CN103483465A - Environment-friendly preparation method of beet pectin - Google Patents
Environment-friendly preparation method of beet pectin Download PDFInfo
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- CN103483465A CN103483465A CN201310381569.2A CN201310381569A CN103483465A CN 103483465 A CN103483465 A CN 103483465A CN 201310381569 A CN201310381569 A CN 201310381569A CN 103483465 A CN103483465 A CN 103483465A
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- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
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Abstract
The invention discloses an environment-friendly preparation method of beet pectin. According to the method, waste beet pulp of a beet sugar factory is taken as a raw material, and the method comprises the steps of firstly washing the beet pulp with distilled water, filtering, and then drying; preparing the beet pulp and the distilled water into a material solution with the liquid-solid ratio of (100:1)-(10:1), and placing under the conditions of an electrostatic field and an ultrasonic field to perform pretreatment, wherein the intensity of an electric field is 8-32kV and the ultrasonic intensity is 0.35-0.88W/cm<2>; extracting the pectin under subcritical water conditions, wherein the temperature is 100-300 DEG C, the pressure is 2MPa-20MPa, the pressure conversion period is 1-3 times, and the total extraction time is 5min-90min; filtering, concentrating, then precipitating with isopropanol, centrifuging, then further washing with isopropanol, and freeze-drying to obtain the beet pectin. The method disclosed by the invention has the characteristics of environmental friendliness, no pollution, short time of process flow, high product yield, stable nature and high edible safety.
Description
Technical field
The present invention relates to a kind of beet pectin, particularly relate to a kind of environment-friendly preparation method thereof of beet pectin, belong to the green manufacture field of food.
Background technology
Pectin is a kind of natural high moleculer eompound mainly be comprised of galacturonic acid, has good gelation and emulsifying property, has been widely used in food, medicine, daily use chemicals and textile industry.According to the content of gamma value in pectin and neutral sugar, different purposes can be arranged, generally can be divided into high ester rapid hardening pectin, high ester slow pectin, low-ester pectin, pharmacy pectin and extraordinary low-ester pectin.The pectin of industrialization at present is mainly to extract and obtain from apple residue and orange peel class pericarp, contain abundant food fibre in beet dry pulp, wherein water-soluble dietary fibre---the content of pectin is higher, average content reaches 28%, and the beet pectin emulsifying property is better than apple pectin and citrus pectin, so the development potentiality of beet pectin is very large.
The extraction of pectin mainly adopts acid extraction method traditionally, example hydrochloric acid, sulfuric acid, nitric acid, organic acid etc.This kind of method, because cell walls is tough and tensile survivable, the leaching process used time is longer, and extraction yield is low; Use the reagent such as a large amount of soda acids in leaching process, higher to equipment requirements, and easily cause environmental pollution and the wasting of resources.
Summary of the invention
The object of the invention is to extract for current acid system the drawback of pectin, the beet pectin production method of the high and green non-pollution of a kind of extraction yield is provided.
The present invention utilizes ultrasonic and electrostatic field technology synergy pre-treatment beet pulp, and, not containing the subcritical water extraction beet pectin of the chemical reagent such as soda acid, is a kind of environment-friendly preparation method thereof.Green Chemistry has become the forward position of current chemical science development, is the important directions of 21 century chemical developer.The present invention, from the angle of Green Chemistry, be take the waste material from sugar refinery beet pulp as raw material, adopts electrostatic field, ultrasonic, three kinds of green technologies of subcritical water, has effectively avoided the use of soda acid to cause the problems such as serious environment, health, safety and equipment corrosion.By research pre-treatment and extraction conditions, the novel process that a green prepares beet pectin has been proposed, be characterized in that the product yield is high, the used time is short, green non-pollution, edible safety be high.
