CN109602028B - Extraction method of soluble dietary fiber from pineapple peel residues - Google Patents
Extraction method of soluble dietary fiber from pineapple peel residues Download PDFInfo
- Publication number
- CN109602028B CN109602028B CN201811461811.6A CN201811461811A CN109602028B CN 109602028 B CN109602028 B CN 109602028B CN 201811461811 A CN201811461811 A CN 201811461811A CN 109602028 B CN109602028 B CN 109602028B
- Authority
- CN
- China
- Prior art keywords
- dietary fiber
- drying
- soluble dietary
- pineapple peel
- shearing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/20—Reducing nutritive value; Dietetic products with reduced nutritive value
- A23L33/21—Addition of substantially indigestible substances, e.g. dietary fibres
- A23L33/22—Comminuted fibrous parts of plants, e.g. bagasse or pulp
Abstract
The invention relates to the field of agricultural product processing, and discloses a method for extracting soluble dietary fiber from pineapple peel residues. The extraction method of the invention extracts the soluble dietary fiber by processing the pineapple peel residue through the steps of degreasing, double-enzyme hydrolysis, shearing modification, acid bath, alcohol precipitation, drying and the like, has simple extraction method and low cost, and the yield of the finished product of the soluble dietary fiber reaches up to 19.22 percent. The method can provide reference for extracting the soluble dietary fiber in the pineapple peel residue, and has good application prospect.
Description
Technical Field
The invention relates to a method for extracting soluble dietary fiber, in particular to a method for extracting soluble dietary fiber from pineapple peel residues, and belongs to the field of agricultural product processing.
Background
The dietary fiber is a functional food base material which is internationally recognized at present, is called as 'seventh nutrient' after saccharides, protein, fat, vitamins, minerals and water, has the effects of preventing obesity, enhancing immunity, preventing diabetes, preventing colon cancer, inhibiting harmful bacteria and the like, and is one of main raw materials for developing functional foods. Dietary fiber can be classified into two major groups, i.e., Insoluble Dietary Fiber (IDF) and Soluble Dietary Fiber (SDF), according to its solubility in water. The insoluble dietary fiber has water retention and imbibition effects, and can increase body satiety and digestive residue wettability after intake, and can be used for treating obesity and relieving constipation. The soluble dietary fiber can adsorb heavy metal, bile acid and cholesterol, and has remarkable effect in preventing coronary heart disease, improving various chronic diseases and other diseases caused by the improvement of living standard. However, the resource shortage of the water-soluble dietary fiber causes high production and application cost, and limits the application and research and development of related products. Therefore, the search and development of water-soluble dietary fiber from agricultural product processing waste and low-value resources will be an important technical research problem for the development of food industry.
Pineapple, also known as pineapple and yellow pear, belongs to tropical and subtropical fruits. China, Guangdong, Guangxi and Hainan, has wide planting range and is commonly used for producing concentrated fruit juice and the like. The pineapple peel residue is waste after the concentrated pineapple juice is produced, and contains rich dietary fiber. Due to the shortage of processing technology and related research, a large amount of skin slag is discarded, which not only causes resource waste, but also aggravates environmental pollution. Therefore, a set of safe and feasible method for extracting the dietary fiber from the pineapple peel residue with high efficiency and low cost is established, a new way is provided for further resource utilization of the pineapple peel residue, and the method has important significance for prolonging the industrial chain of pineapples and guiding the deep processing of the pineapples. At present, the extraction method of the soluble dietary fiber of the pineapple peel residue mainly comprises a chemical method, a microbial fermentation method, an enzymatic method and the like.
Disclosure of Invention
The invention aims to provide an extraction method of soluble dietary fiber of pineapple peel residue, which adopts double-enzyme hydrolysis, shearing modification and residue acid bath processes to extract the soluble dietary fiber of the pineapple peel residue, so as to obtain a product with high extraction rate and high purity, and achieve the purposes of improving the utilization rate of the pineapple peel residue and realizing high-efficiency utilization of resources.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the extraction method of the soluble dietary fiber of the pineapple peel residue is characterized by comprising the following steps:
(1) degreasing: screening pineapple peel residues discarded in fruit juice processing production, cleaning, blanching with hot water, drying, crushing, and degreasing to obtain a degreased material;
(2) double-enzyme hydrolysis: respectively adding alpha-amylase and papain into the degreased material prepared in the step (1) for hydrolysis reaction, inactivating enzyme after hydrolysis, cooling to room temperature, filtering, and collecting filter residue to obtain dietary fiber raw material; storing the filtrate for later use;
(3) shearing modification: adding an oxalic acid solution into the dietary fiber raw material prepared in the step (2), uniformly mixing, shearing, dispersing and mixing to obtain a modified material;
(4) acid bath: heating and leaching the modified material obtained in the step (3), filtering after leaching is finished, and collecting filtrate;
(5) alcohol precipitation, concentration and drying: combining the filtrates obtained in the steps (2) and (4), and concentrating to 1/8-1/10 of the original volume to obtain a concentrated solution; slowly adding ethanol with the volume concentration of 95% to 3-6 times of the concentrated solution into the concentrated solution, uniformly mixing, standing for 3-8 h at 4 ℃, centrifuging, collecting precipitate, washing for 1-2 times by using ethanol with the volume concentration of 95%, finally drying the precipitate, and grinding into fine powder to obtain the soluble dietary fiber.
