CN101627825A - Novel method for extracting pectin from sweet potato dregs - Google Patents
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Abstract
The invention discloses a novel method for extracting pectin from sweet potato dregs. The method comprises the following steps of: 1) preparing the sweet potato dregs into a suspension, carrying out physical screening processing on the suspension, and removing most starch to obtain dietary fibers with higher purity; 2) using amylase to carry out enzymolysis on residual small amount of starch in the dietary fibers in step 1), carrying out centrifugation, removing supernate, and collecting sediments; and 3) preparing the sediments obtained in step 2) into the suspension, adding Na2HPO4 solution into the suspension to extract the pectin, carrying out centrifugation after extracting, collecting supernatant, and carrying out concentration and drying to obtain pectin powder. The method can make the extraction ratio of the sweet potato pectin reach 95.87 percent and the purity of pectin products reach 91.28 percent (taking Xu55-2 as a material). The method has the advantages of high extraction ratio, high pectin purity, strong practicality, easy industrialization and the like. The products can be directly used as food additives or pharmaceutical excipients. The method not only can improve the comprehensive economic benefit of potato processing, but also can reduce the environmental pollution caused by accumulation of the potato dregs.
Description
Technical field
The present invention relates to a kind of method of from sweet potato dregs, extracting pectin.
Background technology
China is maximum in the world sweet potato producing country, and according to the FAO statistics, China's yield of sweet potato was about 10,700 ten thousand tons in 2005, accounted for 84.64% of whole world total output.In China, sweet potato mainly is to be used to extract starch, making bean vermicelli, vermicelli and exploitation sweet potato beverage etc., produces a large amount of potato slags in the process of processing, accounts for the 10%-14% of raw material, and is different according to kind.Dietary fiber content in the sweet potato dregs is about 22%, and pectin content is about 25% in the Rhizoma Dioscoreae esculentae dietary fiber, is good pectin source.At present, the potato slag is mainly used in animal feed or directly abandons, and causes the significant wastage of environmental pollution and resource.
Dietary fiber is the general name of the cellulose that is difficult for being absorbed by human consumption, hemicellulose, lignin, pectic substance.Pectin is the soluble component in the dietary fiber, has good gelling, thickening stabilities, and emulsification property has been widely used in the processing of jam, jelly, candy, lactic acid and fruit drink and bakery product.Pectin has physiological functions such as the blood fat of adjusting, blood sugar, inhibition tumor growth and diffusion, has vast market prospect in medicine and health products trade.At present, China's pectin annual requirement is about 1500 tons, and with annual 15% speed increase.
Pectin is extracted on a lot of crops such as oranges and tangerines, apple, pears, banana, beet, sugarcane, mango report, and common pectin extraction method all is an one-step method, directly handles raw material, extracts pectin.Extracting method comprises acid system, microbial method, microwave method, enzymatic isolation method and ion-exchange-resin process.There are a large amount of starch in the sweet potato dregs, how to adopt simple and direct, effective ways, obtain high-purity, the high-quality sweet potato pectin is a technical barrier, the method hydrolyzed starch of conventional acidolysis and enzymolysis, extracts not only cost height of pectin, also influences pectin product quality and purity.
Summary of the invention
The purpose of this invention is to provide a kind of method of from sweet potato dregs, extracting pectin.
The method of extracting pectin from sweet potato dregs provided by the present invention may further comprise the steps:
1) sweet potato dregs is made into suspension, described suspension is sieved processing, collection can be a 150-180 μ m screen cloth by the aperture, but can not be by the part of 35-50 μ m screen cloth, and drying obtains dietary fiber;
2) dietary fiber with step 1) is made into suspension, adds the remaining starch in the described dietary fiber of amylase enzymolysis, the centrifugal supernatant of abandoning, and collecting precipitation is standby;
3) with step 2) precipitation that obtains is made into suspension, to wherein adding extractant Na
2HPO
4Extract pectin, centrifugal after extraction finishes, collect supernatant, concentrate drying obtains pectin.