Purpose of the present invention is achieved through the following technical solutions:
A kind of environment-friendly preparation method thereof of beet pectin, contain following steps:
(1), by the beet pulp distilled water wash, filter post-drying;
(2) step (1) gained beet pulp and distilled water are made into to the feed liquid that liquid-solid ratio is 100:1～10:1, are placed under electrostatic field and ultrasonic field condition and carry out pre-treatment, strength of electric field is 8～32kV, and frequency is 5～70kHz, and ultrasound intensity is 0.35～0.88W/cm
2, frequency is 20～50kHz, and the treatment time is 5～30min, and temperature is 25～50 ℃;
(3) under sub-critical water extraction, step (2) the gained feed liquid of take is extracted pectin as raw material, and temperature is 100～300 ℃, and pressure is 2MPa～20MPa, and pressure transformation period is 1～3 time, and extraction total time is 5min～90min; Described pressure refers to first feed liquid is raised to 2MPa～20MPa setting pressure from standard atmospheric pressure transformation period, and constant voltage drops to standard atmospheric pressure after extracting again, and the time that constant voltage is extracted is for extracting total time divided by pressure number transformation period; Described extract refer to total time all pressure in transformation period under setting pressure and design temperature the summation of constant voltage extraction time; Do not comprise the heating-up time, pressure rising time and step-down time;
(4) step (3) gained feed liquid filtered, use isopropanol precipitating after concentrated, use washed with isopropyl alcohol after centrifugal again, lyophilize, obtain beet pectin.
For further realizing the object of the invention, preferably, 2, described washing is the distilled water wash-out 8-15min with 40 ℃-45 ℃ by beet pulp, to remove the small molecules such as residual sucrose, glucose, inorganic salt in beet pulp.Described oven dry is that the beet pulp after washing is filtered to post-drying with nylon cloth; Biodiversity content after beet pulp is dried is not more than 6%.Described feed liquid is filtered and is adopted nylon cloth to filter.Described concentrating is to 5% of original volume at 50～70 ℃ of lower vacuum concentration.The volume of described Virahol is 1～4 times of feed liquid.Described centrifugal rotating speed is 8000-10000rpm.Described lyophilize is at-60 ℃～-55 ℃, dry 20～24h under 0.1～0.2MPa vacuum tightness, and in dried pectin, the massfraction of contained level is not more than 5%.
In the present invention, subcritical water refers at certain pressure but under emergent pressure 22.1MPa condition lower than water, by water by heat to 100 ℃ with upper critical temperature the high temperature below 374.2 ℃, water body still remains on liquid state.
The present invention compared with prior art, has following advantage and beneficial effect:
(1) with classical acid extraction process technology, compare, the whole leaching process of the present invention adopts the method for green non-pollution, environmental pollution and the wasting of resources of having avoided soda acid to cause.
(2) with conventional art, compare, the present invention adopts subcritical water to extract beet pectin, and its preparation time is no more than 60min, than the preparation time of 2～8 hours of conventional high-tension low heat method, has shortened 2～8 times.
(3) with conventional art, compare, the present invention adopts subcritical water to extract beet pectin, extracts main procedure and adopts the subcritical water that does not contain the chemical reagent such as soda acid to be extracted, the pectin molecule degraded that can effectively avoid acid to cause, make product property more stable, edibility is high.
Embodiment
For understanding better the present invention; below in conjunction with embodiment, the present invention is described further; the contriver is to passing through further investigation and test; many successful embodiment have been arranged; below enumerate four specific embodiments, but the scope of protection of present invention is not limited to the scope of embodiment statement.
Embodiment 1:
The first step to remove the small molecules such as sucrose residual in beet pulp, glucose, inorganic salt, after filtering with nylon cloth is dried beet pulp wash-out 10min in the distilled water of 40 ℃ under 40 ℃, and in the control beet pulp, biodiversity content is lower than 6%;
Second step is made into by the beet pulp of oven dry and distilled water feed liquid that liquid-solid ratio is 100:1 and is placed under electrostatic field and ultrasonic field condition and carries out pre-treatment.Strength of electric field is 8kV, and frequency is 5kHz, ultrasound intensity 0.35W/cm
2, frequency is 20kHz, and the treatment time is 5min, and temperature is 25 ℃;
The 3rd step is extracted pectin by pretreated feed liquid being placed under subcritical water (100 ℃, the distilled water under the 2MPa condition) condition.First the speed with 4 ℃/min is warmed up to design temperature (100 ℃), and then boost fast (in 1min), to setting pressure (2MPa), is incubated (100 ℃) constant voltages (2MPa) 5min, and (in 5s) drops to standard atmospheric pressure by pressure fast, takes out feed liquid;
The 4th step will be concentrated into 5% of original volume after the 3rd step gained extracting liquid filtering under 50 ℃, the long-pending centrifugal rear washed with isopropyl alcohol of using of isopropanol precipitating, 8000rpm with monoploid, at-60 ℃, 0.1MPa dry 24h under vacuum tightness, in dried pectin, the massfraction of contained level is not more than 5%, obtains beet pectin.The yield that obtains beet pectin through weighting method is 15.42%.
