heating reaction 3h in 90 DEG C of vortex magnetic stirring apparatus, point
Not Huo get three kinds of leaf powder alkali soluble liquid mixture；
C: separation: the mixture for respectively obtaining step (b) is centrifuged 15min, obtains the extraction containing pectin in 6000r/min
Liquid；
D: purifying: dehydrated alcohol precipitating is added in the extracting solution for respectively obtaining step (c)；According to the body of extracting solution and dehydrated alcohol
Product is observed after precipitating at 6000r/min than being that 1:1 is mixed, is centrifuged 20min, obtain pectin precipitating and redissolve precipitating with water；
E: dry: respectively by the pectin in supernatant obtained by step (d), pre-freeze to be placed in -80 DEG C of refrigerator-freezers for 24 hours, then in cold-trap
Temperature is -60 DEG C, and vacuum degree is vacuum freeze drying 72h under conditions of 0.9mbar, obtains the leaf class high viscosity fruit of three kinds of leaf powder
Glue, grinds save.
The leaf class high viscosity pectin extraction rate of three kinds of leaf powder is measured respectively, and obtained pectin extraction rate is shown in Table 1.
The recovery rate of the different leaf class pectin of table 1
Embodiment 2:
A: the pretreatment of leaf class: green tea being put into pulverizer and is crushed, the sieve of 60 mesh is smashed it through, leaf powder after being sieved,
For use；
B: it extracts: weighing the leaf powder in 100g step (a), be by mass volume ratio with the sodium hydroxide solution that pH is 7-12 respectively
It 1:30(g:mL) is mixed with leaf powder, places it in heating reaction 3h in 90 DEG C of vortex magnetic stirring apparatus, obtain a kind of mixture；
C: separation: the mixture that step (b) is obtained is centrifuged 15min, obtains the extracting solution containing pectin in 6000r/min；
D: purifying: dehydrated alcohol precipitating is added in the extracting solution that step (c) is obtained；According to the volume ratio of extracting solution and dehydrated alcohol
It for 1:1 mixing, observes after precipitating at 6000r/min, is centrifuged 20min, obtain pectin precipitating and redissolve precipitating with water；
E: dry: by the pectin in supernatant obtained by step (d), pre-freeze to be placed in -80 DEG C of refrigerator-freezers for 24 hours, then in condenser temperature
It is -60 DEG C, vacuum degree is vacuum freeze drying 72h under conditions of 0.9mbar, obtains a kind of leaf class high viscosity pectin, grinds
It saves.
Obtained different pH processing is shown in Fig. 1 to pectin viscosity influence.
Comparative example 1:
A: the pretreatment of leaf class: green tea is put into pulverizer and crushes, and smashes it through the sieve of 60 mesh, leaf powder after being sieved, to
With；
B: extract: weigh the leaf powder in 100g step (a), respectively with pH be 9.0 sodium hydroxide solution, deionized water, pH 2
Hydrochloric acid solution, carbohydrate complex enzyme (Viscozyme® L) solution is 1:30(g:mL by mass volume ratio) it is mixed with leaf powder
It closes.Heating reaction 3h in 90 DEG C of vortex magnetic stirring apparatus is placed it in, a kind of mixture is obtained；
C: separation: the mixture that step (b) is obtained is centrifuged 15min, obtains the extracting solution containing pectin in 6000r/min；
D: purifying: dehydrated alcohol precipitating is added in the extracting solution that step (c) is obtained；According to the volume ratio of extracting solution and dehydrated alcohol
It for 1:1 mixing, observes after precipitating at 6000r/min, is centrifuged 20min, obtain pectin precipitating and redissolve precipitating with water；
E: dry: by the pectin in supernatant obtained by step (d), pre-freeze to be placed in -80 DEG C of refrigerator-freezers for 24 hours, then in condenser temperature
It is -60 DEG C, vacuum degree is vacuum freeze drying 72h under conditions of 0.9mbar, obtains a kind of leaf class high viscosity pectin, grinds
It saves.
Obtained pectin extraction rate is shown in Table 2.
Influence of 2 Different Extraction Method of table to pectin extraction rate
Obtained Different Extraction Method is shown in Fig. 2 to pectin viscosity influence.Finally, need to indicate that listed above is several of the invention
Specific embodiment, but present invention is not limited to the above embodiments, it can also be there are many deforming, according to the concept of the present invention to above-mentioned reality
Example mode carries out all deformations caused by various equivalent changes and modification, is considered as within protection scope of the present invention.