Described step 1) suspension is made up of sweet potato dregs and water, and the mass ratio of described sweet potato dregs and water is 1: (40-60), be preferably 1: (50-60); The pH value of described suspension is 5.0-9.0, is preferably 5.0-7.0; The screening time that described screening is handled is 10-20min, and the sifting vibrating frequency is 3.25-3.75Hz, is preferably 3.50-3.75Hz;
Especially be preferably following 1)-3) in any:
1) in the described step 1) suspension, the mass ratio of described sweet potato dregs and water is 1: 50; The pH value of described suspension is 5.0; The screening time is 15min in the described screening processing procedure, and the sifting vibrating frequency is 3.75Hz;
2) in the described step 1) suspension, the mass ratio of described sweet potato dregs and water is 1: 60; The pH value of described suspension is 7.0; The screening time is 10min in the described screening processing procedure, and the sifting vibrating frequency is 3.75Hz;
3) in the described step 1) suspension, the mass ratio of described sweet potato dregs and water is 1: 60; The pH value of described suspension is 5.0; The screening time is 20min in the described screening processing procedure, and the sifting vibrating frequency is 3.50Hz.
Described step 2) method is that the dietary fiber with step 1) is made into suspension, handles through gelatinization, and is centrifugal then to wherein adding the amylase degradable starch, abandons supernatant, collecting precipitation; Wherein, described step 2) suspension is made up of dietary fiber and water, and the mass ratio of described dietary fiber and water is 1: (60-100); Described diastatic consumption is that every gram dietary fiber adding 1-5ml concentration is 0.5% amylase, and described centrifugal RCF is 1000-2000g, and centrifugation time is 30min.
Described Na
2HPO
4Consumption be that to add 2-8ml concentration be the Na of 1M for every gram dietary fiber
2HPO
4Solution, the described centrifugal RCF of step 3) is 1000-2000g, centrifugation time is 30min.
Described step 3) suspension is by step 2) precipitation and the water collected forms, and the mass ratio of described precipitation and water is 1: (60-140); The temperature of described extraction is 70-90 ℃; Extraction time is 2-10h;
Be preferably following 1)-3) in any:
1) in the step 3), the mass ratio of described precipitation and water is 1: 80; Described extraction temperature is 85 ℃; Described extraction time is 6h;
2) in the step 3), described precipitation is 1: 100 with the water quality ratio; Described extraction temperature is 80 ℃; Described extraction time is 8h;
3) in the step 3), described precipitation is 1: 100 with the water quality ratio; Described extraction temperature is 85 ℃; Described extraction time is 6h.
Sweet potato dregs of the present invention is that batch production is produced waste residue that sweet potato starch produced or other food industry and used sweet potato to be waste residue that raw material produced.
Method of the present invention is material with the sweet potato dregs, separates obtaining dietary fiber earlier quickly and easily by a kind of physics method for sieving, on the basis that obtains high-purity edible fiber, extracts pectin then, screens out starch in reclaiming the dietary fiber process.This extracts the method for pectin, and pectin recovery rate and purity height, impurity are few, can be applied to large-scale industrial production.
Adopting method of the present invention, is raw material with Xu 55-2 sweet potato dregs, and the dietary fiber recovery rate is 83.18%, purity 81.25%, and pectin recovery rate, purity peak can reach 95.87%, 91.28% respectively.
Method of the present invention has the following advantages:
1, can reclaim starch in the extraction pectin process;
2, can obtain high-quality and highly purified dietary fiber by the screening processing;
3, extraction process is simple, easy to operate;
4, low, the easy batch production production of cost;
5, pectin recovery rate and purity are higher, and quality better can directly be used as food additives and medicine auxiliary material.
6, this method also is applicable to starch-containing higher raw material such as potato residues, manioc waste, and the extraction of dietary fiber and pectic substance not only can improve the overall economic efficiency of potato class processing, has also reduced the environmental pollution that the potato slag muck manufactures.
Description of drawings
Fig. 1 is a pectous extracting method flow chart of the present invention.
Fig. 2 is the particle size distribution figure of sweet potato starch among the embodiment 1.
Fig. 3 is the dietary fiber screening plant among the embodiment 1, and A is a constant temperature oscillator, and B is the standard test sieve in different apertures.
Fig. 4 is the food fibre powder of embodiment 2 preparations.