The present embodiment beet pectin preparation time only comprises pretreatment time and extracts total time for 10min() 10min, be significantly less than 2～8 hours of classical acid extraction method; The method gained pectin is not owing to being subject to sour degraded, and molecular weight is determined as 120kDa through GPC, larger than the beet pectin molecular weight (≤100kDa) extracted under acidic conditions; In extracting solution, except beet pectin, filter residue is mainly the biodegradable components such as Mierocrystalline cellulose and hemicellulose, and filtrate is mainly water-soluble carbohydrate, not containing the poisonous chemical reagent such as soda acid, environmentally safe.
Embodiment 2:
The first step to remove the small molecules such as sucrose residual in beet pulp, glucose, inorganic salt, after filtering with nylon cloth is dried beet pulp wash-out 10min in the distilled water of 40 ℃ under 40 ℃, and in the control beet pulp, biodiversity content is lower than 6%;
Second step is made into by the beet pulp of oven dry and distilled water feed liquid that liquid-solid ratio is 10:1 and is placed under electrostatic field and ultrasonic field condition and carries out pre-treatment.Strength of electric field is 32kV, and frequency is 70kHz,, ultrasound intensity 0.88W/cm
2, frequency is 50kHz, and the treatment time is 30min, and temperature is 50 ℃;
The 3rd step is extracted pectin by pretreated feed liquid under subcritical water (300 ℃, the distilled water under 20MPa) condition.This step first is warmed up to design temperature (300 ℃) with the speed of 4 ℃/min, and three pressure take out feed liquid after transformation period; Extract total time 90min three transformation periods.Wherein feed liquid is boosted to (1min in) to setting pressure (20MPa) fast from standard atmospheric pressure, under insulation (300 ℃) constant voltages (20MPa) condition, extract 30min, (5s is interior) drops to standard atmospheric pressure by pressure fast, is a pressure transformation period; Extract refer to total time all pressure in transformation period under setting pressure and design temperature the summation of constant voltage extraction time; Do not comprise the heating-up time, pressure rising time and step-down time;
The 4th step will be concentrated into 5% of original volume after the 3rd step gained extracting liquid filtering under 70 ℃, the long-pending centrifugal rear washed with isopropyl alcohol of using of isopropanol precipitating, 10000rpm with tetraploid, at-60 ℃, 0.1MPa dry 24h under vacuum tightness, in dried pectin, the massfraction of contained level is not more than 5%, obtains beet pectin.The yield that obtains beet pectin through weighting method is 15.38%.
The present embodiment beet pectin preparation time is only 60min, and this time comprises pretreatment time and extracts total time, is significantly less than 2～8 hours of classical acid extraction method; The method gained pectin is not owing to being subject to sour degraded, and molecular weight is determined as 112kDa through GPC, larger than the beet pectin molecular weight (≤100kDa) extracted under acidic conditions; In extracting solution, except beet pectin, filter residue is mainly the biodegradable components such as Mierocrystalline cellulose and hemicellulose, and filtrate is mainly water-soluble carbohydrate, not containing the poisonous chemical reagent such as soda acid, environmentally safe.
Embodiment 3:
The first step to remove the small molecules such as sucrose residual in beet pulp, glucose, inorganic salt, after filtering with nylon cloth is dried beet pulp wash-out 10min in the distilled water of 40 ℃ under 40 ℃, and in the control beet pulp, biodiversity content is lower than 6%;
Second step is made into by the beet pulp of oven dry and distilled water feed liquid that liquid-solid ratio is 50:1 and is placed under electrostatic field and ultrasonic field condition and carries out pre-treatment.Strength of electric field is 12kV, and frequency is 60kHz,, ultrasound intensity 0.55W/cm
2, frequency is 40kHz, and the treatment time is 10min, and temperature is 30 ℃;
The 3rd step is extracted pectin by pretreated feed liquid under subcritical water (150 ℃, the distilled water under 15MPa) condition.First the speed with 4 ℃/min is warmed up to design temperature (150 ℃), two pressure (boost (in 1min) to setting pressure (15MPa) by feed liquid from standard atmospheric pressure transformation period fast, extract 15min under insulation (150 ℃) constant voltages (15MPa) condition, (5s in) drops to standard atmospheric pressure by pressure fast, completes a pressure transformation period) after take out feed liquid.Extract total time 30min two transformation periods;
The 4th step will be concentrated into 5% of original volume after the 3rd step gained extracting liquid filtering under 60 ℃, the long-pending centrifugal rear washed with isopropyl alcohol of using of isopropanol precipitating, 9000rpm with triploid, at-60 ℃, 0.1MPa dry 24h under vacuum tightness, in dried pectin, the massfraction of contained level is not more than 5%, obtains beet pectin.The yield that obtains beet pectin through weighting method is 16.42%.