Further, the hot water blanching temperature in the step (1) is 85-100 ℃, and the blanching time is 1-3 min; the drying method of the pineapple peel residues comprises the following steps: drying with hot air at 45-60 ℃ for 36-48 h; crushing and sieving with a 40-100 mesh sieve; the degreasing operation is as follows: according to the material-liquid ratio of 1: adding petroleum ether into the crushed material in a ratio of 3-6 (m/v), stirring and soaking at room temperature for 1-4 h, performing suction filtration, and air-drying to obtain the degreased material.
Further, the hydrolysis reaction in the step (2) comprises the following steps: adding distilled water into the degreased material according to a material-liquid ratio of 1:30-45 (m/v), adjusting the pH of the material liquid to 6.0-7.5, adding alpha-amylase accounting for 1-5% of the weight of the degreased material, carrying out water bath at 50-75 ℃ for 20-60 min, cooling to 40-60 ℃, adding papain accounting for 0.1-0.6% of the weight of the degreased material, and carrying out water bath for 20-60 min; continuously stirring, inactivating enzyme at 95 deg.C for 5min after hydrolysis, cooling to room temperature, filtering, and collecting residue to obtain dietary fiber raw material.
Preferably, the hydrolysis reaction in step (2) comprises the following steps: adding distilled water into the degreased material according to a material-liquid ratio of 1:30 (m/m), adjusting the pH value of the material liquid to 6.5, adding alpha-amylase accounting for 3% of the weight of the degreased material, carrying out water bath at 65 ℃ for 40min, cooling to 55 ℃, adding papain accounting for 0.2% of the weight of the degreased material, and carrying out water bath for 30 min; heating at 95 deg.C to inactivate enzyme for 5min after hydrolysis, cooling to room temperature, filtering, and collecting residue to obtain dietary fiber raw material.
Further, the mass fraction of the oxalic acid solution added in the step (3) is 1-5%, and the ratio of the added oxalic acid solution to the dietary fiber raw materials is 1:10 to 50 (m/v); the shearing apparatus is a high-speed shearing apparatus, the shearing speed is 7000-10000 r/min, and the shearing time is 10-50 min.
Preferably, the mass fraction of the oxalic acid solution in the step (3) is 3.2%, the shearing speed of the high-speed shearing machine for dispersion is 9000r/min, the shearing time is 20min, and the ratio of the added oxalic acid solution to the dietary fiber raw material is 1:34 (m/v).
Further, the acid bath leaching conditions in the step (4) are as follows: the leaching temperature is 50-100 ℃, and the leaching time is 0.5-3.0 h.
Preferably, the acid bath leaching conditions in the step (4) are as follows: the leaching temperature is 88 ℃, and the leaching time is 2 h.
Further, in the step (5), the filtrate is concentrated under vacuum and reduced pressure; the conditions for the centrifugation were: centrifuging at 4000-7000 r/min for 5-10 min, and freeze-drying the precipitate under the specific conditions: the temperature is-40 to-60 ℃, the pressure is 6 to 15Pa, and the drying time is 24 to 36 hours.
Compared with the prior art, the invention has the following beneficial effects: the extraction process provided by the invention is simple to operate, the extraction cost is low, the finished product has a high extraction rate, and the extraction rate of the soluble dietary fibers in the pineapple peel residues is up to 19.22%. The soluble dietary fiber obtained by the method has high purity, good physicochemical function and safe and reliable use, can provide reference basis for extraction of the soluble dietary fiber, and has good application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 Effect of acid species on SDF yield of pineapple bran
FIG. 2 influence of oxalic acid concentration on SDF yield of pineapple bran
FIG. 3 influence of extraction time on SDF yield of pineapple bran
FIG. 4 influence of extraction temperature on SDF yield of pineapple bran
FIG. 5 Effect of feed liquid ratio on SDF yield of pineapple bran
FIG. 6 is a curved surface diagram showing the influence of different extraction conditions on the SDF yield of pineapple peel residues
FIG. 7 influence of different extraction methods on SDF yield of pineapple peel residue
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to specific examples, which are only used for illustrating the present invention and do not limit the scope of the present invention. The experimental procedures used in the following examples are all conventional procedures unless otherwise specified. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A method for extracting soluble dietary fiber from pineapple peel residues comprises the following steps:
(1) degreasing: screening pineapple peel residues discarded in fruit juice processing production, cleaning, blanching with hot water at 85 ℃ for 3min, and drying with hot air at 45 ℃ for 48 h; crushing, sieving with a 40-mesh sieve, adding petroleum ether according to a material-to-liquid ratio of 1:5 (m/v), stirring and soaking at room temperature for 1h, performing suction filtration, and air-drying to obtain a degreased material;
(2) double-enzyme hydrolysis: adding distilled water into the degreased material prepared in the step (1) according to the material-liquid ratio of 1:30 (m/v), adjusting the pH value of the material liquid to 6.0, adding alpha-amylase accounting for 1% of the weight of the degreased material, carrying out water bath at 50 ℃ for 60min, cooling to 40 ℃, adding papain accounting for 0.1% of the weight of the degreased material, and carrying out water bath for 60 min; continuously stirring, heating to 95 deg.C after hydrolysis, inactivating enzyme for 5min, cooling to room temperature, filtering, and collecting residue to obtain dietary fiber raw material; storing the filtrate for later use;
(3) shearing modification: adding 1% by mass of oxalic acid solution into the dietary fiber raw material prepared in the step (2), wherein the ratio of the added oxalic acid solution to the dietary fiber raw material is 1:10 (m/v), uniformly mixing, shearing, dispersing and mixing by using a high-speed shearing instrument, wherein the shearing speed is 7000r/min, and the shearing time is 50min to obtain a modified material;
(4) acid bath: transferring the modified material obtained in the step (3) to a constant-temperature water bath vibration pot, leaching for 0.5h at 100 ℃, filtering after leaching is finished, and collecting filtrate;
(5) alcohol precipitation, concentration and drying: combining the filtrates obtained in the steps (2) and (4), and concentrating under vacuum to 1/8 of the original volume to obtain a concentrated solution; slowly adding ethanol with volume of 4 times of that of the concentrated solution into the concentrated solution, wherein the volume concentration of the ethanol is 95%, uniformly mixing, standing at 4 ℃ for 8h, centrifuging at 7000r/min for 5min, collecting precipitate, washing with ethanol with volume concentration of 95% for 1 time, freeze-drying the precipitate at-40 ℃ under the pressure of 15Pa for 36h, and grinding into fine powder to obtain the soluble dietary fiber.
Example 2
A method for extracting soluble dietary fiber from pineapple peel residues comprises the following steps:
(1) degreasing: screening pineapple peel residues discarded in fruit juice processing production, cleaning, blanching with hot water at 90 ℃ for 3min, and drying with hot air at 50 ℃ for 40 h; crushing, sieving with a 60-mesh sieve, adding petroleum ether according to a material-to-liquid ratio of 1:6 (m/v), stirring and soaking at room temperature for 3 hours, performing suction filtration, and air-drying to obtain a degreased material;
(2) double-enzyme hydrolysis: adding distilled water into the degreased material prepared in the step (1) according to the material-liquid ratio of 1:30 (m/v), adjusting the pH value of the material liquid to 7.5, adding alpha-amylase accounting for 2.5% of the weight of the degreased material, carrying out water bath at 75 ℃ for 20min, cooling to 60 ℃, adding papain accounting for 0.3% of the weight of the degreased material, and carrying out water bath for 20 min; continuously stirring, heating to 95 deg.C after hydrolysis, inactivating enzyme for 5min, cooling to room temperature, filtering, and collecting residue to obtain dietary fiber raw material; storing the filtrate for later use;
(3) shearing modification: adding an oxalic acid solution with the mass fraction of 5% into the dietary fiber raw material prepared in the step (2), wherein the ratio of the added oxalic acid solution to the dietary fiber raw material is 1:50 (m/v), uniformly mixing, shearing for 10min by using a high-speed shearing instrument at 10000r/min, dispersing, and mixing to obtain a modified material;
(4) acid bath: placing the modified material obtained in the step (3) in a constant-temperature water bath, leaching for 3.0h at 50 ℃, filtering after leaching is finished, and collecting filtrate;
(5) alcohol precipitation, concentration and drying: combining the filtrates obtained in the steps (2) and (4), and concentrating under vacuum to 1/10 of the original volume to obtain a concentrated solution; slowly adding ethanol with volume of 4 times of that of the concentrated solution into the concentrated solution, wherein the volume concentration of the ethanol is 95%, uniformly mixing, standing at 4 ℃ for 8h, centrifuging at 4000r/min for 10min, collecting precipitate, washing with ethanol with volume concentration of 95% for 2 times, freeze-drying the precipitate at-60 ℃ under the pressure of 6Pa for 24h, and grinding into fine powder to obtain the soluble dietary fiber. .
