CN115073621B - Preparation method of arabinoxylan - Google Patents
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- CN115073621B CN115073621B CN202210650819.7A CN202210650819A CN115073621B CN 115073621 B CN115073621 B CN 115073621B CN 202210650819 A CN202210650819 A CN 202210650819A CN 115073621 B CN115073621 B CN 115073621B
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- C08B37/0057—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Xylans, i.e. xylosaccharide, e.g. arabinoxylan, arabinofuronan, pentosans; (beta-1,3)(beta-1,4)-D-Xylans, e.g. rhodymenans; Hemicellulose; Derivatives thereof
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Abstract
The invention discloses a preparation method of araboxylan, which utilizes ionic liquid to extract araboxylan from vinegar residue so as to realize comprehensive utilization of vinegar residue resources. The method takes vinegar residue as a raw material, and the arabinoxylan is obtained by crushing, sieving, degreasing and deproteinizing, treating with ionic liquid, concentrating and filtering, and freeze-drying in vacuum. The method can effectively extract the arabinoxylan from the vinegar residue, and the obtained arabinoxylan can be used for physicochemical property analysis, structural analysis, biological activity research and the like. The invention adopts the ionic liquid method to extract the arabinoxylan in the vinegar residue, thereby greatly improving the yield of the arabinoxylan, the yield of the polysaccharide is 30.2 percent, the extraction rate reaches more than 94 percent, and the extraction is obviously higher than that of the traditional enzyme method; the vinegar residue polysaccharide is separated by adopting the environment-friendly ionic liquid, so that the problems of low hydrothermal and enzymatic yield and environmental pollution caused by an alkaline method in the prior art are solved.
Description
Technical Field
The invention relates to a preparation method of arabinoxylan, in particular to a method for preparing the arabinoxylan by vinegar residue.
Background
With the rapid development of the vinegar industry, the problem of environmental pollution caused by vinegar residues, which are byproducts generated in the vinegar brewing process, cannot be ignored. The vinegar residue resources in China are rich, and most of the vinegar residues are not scientifically and reasonably utilized at present. Common processing modes of the vinegar residue mainly comprise ensiling, drying, microbial fermentation and the like. The new development form also puts new requirements on the comprehensive utilization of the vinegar residue. The vinegar residue waste is difficult to degrade, certain environmental pollution hidden danger exists, and the treatment of the vinegar residue becomes a problem which needs to be solved urgently in the healthy development of the vinegar brewing industry in China. Actively explores the comprehensive utilization way and the new method of the vinegar residue resource, thoroughly solves the problem of the vinegar residue pollution to the environment, and has important significance for improving the production environment of production enterprises and increasing the economic and social benefits of the enterprises.
The vinegar residue is a byproduct in the vinegar making process, and the vinegar residue has high crude fiber content (mainly comprising cellulose, hemicellulose and lignin), wherein the Arabinoxylan (AX) serving as a main component of the hemicellulose is rich. AX has high viscosity and high water binding property, and can be used as food thickener and stabilizer; the compound also has a plurality of important physiological activities, such as functions of reducing cholesterol, reducing blood sugar, resisting oxidation, regulating immunity and the like, and has high application value and wide application prospect. They can be classified into water-soluble arabinoxylans and water-insoluble arabinoxylans according to their solubility. The distribution, content and even structure of the corn are different according to different planting conditions and species differences of the corn.
At present, the research on AX mainly focuses on cereal crops such as corn, wheat and barley, and the extraction method mainly comprises the following steps: hydrothermal extraction, enzymatic extraction and alkaline extraction. The water has the advantages of no toxicity, no harm, low cost, easy obtaining, no need of recovery and the like, so the water is an ideal extracting agent. However, water is used as an extracting agent, so that the water solvent cannot break the crosslinking action of AX and other substances in cell walls under certain conditions, and the extraction rate of AX is low; the enzyme extraction technology is mild in condition, can recover effective components to the maximum extent, is green and pollution-free, represents the development direction of AX, but the enzyme extraction rate is generally lower; at present, the industrial preparation of AX mainly adopts an alkali extraction technology, but has the problems of great environmental pollution and easy damage to active groups such as ferulic acid in a molecular structure. Relatively few researches on araboxylan in the vinegar residue are conducted at home and abroad, so that the development of an environment-friendly vinegar residue araboxylan extraction method is of great significance.