The present embodiment beet pectin preparation time is only 40min, and this time comprises pretreatment time and extracts total time, is significantly less than 2～8 hours of classical acid extraction method; Molecular weight is determined as 116kDa through GPC, larger than the beet pectin molecular weight (≤100kDa) extracted under acidic conditions; In extracting solution, except beet pectin, filter residue is mainly the biodegradable components such as Mierocrystalline cellulose and hemicellulose, and filtrate is mainly water-soluble carbohydrate, not containing the poisonous chemical reagent such as soda acid, environmentally safe.
Embodiment 4:
The first step to remove the small molecules such as sucrose residual in beet pulp, glucose, inorganic salt, after filtering with nylon cloth is dried beet pulp wash-out 10min in the distilled water of 40 ℃ under 40 ℃, and in the control beet pulp, biodiversity content is lower than 6%;
Second step is made into by the beet pulp of oven dry and distilled water feed liquid that liquid-solid ratio is 70:1 and is placed under electrostatic field and ultrasonic field condition and carries out pre-treatment.Strength of electric field is 28kV, and frequency is 55kHz,, ultrasound intensity 0.70W/cm
2, frequency is 30kHz, and the treatment time is 30min, and temperature is 40 ℃;
The 3rd step is extracted pectin by pretreated feed liquid under subcritical water (120 ℃, the distilled water under 10MPa) condition.First the speed with 4 ℃/min is warmed up to design temperature (120 ℃), two pressure (boost (in 1min) to setting pressure (10MPa) by feed liquid from standard atmospheric pressure transformation period fast, extract 10min under insulation (120 ℃) constant voltages (10MPa) condition, (5s in) drops to standard atmospheric pressure by pressure fast, completes a pressure transformation period) after take out feed liquid.Extract total time 20min two transformation periods;
The 4th step will be concentrated into 5% of original volume after the 3rd step gained extracting liquid filtering under 65 ℃, the long-pending centrifugal rear washed with isopropyl alcohol of using of isopropanol precipitating, 9000rpm with tetraploid, at-60 ℃, 0.1MPa dry 24h under vacuum tightness, in dried pectin, the massfraction of contained level is not more than 5%, obtains beet pectin.The yield that obtains beet pectin through weighting method is 18.32%.
The present embodiment beet pectin preparation time is only 40min, and this time comprises pretreatment time and extracts total time, is significantly less than 2～8 hours of classical acid extraction method; ; Molecular weight is determined as 118kDa through GPC, larger than the beet pectin molecular weight (≤100kDa) extracted under acidic conditions; In extracting solution, except beet pectin, filter residue is mainly the biodegradable components such as Mierocrystalline cellulose and hemicellulose, and filtrate is mainly water-soluble carbohydrate, not containing the poisonous chemical reagent such as soda acid, environmentally safe.
As can be seen from the above embodiments, through the electrostatic field of different condition and the beet pectin of ultrasonic pretreatment and subcritical water extraction, can prepare and meet industrial production and the high beet pectin product of edible safety.Compare with traditional extraction technology, adopt the subcritical water required time to be no more than 60min, than the preparation time of 2～8 hours of classical acid extraction method, shortened 2～8 times.Simultaneously, also can avoid the degraded of pectin molecule under acidic conditions.Owing to not adding the poisonous and harmful chemical reagent in leaching process, avoided the pollution of environment.