Example 3
A method for extracting soluble dietary fiber from pineapple peel residues comprises the following steps:
(1) degreasing: screening pineapple peel residues discarded in fruit juice processing production, cleaning, blanching with hot water at 90 ℃ for 2min, and drying with hot air at 55 ℃ for 48 h; crushing, sieving with a 80-mesh sieve, adding petroleum ether according to a material-to-liquid ratio of 1:3 (m/v), stirring and soaking at room temperature for 4 hours, performing suction filtration, and air-drying to obtain a degreased material;
(2) double-enzyme hydrolysis: adding distilled water of 40 times of the weight of the degreased material prepared in the step (1), adjusting the pH value of the material liquid to 6.5, adding alpha-amylase of 3% of the weight of the degreased material, carrying out water bath at 65 ℃ for 40min, cooling to 55 ℃, adding papain of 0.2% of the weight of the degreased material, and carrying out water bath for 30 min; continuously stirring, heating to 95 deg.C after hydrolysis, inactivating enzyme for 5min, cooling to room temperature, filtering, and collecting residue to obtain dietary fiber raw material; storing the filtrate for later use;
(3) shearing modification: adding 3.2% by mass of oxalic acid solution into the dietary fiber raw material prepared in the step (2), wherein the ratio of the added oxalic acid solution to the dietary fiber raw material is 1:34 (m/v), uniformly mixing, shearing, dispersing and mixing by using a high-speed shearing instrument, wherein the shearing speed is 8000r/min, and the shearing time is 15min to obtain a modified material;
(4) acid bath: transferring the modified material obtained in the step (3) to a constant-temperature water bath kettle, adding distilled water, leaching for 2 hours at 88 ℃, filtering after leaching is finished, and collecting filtrate;
(5) alcohol precipitation, concentration and drying: combining the filtrates obtained in the steps (2) and (4), and concentrating under vacuum to 1/9 of the original volume to obtain a concentrated solution; slowly adding ethanol with the volume 4 times that of the concentrated solution into the concentrated solution, wherein the volume concentration of the ethanol is 95%; mixing, standing at 4 deg.C for 6 hr, centrifuging at 5000r/min for 10min, collecting precipitate, washing with 95% ethanol for 2 times, freeze drying at-50 deg.C under 10Pa for 30 hr, and grinding into fine powder to obtain soluble dietary fiber.
Example 4
A method for extracting soluble dietary fiber from pineapple peel residues comprises the following steps:
(1) degreasing: screening pineapple peel residues discarded in fruit juice processing production, cleaning, blanching with hot water at 100 ℃ for 1min, and drying with hot air at 60 ℃ for 36 h; crushing, sieving with a 100-mesh sieve, adding petroleum ether according to a material-to-liquid ratio of 1:4 (m/v), stirring and soaking at room temperature for 3 hours, performing suction filtration, and air-drying to obtain a degreased material;
(2) double-enzyme hydrolysis: adding 45 times of distilled water by weight into the degreased material prepared in the step (1), adjusting the pH value of the material liquid to 6.5, adding alpha-amylase accounting for 5% of the weight of the degreased material, carrying out water bath at 65 ℃ for 40min, cooling to 55 ℃, adding papain accounting for 0.6% of the weight of the degreased material, and carrying out water bath for 30 min; continuously stirring, heating to 95 deg.C after hydrolysis, inactivating enzyme for 5min, cooling to room temperature, filtering, and collecting residue to obtain dietary fiber raw material; storing the filtrate for later use;
(3) shearing modification: adding 3.2% by mass of oxalic acid solution into the dietary fiber raw material prepared in the step (2), wherein the ratio of the added oxalic acid solution to the dietary fiber raw material is 1:40 (m/v), uniformly mixing, shearing, dispersing and mixing by using a high-speed shearing instrument, wherein the shearing speed is 9000r/min, and the shearing time is 20min to obtain a modified material;
(4) acid bath: transferring the modified material obtained in the step (3) to a constant-temperature water bath, leaching for 2h at 88 ℃, filtering after leaching is finished, and collecting filtrate;
(5) alcohol precipitation, concentration and drying: combining the filtrates obtained in the steps (2) and (4), and concentrating under vacuum to 1/8 of the original volume to obtain a concentrated solution; slowly adding ethanol with volume of 4 times of that of the concentrated solution into the concentrated solution, wherein the volume concentration of the ethanol is 95%, uniformly mixing, standing at 4 ℃ for 7h, centrifuging at 6000r/min for 8min, collecting precipitate, washing with ethanol with volume concentration of 95% for 2 times, freeze-drying the precipitate at-60 ℃ under the pressure of 9Pa for 36h, and grinding into fine powder to obtain the soluble dietary fiber.
In the above embodiment, the pH of the feed liquid is adjusted, and a suitable pH adjusting agent, such as a NaOH solution with a certain concentration, can be selected according to the use of the prepared dietary fiber. For the convenience of operation, a 9% NaOH solution is selected in this application.
Furthermore, the method also comprises the steps of carrying out acid bath extraction on the soluble dietary fiber of the pineapple peel residues based on the optimal extraction conditions and the optimal factor level, and verifying the model prediction result by using the obtained yield. The optimal extraction conditions and the optimal factor level of the acid bath extraction are mainly obtained by single factor tests and a response surface analysis method, and the response surface Design is realized by Design-Expert 8.0.6 software.
In the research and development process of the technical scheme, the acid species of the action of extracting the soluble dietary fiber of the pineapple peel residue in the acid bath are screened, the acid bath process conditions are optimized, and the optimal technical scheme is obtained as follows: oxalic acid with the mass fraction of 3.2 percent is taken as an extracting agent, the mixture liquid ratio of 1:34g/mL is extracted at 88 ℃ for 2 hours, and the yield of the soluble dietary fiber of the pineapple peel residue under the condition is 19.22 +/-0.08 percent. The concrete description is as follows.