Fig. 5 is the dry back sweet potato pectin powder of embodiment 2 preparations.
The gel that Fig. 6 forms for sweet potato pectin.
Fig. 7 is the calibration curve of galacturonic acid content among the embodiment 2.
The specific embodiment
Technical scheme of the present invention is sweet potato dregs → preparation Rhizoma Dioscoreae esculentae dietary fiber (recovery starch) → extraction pectin, and the pectous extracting method flow process is seen Fig. 1, and concrete steps are as follows successively:
1, after the dry sweet potato dregs dehydration, tiling, thickness is no more than 1cm, and 60 ℃ of air-dry dry 24h of temperature do not stop to stir, and raw material are heated evenly, dried sweet potato dregs water content 5%.
2, pulverize mensuration pulverizing back sweet potato dregs powder and directly distribute (in 0～150 mu m range, requiring wherein, the particle of 35～150 μ m accounts for 50～70%), preferably pulverize the time, be beneficial to screening removal starch.
3, the sweet potato dregs after screening is pulverized, by certain solid-liquid ratio, be made into suspension, regulate pH value (5.0～9.0), the Rhizoma Dioscoreae esculentae dietary fiber suspension passes through time sieve of a 35-50 μ m more earlier through 150-180 μ m primary dcreening operation, regulate vibration frequency, control time, remove desizing, the part that inferior sieve is held back is dietary fiber.
4, the dry time sieve of collecting is held back part, drying, and the control moisture is below 5%.
5, pulverize dry back dietary fiber and pulverize (the pulverizing time is identical with the sweet potato dregs pulverizing time), crossing the aperture is the standard screen of 180 μ m.
6, remove starch dietary fiber and water by certain solid-liquid ratio, be made into suspension, homogeneous, the high temperature gelatinization, every gram dietary fiber adding 1-5ml concentration is 0.5% amylase, 60 ℃ of oscillating reactions 30 minutes, 1000-2000g removes supernatant after centrifugal 30 minutes.
7, centrifuged deposit is collected in the extraction of pectin, and it is outstanding turbid to add water by certain solid-to-liquid ratio, and every gram dietary fiber adds the Na of 2-8ml
2HPO
4Solution, extracts 2-10h, centrifugal 30 minutes of 1000-2000g by 70-90 ℃.
8, dry that the supernatant warp is concentrated, freezing or spray-drying gets the pectin finished product.
The process optimization of embodiment 1, extraction sweet potato pectin
1, sweet potato dregs is pulverized and particle size determination
Laser granulometry (BT-9300H) is measured the size distribution of sweet potato starch, the screening aperture when determining to remove starch.The result shows that the granularity of sweet potato starch mainly is distributed in 0-35 μ m (see figure 2).
Take by weighing 30g sweet potato dregs (kind is Xu 55-2), pulverize with Universalpulverizer (FW100 type), observe different pulverizing time sweet potato dregs particle size distribution ranges (sweet potato dregs granularity 0-150 μ m, and 35～150 μ m particles account for total amount 50～70% and are the best pulverizing time), determine that finally the best pulverizing time is 20s.
2, from sweet potato dregs, separate Rhizoma Dioscoreae esculentae dietary fiber
With the sweet potato dregs after pulverizing earlier through a primary dcreening operation (mesh size is 150-180 μ m), with the dietary fiber that guarantees to obtain below certain particle size, again by time sieve (mesh size be 35-50 μ m) of an aperture, except that desizing greater than known starch granularity.Two sieves are under extraneous dynamic action, and double vibrations sieves (screening plant is seen Fig. 3).Concrete grammar is as follows: the sweet potato dregs after will pulverizing mixes (mass ratio 1: 40-60) be made into suspension with water by certain solid-liquid ratio, regulator solution pH value (5.0-9.0), control screening time (10-20min) and sifting vibrating frequency (3.25-3.75Hz), screen out starch, obtain food fibre powder, pass through L
93
4Orthogonal test, (the quadrature factor level sees Table 1) is optimized the sieving technology parameter, and having drawn the optimum process parameter is solid-liquid ratio 1: 60, and suspension pH value is 5.0, and the screening time is 20min, double vibrations frequency 3.75Hz (orthogonal experiments sees Table 2).