Claims (8)
1. the environment-friendly preparation method thereof of a beet pectin is characterized in that containing following steps:
(1), by the beet pulp distilled water wash, filter post-drying;
(2) step (1) gained beet pulp and distilled water are made into to the feed liquid that liquid-solid ratio is 100:1～10:1, are placed under electrostatic field and ultrasonic field condition and carry out pre-treatment, strength of electric field is 8～32kV, and frequency is 5～70kHz, and ultrasound intensity is 0.35～0.88W/cm
2, frequency is 20～50kHz, and the treatment time is 5～30min, and temperature is 25～50 ℃;
(3) under sub-critical water extraction, step (2) the gained feed liquid of take is extracted pectin as raw material, and temperature is 100～300 ℃, and pressure is 2MPa～20MPa, and pressure transformation period is 1～3 time, and extraction total time is 5min～90min; Described pressure refers to first feed liquid is raised to 2MPa～20MPa setting pressure from standard atmospheric pressure transformation period, and constant voltage drops to standard atmospheric pressure after extracting again, and the time that constant voltage is extracted is for extracting total time divided by pressure number transformation period; Described extract refer to total time all pressure in transformation period under setting pressure and design temperature the summation of constant voltage extraction time; Do not comprise the heating-up time, pressure rising time and step-down time;
(4) step (3) gained feed liquid filtered, use isopropanol precipitating after concentrated, use washed with isopropyl alcohol after centrifugal again, lyophilize, obtain beet pectin.
2. the environment-friendly preparation method thereof of beet pectin according to claim 1, it is characterized in that: described washing is the distilled water wash-out 8-15min with 40 ℃-45 ℃ by beet pulp.
3. the environment-friendly preparation method thereof of beet pectin according to claim 1 is characterized in that: described oven dry is that the beet pulp after washing is filtered to post-drying with nylon cloth; Biodiversity content after beet pulp is dried is not more than 6%.
4. the environment-friendly preparation method thereof of beet pectin according to claim 1, is characterized in that: the filtration of described feed liquid filtration employing nylon cloth.
5. the environment-friendly preparation method thereof of beet pectin according to claim 1 is characterized in that: described concentrated be to 5% of original volume at 50～70 ℃ of lower vacuum concentration.
6. the environment-friendly preparation method thereof of beet pectin according to claim 1 is characterized in that: the volume of described Virahol is feed liquid 1～4 times.
7. the environment-friendly preparation method thereof of beet pectin according to claim 1, it is characterized in that: described centrifugal rotating speed is 8000-10000rpm.
8. the environment-friendly preparation method thereof of beet pectin according to claim 1, it is characterized in that: described lyophilize is at-60 ℃～-55 ℃, dry 20～24h under 0.1～0.2MPa vacuum tightness, in dried pectin, the massfraction of contained level is not more than 5%.
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| PCT/CN2013/090062 WO2015027645A1 (en) | 2013-08-28 | 2013-12-20 | Preparation method for beet pulp pectin |
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| CN105294883A (en) * | 2015-10-13 | 2016-02-03 | 华南理工大学 | Method for preparing beet pectin in diluted acid-pressing way |
| CN105440155A (en) * | 2015-12-28 | 2016-03-30 | 西北农林科技大学 | Pectin extraction method |
| CN108892741A (en) * | 2018-07-27 | 2018-11-27 | 齐鲁工业大学 | A kind of extracting method of peach pectin |
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| CN103923226A (en) * | 2014-04-23 | 2014-07-16 | 赛珂睿德生物医药科技(上海)有限公司 | Method for pretreating raw material for preparing pectin |
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| CN105294883A (en) * | 2015-10-13 | 2016-02-03 | 华南理工大学 | Method for preparing beet pectin in diluted acid-pressing way |
| CN105294883B (en) * | 2015-10-13 | 2017-06-20 | 华南理工大学 | A kind of method that diluted acid-pressurization prepares beet pectin |
| CN105440155A (en) * | 2015-12-28 | 2016-03-30 | 西北农林科技大学 | Pectin extraction method |
| CN105440155B (en) * | 2015-12-28 | 2018-05-25 | 西北农林科技大学 | A kind of pectin extraction method |
| CN108892741A (en) * | 2018-07-27 | 2018-11-27 | 齐鲁工业大学 | A kind of extracting method of peach pectin |
| WO2021090898A1 (en) * | 2019-11-08 | 2021-05-14 | 日本甜菜製糖株式会社 | Method for producing water-soluble polysaccharides |
| JP7425083B2 (en) | 2019-11-08 | 2024-01-30 | 日本甜菜製糖株式会社 | Method for producing water-soluble polysaccharides |
| WO2023231292A1 (en) * | 2022-05-31 | 2023-12-07 | 华南理工大学 | Beet pulp all-component emulsifying thickener, preparation method therefor, and application thereof |
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Application publication date: 20140101 |