Claims (8)
1. a kind of method for extracting high viscosity pectin from leaf category biomass, it is characterised in that: the step includes:
(a): the pretreatment of leaf category biomass material: rejecting undesirable leaf class, crush cured leaf after cleaning up；
(b): extracting: alkaline solution being added in the leaf powder that step (a) obtains, obtains a kind of mixture after heating reaction；
(c): separation: the isolated extracting solution containing pectin of the mixture that step (b) is obtained；
(d): purifying: pectin precipitating reagent is added in the extracting solution that step (c) is obtained, and separates after mixing, and acquisition pectin, which precipitates, to be used in combination
Water redissolves precipitating；
(e): dry: the pectin in supernatant obtained by step (d) being dried, a kind of leaf class high viscosity pectin finished product is obtained.
2. a kind of method for extracting high viscosity pectin from leaf category biomass according to claim 1, it is characterised in that: step
Suddenly the mass volume ratio of leaf powder and aqueous slkali is mixed according to g:mL for 1:1-120 in (b).
3. a kind of method for extracting high viscosity pectin from leaf category biomass according to claim 1, it is characterised in that: institute
State sodium hydroxide or potassium hydroxide solution that the alkaline solution being added in step (b) is pH range 7-12.
4. a kind of method for extracting high viscosity pectin from leaf category biomass according to claim 1, it is characterised in that: institute
Stating step (b) reaction temperature is 15 DEG C -100 DEG C, heating time 10min-24h.
5. a kind of method for extracting high viscosity pectin from leaf category biomass according to claim 1, it is characterised in that: step
Suddenly adoptable separation method includes one of centrifugation, ultrafiltration, absorption or various ways in (c).
6. a kind of method for extracting high viscosity pectin from leaf category biomass according to claim 6, it is characterised in that: super
Filter sizes are less than 150kDa.
7. a kind of method for extracting high viscosity pectin from leaf category biomass according to claim 1, it is characterised in that: step
Suddenly the precipitating reagent in (d) includes one of acid solution or organic solvent；The organic solvent is ethyl alcohol.
8. a kind of method for extracting high viscosity pectin from leaf category biomass according to claim 1, it is characterised in that: institute
The drying proposal method for stating step (e) includes oven drying, freeze-drying or spray drying process.
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Citations (7)
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|---|---|---|---|---|
| CN85106947A (en) * | 1985-08-30 | 1986-07-02 | 上海市食品工业研究所 | From sunflower plate and bar, extract the method for edible low-ester pectin |
| UA62090A (en) * | 2002-10-14 | 2003-12-15 | A method for producing pectin from sugar-beet press (variants) | |
| US20070031572A1 (en) * | 2003-07-07 | 2007-02-08 | Kmc Kartoffelmelcentralen Amba | Method for preparing fibre-containing pectin and products and uses thereof |
| CN102372791A (en) * | 2010-08-10 | 2012-03-14 | 刘华敏 | Preparation process of pectin with maize straw |
| EP2718330A1 (en) * | 2011-06-06 | 2014-04-16 | CP Kelco ApS | Process for extraction of pectin |
| CN104371039A (en) * | 2014-10-16 | 2015-02-25 | 南京师范大学 | Corn cob soluble dietary fiber-pectin and preparation method thereof |
| CN109384860A (en) * | 2018-10-24 | 2019-02-26 | 福州大学 | A method of extracting natural pectin from leaf category biomass |
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2019
- 2019-07-26 CN CN201910679925.6A patent/CN110272507A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85106947A (en) * | 1985-08-30 | 1986-07-02 | 上海市食品工业研究所 | From sunflower plate and bar, extract the method for edible low-ester pectin |
| UA62090A (en) * | 2002-10-14 | 2003-12-15 | A method for producing pectin from sugar-beet press (variants) | |
| US20070031572A1 (en) * | 2003-07-07 | 2007-02-08 | Kmc Kartoffelmelcentralen Amba | Method for preparing fibre-containing pectin and products and uses thereof |
| CN102372791A (en) * | 2010-08-10 | 2012-03-14 | 刘华敏 | Preparation process of pectin with maize straw |
| EP2718330A1 (en) * | 2011-06-06 | 2014-04-16 | CP Kelco ApS | Process for extraction of pectin |
| CN104371039A (en) * | 2014-10-16 | 2015-02-25 | 南京师范大学 | Corn cob soluble dietary fiber-pectin and preparation method thereof |
| CN109384860A (en) * | 2018-10-24 | 2019-02-26 | 福州大学 | A method of extracting natural pectin from leaf category biomass |
Non-Patent Citations (3)
| Title |
|---|
| CHEN ZHANG, ET AL.: "Improving viscosity and gelling properties of leaf pectin by comparing five pectin extraction methods using green tea leaf as a model material", 《FOOD HYDROCOLLOIDS》 * |
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