Influence of acid species on yield of soluble dietary fiber of pineapple peel residue
Taking 11 parts of degreased pineapple peel powder, 2g of degreased pineapple peel powder, respectively placing the degreased pineapple peel powder in a 100mL triangular flask, adding distilled water according to the material-liquid ratio of 1:30g/mL, adjusting the pH of the material liquid to 6.5, simultaneously adding 3% of alpha-amylase into each sample, carrying out water bath at 65 ℃ for 40min, cooling to 55 ℃, adding 0.2% of papain, and carrying out water bath for 30 min; inactivating enzyme at 95 deg.C for 5min after hydrolysis, cooling, filtering, and collecting filtrate 1 and residue 1. Respectively adding 30 times of acid extraction agent (mass fraction of 3%) into residue 1, mixing, shearing at 9000r/min for 20min, transferring into constant temperature water bath, leaching at 80 deg.C for 1.5h, filtering, and collecting filtrate 2. And (3) concentrating and precipitating the filtrate 1 and the filtrate 2 respectively, drying, mixing, weighing and calculating the yield of the soluble dietary fiber.
The results show that when oxalic acid is used as the extracting agent, the yield of the soluble dietary fiber in the pineapple peel residue reaches the highest value, namely 15.20 +/-0.13%, so that the oxalic acid is used as the extracting solvent in the test (figure 1).
Determination of technological parameters of soluble dietary fiber extracted from pineapple peel residue by oxalic acid
(1) The influence of different extraction conditions on the yield of the soluble dietary fiber of the pineapple peel residue is as follows: the single-factor experiment sets factors of oxalic acid concentration, extraction time, extraction temperature and feed-liquid ratio, and respectively inspects the influence of 4 factors on the yield of the soluble dietary fiber of the pineapple peel residue. The fixed extraction time is 1.5h, the extraction temperature is 80 ℃, the material-liquid ratio is 1:30g/mL, and the oxalic acid concentration is 1, 2, 3, 4 and 5 percent respectively; the feed liquid ratio is fixed to be 1:30g/mL, the concentration of oxalic acid is 3 percent, the extraction temperature is 80 ℃, and the extraction time is respectively 0.5, 1.0, 1.5, 2.0, 2.5 and 3.0 h; the ratio of the fixed feed to the liquid is 1:30g/mL, the concentration of oxalic acid is 3%, the extraction time is 2h, and the extraction temperatures are respectively 50, 60, 70, 80, 90 and 100 ℃; fixing the concentration of oxalic acid to be 3%, extracting for 2h, and extracting at 90 ℃ with the material-liquid ratio of 1:10, 1:20, 1:30, 1:40 and 1:50g/mL respectively.
The result shows that the SDF yield is increased along with the increase of the concentration of the acid in the range of 1-3% of the concentration of the oxalic acid, and the maximum SDF yield is reached when the concentration is 3%. This is probably because the higher the concentration of acid, the greater the degree of cell dissociation and the greater the elution of SDF from the cells. However, when the concentration is higher than 3%, the SDF yield tends to decrease slowly, which may be caused by degradation of SDF dissolved in cells due to an excessively high acid environment, thereby decreasing the SDF yield. In general, the concentration of oxalic acid is preferably 3% (FIG. 2).
The SDF yield is gradually increased along with the extension of the extraction time, the SDF yield reaches the maximum when the extraction time is 2 hours, and the extraction time is continuously prolonged, so that the SDF yield is gradually reduced. The extraction time is too short, and the SDF is not completely dissolved out; the extraction time is too long, the SDF is likely to be degraded in a high-temperature environment, other impurities are likely to be dissolved out to influence the yield of the SDF, and the extraction time is preferably selected to be 2h in comprehensive consideration (figure 3).
The SDF yield increases and then decreases with the increase of the extraction temperature, and reaches the maximum value when the extraction temperature is 90 ℃. This is probably due to the fact that the increase in temperature accelerates the thermal movement of the molecules, increasing the rate of solvent exchange, which in turn leads to more dissolution of SDF in the cells. However, the temperature is too high, the viscosity of the solution becomes high, the molecular motion speed is slowed down, and the dissolution of fiber substances is prevented, so that the SDF yield is reduced (FIG. 4).
There is also a significant effect on the feed liquor ratio on SDF yield. When the ratio of the material to the liquid is 1: 10-1: 20g/mL, the SDF yield is increased along with the increase of the ratio of the material to the liquid, and when the ratio of the material to the liquid is 1:30g/mL, the SDF yield reaches the maximum. Thereafter, the feed-to-liquid ratio continued to be increased, and the increase in SDF yield was insignificant. When the feed-liquid ratio is increased, the concentration difference between the external solution and the cell liquid is increased, the osmosis is accelerated, and more SDF is dissolved out of the cells. When the feed-liquid ratio is increased to a certain value, the intracellular and extracellular liquid concentrations reach a balance, and the SDF does not seep out along with cytosol, so that the SDF yield tends to be constant. In addition, the excessive ratio of the feed to the liquid increases the difficulty of the subsequent concentration process and the energy consumption is large, so the ratio of the feed to the liquid is preferably fixed to be 1:30g/mL (figure 5).