Disclosure of Invention
The invention aims to: the invention aims to provide a preparation method of the arabinoxylan, which has high extraction rate, simple method and environmental protection.
The technical scheme is as follows: the preparation method of the arabinoxylan uses the vinegar residue as a raw material, and the arabinoxylan is extracted from the vinegar residue by using the ionic liquid.
Preferably, the ionic liquid is 1-butyl-3-methylimidazole chloride salt.
The method for extracting the arabinoxylan from the vinegar residue by using the ionic liquid comprises the following steps of:
(1) Pretreating a vinegar residue sample to obtain a dry vinegar residue powder sample;
(2) Removing starch in the vinegar residue powder sample to obtain the de-starch vinegar residue;
(3) Removing protein in the de-starch and de-protein vinegar residue to obtain de-starch and de-protein vinegar residue;
(4) Preparing vinegar residue holocellulose by using the de-starch and de-protein vinegar residue;
(5) Adding ionic liquid into the vinegar residue holocellulose, stirring and reacting in a water bath, standing, removing precipitates, and recovering a filtrate; concentrating the filtrate, adding tetrahydrofuran, standing, collecting precipitate, and repeatedly cleaning the precipitate with anhydrous ethanol and distilled water for several times to obtain arabinoxylan.
Further comprises a step (6) of freeze-drying the arabinoxylan obtained in the step (5) in vacuum to obtain solid powder of the arabinoxylan.
Further, in the step (1), the vinegar residue sample pretreatment method comprises the steps of drying the vinegar residue, grinding, crushing and sieving for later use. Specifically, the drying temperature of the vinegar residue is 105 ℃.
Further, in the step (2), the method for removing starch in the vinegar residue powder sample is to sequentially add water and high-temperature resistant alpha-amylase to the vinegar residue powder sample to carry out enzymolysis to remove starch. Wherein the ratio of the vinegar residue powder sample to the water is 50g:400-500mL, the ratio of the addition amount of the high-temperature resistant alpha-amylase to the water amount is 4mL: 400-500mL; the enzymolysis condition is 60-80 deg.C water bath for 1-2h.
Further, in the step (3), the method for removing the protein in the de-starch vinegar residue is to adjust the pH of the de-starch vinegar residue solution, add neutral protease, continue to adjust the pH after the reaction is finished, add saccharifying enzyme, and collect the precipitate after the reaction is finished, namely the de-starch and de-protein vinegar residue.
Specifically, firstly, adjusting the pH value to 7.5, wherein the addition amount of neutral protease is 25g, the vinegar residue powder sample corresponds to 1g of neutral protease, and the enzymolysis condition of the neutral protease is 60-80 ℃ water bath for 1-2h; then continuously adjusting the pH value to 4.5, adding the same amount of saccharifying enzyme as that of neutral protease, and carrying out water bath on the saccharifying enzyme for 1-2h at the temperature of 60-80 ℃; and finally, centrifuging at 4000r/min, collecting precipitate to obtain the de-starch and de-protein vinegar residue, and drying for later use.
Further, in the step (4), adding a sodium chlorite solution into the de-starch and de-protein vinegar residue, adjusting the pH value, reacting for a period of time, collecting the filtered solid matter, and drying to obtain the vinegar residue holocellulose. Wherein, the pH value is adjusted to 4.2-4.7, and the mixture is bathed in water at the temperature of 60-80 ℃ for 1-2h; after the reaction, the mixture is immediately cooled, and after filtration, the solid matter is dried at 50 ℃ overnight. This sample was vinegar residue holocellulose.
Furthermore, the addition amount of the sodium chlorite solution is 200-300mL of 0.6-0.8% sodium chlorite solution per 1g of the starch-removed and protein-removed vinegar residue.