3, from Rhizoma Dioscoreae esculentae dietary fiber, extract pectin
Accurately take by weighing 0.25g step 2) preparation Rhizoma Dioscoreae esculentae dietary fiber, add 20mL distilled water, 12000 rev/mins of homogeneous 20s, 100 ℃ of gelatinization 5min, be cooled to below 60 ℃, to wherein adding 0.25～1.25ml concentration is 0.5% AMS (the extensive and profound in meaning star in Beijing) solution, and 60 ℃ of oscillating reactions 30min remove starch.Reacted suspension is abandoned supernatant, collecting precipitation with the centrifugal 30min of the rotating speed of 1500g.To precipitate by certain solid-liquid ratio outstanding turbid, adding (0.5～2ml) 1M Na
2HPO
4Solution, the control temperature and time extracts pectin, and pectin extracting soln is concentrated, is the sweet potato pectin powder after the drying.On the basis of single factor experiment, be factor with extraction solid-liquid ratio, extraction time, extraction temperature, be the secondary rotating orthogonal test (seeing Table 3-table 5) that index is carried out three factors, five levels with the pectin recovery rate.Single factor experiment and secondary rotating orthogonal result of the test show that it is AMS 0.5ml, 1M Na that pectin extracts the optimum process parameter
2HPO
41.5ml, solid-liquid ratio 1: 100, extract 85 ℃ of temperature, extraction time 6h.
Table 1 sieving technology parameter quadrature factor level table
Table 2 sieving technology parameter Orthogonal Experiment and Design (L
93
4) and table as a result
To temperature (Z
1), extraction time (Z
2), solid-liquid ratio (Z
3) to do conversion as follows: X1=(Z1-80)/5, X2=(Z2-6)/2, X3=(Z3-100)/20 is an independent variable with X1, X2, X3, and the recovery rate of pectin is response (Y), and experimental design and result of the test see Table 3.
Table 4 secondary rotating orthogonal experimental design and table as a result thereof
The test data of his-and-hers watches 4 is analyzed, and the ternary quadratic regression equation that obtains each factor and recovery rate is Y=95.52493+3.16283X
1+ 4.88009X
2+ 2.36151X
3-1.81021X
1 2-4.37229X
2 2-4.30974X
3 2+ 1.92435X
1X
3Analysis of variance table sees Table 5.
Table 5 secondary rotating orthogonal result of the test analysis of variance table
Embodiment 2, sweet potato pectin recovery rate and purity detecting
1, sweet potato dregs is pulverized and particle size determination
Take by weighing the sweet potato dregs (kind is Xu 55-2) of 30g drying, pulverize 20s with Universalpulverizer (FW100 type), measure different pulverizing time sweet potato dregs particle size distribution ranges, the result shows the sweet potato dregs granularity smaller or equal to 150 μ m, and 35～150 μ m particles account for total amount 50～70%.
2, from sweet potato dregs, separate Rhizoma Dioscoreae esculentae dietary fiber
The 15g sweet potato dregs that step 1) is obtained and water are to mix at 1: 60 by mass ratio, be made into suspension, regulator solution pH value is 5.0, double vibrations frequency 3.75Hz sieves 20min, screen out starch, obtain 3.66g dietary fiber (this number is following DF1) (see figure 4), wherein total dietary fiber content is 2.97g (this number is following DF2)
Dietary fiber recovery rate and purity computational methods are as follows:
Dietary fiber recovery rate (%)=DF2 * 100/DF
Dietary fiber purity (%)=DF2 * 100/DF1
Total dietary fiber content in DF-sample
The dietary fiber weight of DF1-from sample, sieve out
Total dietary fiber content among DF2-DF1
The total dietary fiber assay adopts enzyme-gravimetric method, with reference to AOAC991.43.Detection shows that sieve method gained dietary fiber recovery rate is 83.18%, purity 81.25%.