(2) Optimizing extraction conditions: on the basis of a single-factor test, the oxalic acid concentration, the extraction time, the extraction temperature and the material-liquid ratio are used as independent variables, the yield of the soluble dietary fiber of the pineapple peel residue is used as a response value, a response surface optimization test with 4-factor 3 level is carried out according to a method designed by a Box-Behnken test, so as to determine the optimal extraction process, and the factor level is shown in Table 1.
TABLE 1 factor level table
TABLE 2 Box-Benhnken design test times table
TABLE 3 analysis of variance of regression equation
Note: indicates significant difference height (p<0.01); indicates significant difference (p<0.05）；
Performing quadratic regression analysis on the data of the table 2 by using Design-Expert 8.0.6 software to obtain a quadratic polynomial regression equation:
Y=-197.63+21.66A+11.12B+3.25C+1.68D+0.90AB-0.10AC-0.07AD-9.00BC+ 0.07BD+1.25CD-1.96A2-3.81B2-0.02C2-0.03D2(ii) a In the formula: y represents the yield of the soluble dietary fiber of the pineapple peel residue; a represents oxalic acid concentration, B represents extraction time, C represents extraction temperature, and D represents feed-liquid ratio. The model of the binary regression equation was subjected to significance testing and analysis of variance, with the results shown in table 3. As can be seen from Table 3, the regression model reached a very significant value: (p<0.01), statistically significant. Correction decision coefficient of modelR 2 =0.9126, which shows that the model fitting degree is good, and the SDF yield can be accurately and reliably predicted and analyzed. First order D, second order A of the equation2、C2And D2Has very obvious influence on the SDF yield, a primary term A, C and a secondary term B2Has obvious influence on the SDF yield, and the interactive items AB, AC, AD, BC, BD and CD have no influence on the SDF yieldSignificant impact (fig. 6). The primary and secondary order of the influence of 4 factors on the SDF yield is D>A>C>B, i.e. ratio of feed to liquid>Oxalic acid concentration>Temperature of extraction>And (4) extracting time. Through software analysis, the optimal extraction conditions of the pineapple peel residue SDF are as follows: the concentration of oxalic acid is 3.2 percent, the extraction time is 2 hours, the extraction temperature is 88 ℃, the feed-liquid ratio is 1:34g/mL, and under the condition, the yield of SDF is predicted to be 19.41 percent. To confirm the accuracy and practicality of this equation, a validation experiment was performed. The result of the verification test shows that under the optimal extraction condition, the yield of the SDF of the pineapple peel residue is 19.22 +/-0.05%. The equation is well fitted with the actual situation, and the response surface method is suitable for regression analysis and parameter optimization of the SDF extraction process of the pineapple peel residues.
Comparison of extraction rates of soluble dietary fibers of pineapples by different extraction methods
Taking 7 parts of degreased pineapple peel residue dry powder, each 2g, respectively placing the degreased pineapple peel residue dry powder into a triangular flask with the volume of 100mL, hydrolyzing by alpha-amylase to remove starch, performing enzymolysis by papain to remove protein, and then extracting the pineapple peel residue SDF according to the following 7 methods, wherein the extraction conditions of each method are as follows:
(1) water extraction: leaching at 55 ℃ for 1h, wherein the material-liquid ratio is 1:40 g/mL;
(2) the cellulase method comprises the following steps: 5% of cellulase, 60min of enzymolysis time, 50 ℃ of enzymolysis temperature, 5.5 pHs and 1:40g/mL of feed liquid ratio; inactivating enzyme at 95 deg.C for 5min after hydrolysis;
(3) ultrasonic-cellulase method: the adding amount of cellulase is 5.1 percent, the ultrasonic power is 180W, the ultrasonic time is 40min, the ultrasonic temperature is 45 ℃, and the feed-liquid ratio is 1:42 g/mL; inactivating enzyme at 95 deg.C for 5 min;
(4) shear-cellulase method: the shearing speed is 9000rpm, the shearing time is 20min, the material-liquid ratio is 1:45g/mL, the addition amount of cellulase is 5%, the enzymolysis temperature is 50 ℃, the enzymolysis time is 2h, and the pH is 4.5; inactivating enzyme at 95 deg.C for 5min after hydrolysis;
(5) cellulase-chemical method: the feed liquid ratio is 1:50g/mL, the feed liquid pH is 4.0, the cellulase addition amount is 6%, the hydrolysis temperature is 60 ℃, the hydrolysis time is 60min, and after the hydrolysis is finished, the enzyme is inactivated at 95 ℃ for 5 min; filtering, and carrying out alkaline hydrolysis on filter residues at the temperature of 60 ℃ for 1.5h, wherein the pH value of alkaline hydrolysis is 11.0;
(6) an oxalic acid method: the method is carried out according to the optimized extraction process of the invention, namely, the mass concentration of the oxalic acid solution is 3.2%, the extraction time is 2h, the extraction temperature is 88 ℃, and the material-liquid ratio is 1:34 g/mL;
(7) a hydrochloric acid method: the concentration of hydrochloric acid is 3 percent, the extraction temperature is 79 ℃, the extraction time is 1h, and the material-liquid ratio is 1:42 g/mL.