Further, in the step (5), 30-50g of ionic liquid is added into each 3g of vinegar residue holocellulose. Specifically, 30-50g of ionic liquid is added into every 3g of vinegar residue holocellulose, and the mixture is stirred and reacted for 24-36h in water bath at the temperature of 70-90 ℃; adding 300-500mL of distilled water after the reaction is finished to terminate the reaction, standing, removing the precipitate, and recovering the filtrate; concentrating the filtrate, adding tetrahydrofuran, standing for 12-24 hr, collecting precipitate, and repeatedly cleaning the precipitate with anhydrous ethanol and distilled water for 3 times to obtain arabinoxylan. The supernatant is ionic liquid, and is recovered for continuous use.
The molecular weight analysis method of the arabinoxylan prepared by the method comprises the following steps:
analyzing the molecular weight of the arabinoxylan obtained in step (6) by high performance liquid chromatography equipped with a differential detector; the model of the differential detector is Waters 2414, and the model of the sugar column is PL aquqgel-OH MIXED-H8 μm; the column temperature is 30-50 ℃; the mobile phase is 0.2M NaNO3 and 0.01M NaH2PO4, and the flow rate is 0.8-1.2mL/min.
The monosaccharide composition analysis method prepared by the method comprises the following steps: the monosaccharide composition of the arabinoxylan obtained in step (6) was analyzed by high performance ion exchange chromatography equipped with a pulsed amperometric detector. The type of the chromatographic column is Dionex TM CarboPac TM PA10 (250 x 4.0mm,10 μm); the column temperature is 30-50 ℃; mobile phase a (H2O), mobile phase B (100 mM NaOH), flow rate 0.3-1.0mL/min.
The invention relates to a method for extracting araboxylan from vinegar residue, which realizes the comprehensive utilization of vinegar residue resources. The method takes vinegar residue as a raw material, and the arabinoxylan is obtained by crushing, sieving, degreasing and deproteinizing, treating with ionic liquid, concentrating and filtering, and freeze-drying in vacuum. The method can effectively extract the arabinoxylan from the vinegar residue, and the obtained arabinoxylan can be used for physicochemical property analysis, structural analysis, biological activity research and the like.
The ionic liquid has unique physicochemical properties such as low vapor pressure, high thermal stability, various dissolved substances and the like, is environment-friendly, can be recycled and the like, so that the ionic liquid is widely concerned about the separation and purification of organic compounds and has development potential, and many researchers are dedicated to exploring an extraction method which not only meets the environmental requirements but also can reduce the cost on the basis of ensuring the pretreatment effect. [ Bmim ] Cl (1-butyl-3-methylimidazole chloride) is the ionic liquid with the strongest cellulose dissolving capacity, and the electron donor and acceptor theory can well explain the dissolving principle. The invention utilizes ionic liquid [ Bmim ] Cl (1-butyl-3-methylimidazole chloride) to extract arabinoxylan in vinegar residue. Simplifies the complicated operation process of the traditional alkali extraction method and reduces the environmental pollution, the used ionic liquid is convenient to recover, saves energy, protects the environment and is more friendly to the environment, thus being a green conversion technical route.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: (1) The extraction method of the arabinoxylan in the vinegar residue by the ionic liquid method improves the yield of the arabinoxylan to a great extent, the yield of the polysaccharide is 30.2 percent, the extraction rate reaches more than 94 percent, and the extraction is obviously higher than that of the traditional enzyme method;
(2) The vinegar residue polysaccharide is separated by adopting the environment-friendly ionic liquid, so that the problems of low yield of the conventional hydrothermal and enzymatic methods and environmental pollution caused by an alkaline method are solved;
(3) The preparation method is simple and feasible, can improve the utilization rate of the vinegar residue, improve the added value of food processing byproducts, increase economic benefits, and obtain the polysaccharide with higher purity, thereby having good application value and market potential.
Drawings
FIG. 1 is a flow chart of the extraction process of arabinoxylan according to the present invention;
FIG. 2 shows the measurement results of arabinoxylan by HPLC;
FIG. 3 is a standard sample ion chromatogram.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings.
As shown in figure 1, the invention provides a preparation method of arabinoxylan, which takes vinegar residue as a raw material and utilizes ionic liquid to extract the arabinoxylan from the vinegar residue. Preferably, the ionic liquid is [ Bmim ] Cl (1-butyl-3-methylimidazolium chloride).