3, from Rhizoma Dioscoreae esculentae dietary fiber, extract pectin
Accurately take by weighing 0.25g step 2) preparation Rhizoma Dioscoreae esculentae dietary fiber, add 20mL distilled water, 12000 rev/mins of homogeneous 20s, 100 ℃ of gelatinization 5min, be cooled to below 60 ℃, to wherein adding 0.5ml concentration is 0.5% AMS (the extensive and profound in meaning star in Beijing) solution, and 60 ℃ of oscillating reactions 30min remove starch.Reacted suspension is abandoned supernatant, collecting precipitation with the centrifugal 30min of the rotating speed of 1500g.To precipitate with water is to mix at 1: 100 with mass ratio, is made into suspension, adds 1M Na in suspension
2HPO
4Solution 1ml extracts pectin under 85 ℃ of conditions, extraction time is 6h, and centrifugal 30 minutes of 1500g collects supernatant (pectin extracting soln), pectin extracting soln concentrates, after the drying 0.043g jelly powder (see figure 5), see Fig. 6 by the gel that the sweet potato pectin powder forms.
4, total pectin content is measured referring to " japanese food section electrotechnics is understood new-food analysis method " in the potato slag.Pectin purity employing carbazole sulfuric acid process (McComb, E.A., and McCready, R.M. (1952) Colorimetricdetermination of pectic substances.Anal.Chem, 24,1630-1632), measure galacturonic acid content in the pectin.
The carbazole sulfuric acid process
Principle: pectin hydrolysate-galacturonic acid under the strong acid effect with the carbazole condensation, generate the material of purple, the linear μ g/mL of this material light absorption value and galacturonic acid content
1) calibration curve is drawn
Accurately take by weighing D-galacturonic acid 100mg, be dissolved in the distilled water, be settled to 100mL, fully mixing.Get 1.0,2.0,3.0,4.0,5.0,6.0,7.0,8.0 respectively, the galacturonic acid solution of 9.0mL 100mg/mL is settled to 100mL in volumetric flask, and promptly obtaining one group of concentration is 10,20,30,40, the galacturonic standard acid solution of 50,60,70,80,90 μ g/mL.
Get the 12mL concentrated sulfuric acid respectively in 10 25mL scale test tubes, cool off in the ice bath, add each 2mL of variable concentrations galacturonic acid solution (0-90 μ g/mL, 0 μ g/mL is a blank) respectively, fully behind the mixing, put and heat 10min in the boiling water, be cooled to room temperature, add 0.15% carbazole 1mL in every pipe respectively, fully mixing, after placing 30min under the room temperature, measure light absorption value down in 530nm with ultraviolet specrophotometer.With the galacturonic acid content is abscissa, and light absorption value is an ordinate, and production standard curve (see figure 7) calculates equation of linear regression and is: y=0.0049x-0.0008, r
2=0.9989.
The light absorption value of table 6 calibration curve
2) galacturonic acid content is measured
Get 1mL0.5% (w/v) pectin solution and in volumetric flask, be settled to 50mL, obtain the pectin solution that ultimate density is 0.01% (w/v).Get the 12mL concentrated sulfuric acid in 25mL tool plug scale test tube, ice bath slowly adds the 2mL pectin solution down, abundant mixing, boiling water bath heating 15min, after be cooled to room temperature, add 1mL0.5% carbazole solution, fully mixing, measure light absorption value down in 530nm after placing 30min under the room temperature, calculate the content of galacturonic acid in the pectin by calibration curve.Measure to such an extent that the light absorption value of sample is 0.446, calculating sample galacturonic acid concentration is 91.20 μ g/mL.
According to above data computation pectin recovery rate, pectin yield and pectin purity, concrete computational methods are as follows:
Pectin recovery rate (%)=G * 100/W
Pectin yield (%)=W1 * 100/W2
Pectin purity (%)=G * 100/W1
Total pectin content in W-sweet potato dregs
G-galacturonic acid content
The weight of W1-jelly powder
The weight of W2-sweet potato dregs
Three repetitions are established in experiment.The result shows that the content of total pectin (W) in the 30g sweet potato dregs (W2) (kind is Xu's potato 55-2) is 1.41 ± 0.62g, and the quality of jelly powder (W1) is 1.48 ± 0.48g, and galacturonic acid content is 1.36 ± 0.37g;
Calculating the sweet potato pectin recovery rate is 95.87 ± 0.51%, and pectin yield is 4.93 ± 0.72%, and pectin purity is 91.28 ± 0.58%.