The results of respectively counting the extraction rates of the SDF obtained by the extraction method show that compared with a hot water method, a hydrochloric acid method, an enzymatic method, an ultrasonic-assisted enzymatic method, an enzyme-chemical method and a shearing-enzymatic method, the method provided by the invention has the maximum yield of the SDF obtained by the pineapple peel residue, which is obviously higher than that obtained by other methods, and is respectively 62.38%, 58.12%, 57.75%, 54.42%, 7.49 and 36.58% higher than that obtained by a water extraction method, an enzymatic method, an ultrasonic-enzymatic method, a shearing-enzymatic method, an enzyme-chemical method and a hydrochloric acid method (figure 7).
Claims (2)
1. The extraction method of the soluble dietary fiber of the pineapple peel residue is characterized by comprising the following steps:
(1) degreasing: screening pineapple peel residues discarded in fruit juice processing production, cleaning, blanching with hot water, drying, crushing, and degreasing to obtain a degreased material;
(2) double-enzyme hydrolysis: respectively adding alpha-amylase and papain into the degreased material prepared in the step (1) for hydrolysis reaction, inactivating enzyme after hydrolysis, cooling to room temperature, filtering, and collecting filter residue to obtain dietary fiber raw material; storing the filtrate for later use;
(3) shearing modification: adding an oxalic acid solution into the dietary fiber raw material prepared in the step (2), uniformly mixing, shearing, dispersing and mixing to obtain a modified material;
(4) acid bath: heating and leaching the modified material obtained in the step (3), filtering after leaching is finished, and collecting filtrate;
(5) alcohol precipitation, concentration and drying: combining the filtrates obtained in the steps (2) and (4), and concentrating to 1/8-1/10 of the original volume to obtain a concentrated solution; slowly adding ethanol with the volume concentration of 95% to 3-6 times of the concentrated solution into the concentrated solution, uniformly mixing, standing for 3-8 h at 4 ℃, centrifuging, collecting precipitate, washing for 1-2 times by using ethanol with the volume concentration of 95%, finally drying the precipitate, and grinding into fine powder to obtain the soluble dietary fiber;
the hot water blanching temperature in the step (1) is 85-100 ℃, and the blanching time is 1-3 min; the drying method of the pineapple peel residues comprises the following steps: drying with hot air at 45-60 ℃ for 36-48 h; crushing and sieving with a 40-100 mesh sieve; the degreasing operation is as follows: according to the material-liquid ratio of 1: adding petroleum ether into the crushed material in a ratio of 3-6 (m/v), stirring and soaking at room temperature for 1-4 h, performing suction filtration, and air-drying to obtain a degreased material;
the hydrolysis reaction in the step (2) comprises the following steps: adding distilled water into the degreased material according to a material-liquid ratio of 1:30 (m/m), adjusting the pH value of the material liquid to 6.5, adding alpha-amylase accounting for 3% of the weight of the degreased material, carrying out water bath at 65 ℃ for 40min, cooling to 55 ℃, adding papain accounting for 0.2% of the weight of the degreased material, and carrying out water bath for 30 min; heating at 95 deg.C to inactivate enzyme for 5min after hydrolysis, cooling to room temperature, filtering, and collecting residue to obtain dietary fiber material;
the mass fraction of the oxalic acid solution in the step (3) is 3.2%, the shearing speed of the high-speed shearing instrument for dispersion is 9000r/min, the shearing time is 20min, and the ratio of the added oxalic acid solution to the dietary fiber raw material is 1:34 (m/v);
the leaching conditions in the step (4) are as follows: the leaching temperature is 88 ℃, and the leaching time is 2 h.