The method for extracting the arabinoxylan from the vinegar residue by using the ionic liquid comprises the following steps:
(1) Pretreating a vinegar residue sample: drying vinegar residue at 105 deg.C, grinding, pulverizing, and sieving;
(2) Starch removal: the ratio of the vinegar residue powder sample to the amount of distilled water is 50g:400-500mL, add high temperature resistant alpha-amylase, carry on the enzymolysis, specifically: 4mL of high-temperature resistant alpha-amylase, and 1-2h of water bath at 60-80 ℃;
(3) Deproteinization: adjusting the pH value to 7.5 in the step (2), adding 2g of neutral protease, and carrying out water bath at 60-80 ℃ for 1-2h; adjusting pH to 4.5, adding 2g diastase, and water bath at 60-80 deg.C for 1-2 hr; centrifuging at 4000r/min, collecting precipitate to obtain the de-starch and de-protein vinegar residue, and drying for later use;
(4) Preparing vinegar residue holocellulose: taking 2g of the de-starched and deproteinized vinegar residue obtained in the step (3), adding 400-600mL of 0.6-0.8% sodium chlorite solution, adjusting the pH value to 4.2-4.7, and carrying out water bath at 60-80 ℃ for 1-2h; after the reaction, the mixture is immediately cooled, and after filtration, the solid matter is dried at 50 ℃ overnight. The sample is vinegar residue holocellulose;
(5) Extracting the arabinoxylan: adding 3g of the vinegar residue holocellulose obtained in the step (4) into 30-50g of ionic liquid, and stirring and reacting for 24-36h at 70-90 ℃ in a water bath; adding 300-500mL of distilled water after the reaction is finished to terminate the reaction, standing, removing the precipitate, and recovering the filtrate; concentrating the filtrate, adding tetrahydrofuran, standing for 12-24 hr, collecting precipitate, and repeatedly cleaning the precipitate with anhydrous ethanol and distilled water for 3 times to obtain arabinoxylan. The supernatant is ionic liquid and is recycled for continuous use;
(6) Vacuum freeze drying: and (5) carrying out vacuum freeze drying on the arabinoxylan obtained in the step (5) to obtain solid powder.
Example 1 preparation of arabinoxylans
The embodiment provides a preparation method of arabinoxylan, which comprises the following steps:
(1) Drying vinegar residue, grinding, pulverizing, and sieving.
(2) Placing 50g into an autoclave, inactivating endogenous enzyme activity at 121 deg.C for 15min, transferring into a 1L triangular flask, adding 500mL distilled water, water bathing at 60 deg.C for 2h, adding 4mL high temperature alpha-amylase, and stirring.
(3) Then adjusting the pH value to 7.5 by using 0.275mol/L NaOH solution, adding 2g of neutral protease into water bath at 60 ℃ for 1h to reduce the protein content in the vinegar residue. The pH was adjusted to 4.5 with 0.325mol/L HCl. Adding 2g of saccharifying enzyme, carrying out water bath at 60 ℃ for 1h, continuously stirring to remove residual starch in the vinegar residue, centrifuging at 4000r/min for 10min, washing the precipitate with distilled water for 2-3 times, and drying in an oven at 60 ℃ for 24h to obtain the de-starch and de-protein vinegar residue for later use.
(4) Weighing 20g of vinegar residue powder, placing the powder in 1000mL conical flasks in batches, adding 0.6% sodium chlorite solution until the solid-to-liquid ratio is 1 (w/v), adjusting the pH value to 4.2-4.7 by using glacial acetic acid, sealing the conical flasks, and placing the conical flasks in a 75 ℃ water bath kettle; shaking manually every 20min to mix the reactants. Immediately after the reaction is finished, a large amount of cold water is used for washing the outer wall so that the temperature of the reaction system is rapidly reduced. Filtering with nylon cloth, washing the filtrate with distilled water to neutral, and drying the residual solid at 50 deg.C overnight. This sample was vinegar residue holocellulose.
(5) Placing 3g of fully dried vinegar residue holocellulose into a 500mL round-bottom flask, respectively and slowly adding 30g of pretreated ionic liquid [ Amim ] Cl, and fully dissolving vinegar residue powder in the ionic liquid by using a magnetic stirrer; then stirring the mixture in a water bath at the temperature of 80 ℃ for reaction for 24 hours, adding 300mL of distilled water into a reaction system after the reaction is finished to terminate the reaction, precipitating regenerated cellulose, filtering the regenerated cellulose by a Buchner funnel, and concentrating the filtrate by a rotary evaporator to obtain a primary recovered ionic liquid; adding 100mL of Tetrahydrofuran (THF) into the primarily recovered ionic liquid, standing for 12h, and filtering by a Buchner funnel; repeatedly washing the filter residue with anhydrous ethanol and distilled water for 3 times respectively to obtain arabinoxylan.
Further concentrating the residual filtrate, and vacuum drying at 50 deg.C for 48h to ensure water content below 1%, and recovering ionic liquid for reuse.
(6) Vacuum freeze drying: and (5) carrying out vacuum freeze drying on the arabinoxylan obtained in the step (5) to obtain solid powder.
Example 2 measurement of molecular weight of arabinoxylan
In order to further understand the arabinoxylan obtained under the above extraction conditions, the molecular weight distribution of the arabinoxylan in example 1 was measured by high performance gel chromatography (GPC). The chromatographic conditions are as follows: high performance liquid chromatograph Waters 1525, chromatographic column PL aqqgel-OH MIXED-H8 μm; the model of the differential detector is Waters 2414; the mobile phase used was 0.2M NaNO 3 And 0.01M NaH 2 PO 4 (ii) a The flow rate is 1mL/min; the column temperature is 30 ℃; the sample injection amount is 10 mu L; the results are shown in FIG. 2.
The relative molecular mass of arabinoxylan is closely related to its physiological activity and functional properties in food systems. As can be seen from fig. 2, the extracted arabinoxylan has only one main chromatographic peak, indicating that the polysaccharide extracted by this method is a homogeneous polysaccharide.
Analysis of the molecular structural features of the polysaccharides using GPC software can provide table 1. Coefficient of dispersion (
Mw/Mn) reflects the difference in mass of the substances contained in the sample and their structure, the larger the value of the dispersion coefficient, the larger the difference in structure. The dispersion coefficient of the arabinoxylan extracted by the method is 2.446, which shows that the arabinoxylan extracted by the method has better uniformity and more uniform molecular weight distribution.
TABLE 1 arabinoxylan relative molecular weight distribution
Example 3 arabinoxylan monosaccharide composition analysis
Monosaccharide composition analysis was performed on the polysaccharide in example 1. Monosaccharide composition was determined by high performance ion exchange chromatography with a pulsed amperometric detector.
The chromatographic system used was a Thermo ICS5000+ ion chromatographic system (ICS 5000+, (Thermo)
Fisher Scientific, USA) using Dionex TM CarboPac TM PA10 (250X 4.0mm,10 μm) liquid chromatography column, sample size 5 μ L. Mobile phase A (H) 2 O), mobile phase B (100 mM NaOH), column temperature 30 ℃, and monosaccharide components are analyzed and detected by an electrochemical detector. The mobile phase gradients are shown in table 2. The standard sample chromatogram is shown in FIG. 3.
TABLE 2 gradient of mobile phase
5mg of the polysaccharide sample obtained in example 1 was added to the prepared trifluoroacetic acid solution and heated at 121 ℃ for 2 hours. Introducing nitrogen and drying. Adding methanol for cleaning, blowing dry, repeating methanol cleaning for 2-3 times. Adding water to dissolve and fix the volume, and then passing through a 0.45 mu m micropore filter membrane for sample injection analysis. The results are shown in Table 3.
TABLE 3 arabinoxylan monosaccharide composition
The vinegar residue arabinoxylan mainly comprises arabinose, galactose, glucose and xylose. The degree of side chain substitution was 0.58.
Example 4 in vitro hypoglycemic Activity of arabinoxylans
Diabetes is a global epidemic characterized by hyperglycemia, which can lead to serious cardiovascular and nervous system complications. Postprandial glycemic status is an important factor in the induction of diabetes development, with one of the most effective methods of inhibiting postprandial hyperglycemia being to slow down glucose formation by inhibiting the activity of alpha-glucosidase. The polysaccharide of example 1 was analyzed for in vitro hypoglycemic activity. The in vitro inhibition effect of vinegar residue arabinoxylan on alpha-glucosidase is determined by adopting a pNPG method.
mu.L of polysaccharide sample and 40. Mu.L of alpha-glucosidase (0.1 Unit/mL) were incubated for 10min at 37 ℃ in an incubator. Adding 40 mu L of 1mmol/L p-nitrophenyl-alpha-D-glucopyranoside (pNPG) to initiate reaction, precisely reacting for 30min at 37 ℃, and adding 0.2mol/L Na 2 CO 3 The reaction was terminated (100. Mu.L). The absorbance was measured at 405 nm. Both the reagent and the sample were dissolved with 67mM potassium phosphate buffer (pH = 6.8). No sample was added as a blank control and no enzyme was added as a background control.
The binding of the polysaccharide to the enzyme results in changes in the polarity and molecular conformation of the alpha-glucosidase, with partial loss of enzyme activity. The inhibition rate of the vinegar residue arabinoxylan on the alpha-glucosidase can reach 50.13%.
Claims (8)
1. A preparation method of araboxylan is characterized in that vinegar residue is used as a raw material, and ionic liquid is utilized to extract the araboxylan from the vinegar residue; the ionic liquid is 1-butyl-3-methylimidazole chloride; the method for extracting the arabinoxylan from the vinegar residue by using the ionic liquid comprises the following steps:
(1) Pretreating the vinegar residue sample to obtain a dried vinegar residue powder sample;
(2) Removing starch in the vinegar residue powder sample to obtain the de-starch vinegar residue;
(3) Removing protein in the de-starch and de-protein vinegar residue to obtain de-starch and de-protein vinegar residue;
(4) Preparing vinegar residue holocellulose by using the de-starch and de-protein vinegar residue;
(5) Adding ionic liquid into the vinegar residue holocellulose, stirring and reacting in a water bath, standing, removing precipitates, and recovering a filtrate; concentrating the filtrate, adding tetrahydrofuran, standing, collecting precipitate, and repeatedly cleaning the precipitate with anhydrous ethanol and distilled water for several times to obtain arabinoxylan.
2. The method for producing arabinoxylan according to claim 1, further comprising a step (6) of vacuum freeze-drying the arabinoxylan obtained in the step (5) to obtain a solid powder of arabinoxylan.
3. The method for preparing arabinoxylan according to claim 1, wherein the step (1) of pretreating the vinegar residue sample comprises drying the vinegar residue, grinding and pulverizing the vinegar residue, and sieving the vinegar residue for later use.
4. The method for preparing arabinoxylan according to claim 1, wherein the starch in the vinegar residue powder sample is removed in step (2) by sequentially adding water and thermostable α -amylase to the vinegar residue powder sample, and performing enzymatic hydrolysis to remove the starch.
5. The method of claim 1, wherein the step (3) of removing the proteins in the de-starched vinegar residue comprises adjusting the pH of the de-starched vinegar residue solution, adding neutral protease, after the reaction is finished, continuously adjusting the pH, adding saccharifying enzyme, and collecting the precipitate to obtain the de-starched and de-proteinated vinegar residue.
6. The method for preparing arabinoxylan according to claim 1, wherein in the step (4), sodium chlorite solution is added into the de-starched and de-proteinated vinegar residue, pH is adjusted, reaction is carried out for a period of time, and then the filtered solid matter is collected and dried to obtain the vinegar residue holocellulose.
7. The method of claim 6, wherein the amount of the sodium chlorite solution added is about 200 to 300mL per 1g of the deproteinized vinegar residue, wherein the amount of the sodium chlorite solution added is about 0.6 to about 0.8 percent.
8. The method of preparing arabinoxylan according to claim 1, wherein the amount of the ionic liquid added in step (5) is 30 to 50g per 3g of the vinegar residue holocellulose.
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