Claims (8)
1, a kind of method of extracting pectin from sweet potato dregs may further comprise the steps:
1) sweet potato dregs is made into suspension, described suspension is sieved processing, collection can be a 150-180 μ m screen cloth by the aperture, but can not be by the part of 35-50 μ m screen cloth, and drying obtains dietary fiber;
2) dietary fiber with step 1) is made into suspension, adds degrade remaining starch in the described dietary fiber of amylase, the centrifugal supernatant of abandoning, and collecting precipitation is standby;
3) with step 2) precipitation that obtains is made into suspension, to wherein adding extractant Na
2HPO
4Solution extracts pectin, and is centrifugal after extraction finishes, and collects supernatant, obtains pectin.
2, method according to claim 1 is characterized in that: described step 1) suspension is made up of described potato slag and water, and the mass ratio of described potato slag and water is 1: (40-60); The pH value of described suspension is 5.0-9.0; The screening time was 10-20min during described screening was handled, and the sifting vibrating frequency is 3.25-3.75Hz.
3, method according to claim 2 is characterized in that: in the described step 1) suspension, the mass ratio of described potato slag and water is 1: (50-60); The pH value of described suspension is 5.0-7.0; Described sifting vibrating frequency is 3.50-3.75Hz.
4, method according to claim 3 is characterized in that: in the described step 1) suspension, the pH value of the described potato slag and the mass ratio of water, described suspension, described screening time and sifting vibrating frequency are following 1)-3) in any:
1) in the suspension of described step 1), the mass ratio of described potato slag and water is 1: 50; The pH value of described suspension is 5.0; The described screening time is 15min, and the sifting vibrating frequency is 3.75Hz;
2) in the described step 1) suspension, the mass ratio of described potato slag and water is 1: 60; The pH value of described suspension is 7.0; The described screening time is 10min, and the sifting vibrating frequency is 3.75Hz;
3) in the described step 1) suspension, the mass ratio of described potato slag and water is 1: 60; The pH value of described suspension is 5.0; The described screening time is 20min, and the sifting vibrating frequency is 3.50Hz.
5, according to arbitrary described method among the claim 1-4, it is characterized in that: method described step 2) is that the dietary fiber with step 1) is made into suspension, carries out gelatinization, and is centrifugal then to wherein adding the amylase degradable starch, abandons supernatant, collecting precipitation; Described step 2) suspension is made up of described dietary fiber and water, and the mass ratio of described dietary fiber and water is 1: (60-100); Described diastatic consumption is that every gram dietary fiber adding 1-5ml concentration is 0.5% AMS, and described centrifugal RCF is 1000-2000g, and centrifugation time is 30min.
6, according to arbitrary described method among the claim 1-5, it is characterized in that: described Na
2HPO
4Consumption be that to add 2-8ml concentration be the Na of 1M for every gram dietary fiber
2HPO
4, the described centrifugal RCF of step 3) is 1000-2000g, centrifugation time is 30min.
7, according to arbitrary described method among the claim 1-6, it is characterized in that: described step 3) suspension is made up of described precipitation and water, and the mass ratio of described precipitation and water is 1: (60-140); The temperature of described extraction is 70-90 ℃, and extraction time is 2-10h.
8, method according to claim 7 is characterized in that: in the described step 3), the mass ratio of described precipitation and water, the temperature of described extraction, described extraction time are following 1)-3) in any:
1) in the step 3), the mass ratio of described precipitation and water is 1: 80; Described extraction temperature is 85 ℃; Described extraction time is 6h;
2) in the step 3), described precipitation is 1: 100 with the water quality ratio; Described extraction temperature is 80 ℃; Described extraction time is 8h;
3) in the step 3), described precipitation is 1: 100 with the water quality ratio; Described extraction temperature is 85 ℃; Described extraction time is 6h.
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| CN102558386A (en) * | 2012-01-18 | 2012-07-11 | 河南科技学院 | Method for extracting pectin from sweet potato dregs |
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