2. The method for extracting the soluble dietary fiber from the pineapple bran as claimed in claim 1, wherein the method comprises the following steps: in the step (5), the filtrate is concentrated under vacuum and reduced pressure; the conditions for the centrifugation were: centrifuging at 4000-7000 r/min for 5-10 min, and freeze-drying the precipitate under the specific conditions: the temperature is-40 to-60 ℃, the pressure is 6 to 15Pa, and the drying time is 24 to 36 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811461811.6A CN109602028B (en) | 2018-12-02 | 2018-12-02 | Extraction method of soluble dietary fiber from pineapple peel residues |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811461811.6A CN109602028B (en) | 2018-12-02 | 2018-12-02 | Extraction method of soluble dietary fiber from pineapple peel residues |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109602028A CN109602028A (en) | 2019-04-12 |
| CN109602028B true CN109602028B (en) | 2021-10-08 |
Family
ID=66005791
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811461811.6A Active CN109602028B (en) | 2018-12-02 | 2018-12-02 | Extraction method of soluble dietary fiber from pineapple peel residues |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109602028B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110839874A (en) * | 2019-11-19 | 2020-02-28 | 广东工业大学 | Water-soluble dietary fiber and application |
| CN111227262A (en) * | 2020-02-11 | 2020-06-05 | 临沂大学 | Preparation method of green radish dietary fiber rich in oxidized and reduced glucoraphanin |
| CN115606813A (en) * | 2022-10-13 | 2023-01-17 | 中国林业科学研究院林产化学工业研究所 | Myrtle dietary fiber with anti-saccharification activity and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20120036685A (en) * | 2010-10-08 | 2012-04-18 | 영농조합법인 속리바이오텍 | Extract method of dietary fiber of dried radish leaf and extracted dietary fiber by this method |
| CN103976371A (en) * | 2014-06-03 | 2014-08-13 | 中国农业大学 | Method for extracting ponkan dietary fibers through extrusion modification and enzymolysis coupling |
| CN104222889A (en) * | 2014-09-10 | 2014-12-24 | 中国科学院过程工程研究所 | Wolfberry soluble dietary fiber and preparation method thereof |
| CN105433394A (en) * | 2015-12-04 | 2016-03-30 | 重庆三零三科技有限公司 | Preparation method of pineapple residue soluble dietary fiber |
| CN105661559A (en) * | 2016-01-20 | 2016-06-15 | 山东禹王生态食业有限公司 | Method using ultrasonic-assisted enzyme method to extract water-soluble dietary fibers in pre-acidified soybean dregs |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2008331430A1 (en) * | 2007-12-05 | 2009-06-11 | Nutrifina Pty Ltd | Dietary fiber and method for preparing dietary fiber |
-
2018
- 2018-12-02 CN CN201811461811.6A patent/CN109602028B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20120036685A (en) * | 2010-10-08 | 2012-04-18 | 영농조합법인 속리바이오텍 | Extract method of dietary fiber of dried radish leaf and extracted dietary fiber by this method |
| CN103976371A (en) * | 2014-06-03 | 2014-08-13 | 中国农业大学 | Method for extracting ponkan dietary fibers through extrusion modification and enzymolysis coupling |
| CN104222889A (en) * | 2014-09-10 | 2014-12-24 | 中国科学院过程工程研究所 | Wolfberry soluble dietary fiber and preparation method thereof |
| CN105433394A (en) * | 2015-12-04 | 2016-03-30 | 重庆三零三科技有限公司 | Preparation method of pineapple residue soluble dietary fiber |
| CN105661559A (en) * | 2016-01-20 | 2016-06-15 | 山东禹王生态食业有限公司 | Method using ultrasonic-assisted enzyme method to extract water-soluble dietary fibers in pre-acidified soybean dregs |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109602028A (en) | 2019-04-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109602028B (en) | Extraction method of soluble dietary fiber from pineapple peel residues | |
| CN107177007B (en) | A kind of preparation method of Auricularia polysaccharide | |
| CN102302083B (en) | Method for extracting tea protein product | |
| CN102321189B (en) | Comprehensive extraction process for auricularia auricula polysaccharide | |
| CN106146687B (en) | A kind of method of pectin in extraction citrus peel residue | |
| CN103478400B (en) | High-purity rice bran protein and rice bran fibers and preparation method thereof | |
| CN106072672A (en) | A kind of production technology activating wheat-bran dietary fiber | |
| CN102885318A (en) | Method for extracting sweet potato dietary fibers | |
| CN107495394A (en) | A kind of steam blasting is modified the method with enzymolysis coupling extraction dietary fibers from peanuts | |
| CN102224907A (en) | Method for extracting dietary fibers from bean pods | |
| CN108003251A (en) | A kind of extracting method of pineapple bran polysaccharide | |
| CN105399855A (en) | Method for preparing oat beta-glucan through ball milling | |
| CN101560264A (en) | Process combination for extracting polysaccharide in golden mushroom mycelium cells and determination method thereof | |
| CN101695364B (en) | Method for preparing dietary fiber by apricot residue | |
| CN102640905B (en) | Method for extracting water-insoluble dietary fiber of osmunda cinnamomea | |
| CN109288072A (en) | A kind of preparation method of mandarin orange pomace nano-dietary fiber | |
| CN112778438A (en) | Method for improving pachyman extraction rate by steam explosion and enzymolysis technology | |
| CN101690525A (en) | Method for extracting myrica seed oil | |
| CN107090478B (en) | Method for extracting water-soluble dietary fiber from lentinus edodes stems | |
| CN111184224A (en) | Preparation method and application of high-activity dietary fiber powder | |
| CN110537690A (en) | Preparation method of Chinese yam mud and product thereof | |
| CN113331430A (en) | Method for preparing soluble dietary fiber from citrus fruit peel residues | |
| CN110283860B (en) | Gracilaria tenuistipitata polysaccharide extracted by ultrasonic-assisted composite enzymolysis and extraction method thereof | |
| CN101797036A (en) | Preparation method of canna edulis ker soluble dietary fiber | |
| CN106434789A (en) | Method for extracting soluble dietary fiber in coffee peel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |