CN115368486B - Ternary eutectic solvent and application thereof in procambarus clarkia shell chitin extraction - Google Patents
Ternary eutectic solvent and application thereof in procambarus clarkia shell chitin extraction Download PDFInfo
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- 239000002904 solvent Substances 0.000 title claims abstract description 69
- 229920002101 Chitin Polymers 0.000 title claims abstract description 63
- 230000005496 eutectics Effects 0.000 title claims abstract description 57
- 238000000605 extraction Methods 0.000 title claims abstract description 42
- 241000238030 Procambarus clarkii Species 0.000 title claims abstract description 36
- MBLBDJOUHNCFQT-LXGUWJNJSA-N aldehydo-N-acetyl-D-glucosamine Chemical compound CC(=O)N[C@@H](C=O)[C@@H](O)[C@H](O)[C@H](O)CO MBLBDJOUHNCFQT-LXGUWJNJSA-N 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 11
- 241000238557 Decapoda Species 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 54
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 36
- 229910052739 hydrogen Inorganic materials 0.000 claims description 26
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 19
- 235000019743 Choline chloride Nutrition 0.000 claims description 19
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 19
- 229960003178 choline chloride Drugs 0.000 claims description 19
- 239000004310 lactic acid Substances 0.000 claims description 18
- 235000014655 lactic acid Nutrition 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 235000011054 acetic acid Nutrition 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims 1
- 238000012216 screening Methods 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 18
- 230000007935 neutral effect Effects 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000011033 desalting Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000005580 one pot reaction Methods 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract 2
- 238000003760 magnetic stirring Methods 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 description 24
- 238000005303 weighing Methods 0.000 description 14
- 230000000694 effects Effects 0.000 description 11
- 102000004169 proteins and genes Human genes 0.000 description 9
- 108090000623 proteins and genes Proteins 0.000 description 9
- 239000000376 reactant Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 239000000370 acceptor Substances 0.000 description 5
- 238000005115 demineralization Methods 0.000 description 5
- 230000002328 demineralizing effect Effects 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 5
- 239000011707 mineral Substances 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 238000000874 microwave-assisted extraction Methods 0.000 description 4
- 229930014626 natural product Natural products 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
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- 125000000524 functional group Chemical group 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 229920001222 biopolymer Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003544 deproteinization Effects 0.000 description 1
- 150000002016 disaccharides Chemical class 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
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- 230000005588 protonation Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
Abstract
The invention discloses a ternary eutectic solvent and application thereof in procambarus clarkia shell chitin extraction, and specifically comprises the following steps: collecting the shrimp shells processed by procambarus clarkia, drying and crushing the shrimp shells after washing, decontaminating and deproteinizing, adding procambarus clarkia shell powder into the prepared ternary eutectic solvent, heating, carrying out ultrasonic treatment and continuous magnetic stirring reaction for a period of time until the microstructure of the shrimp shell powder is fully dissociated, adding a back extraction solvent into the reaction solution at room temperature, centrifuging until the obtained precipitate is neutral in pH, and drying the precipitate to obtain the chitin. The ternary eutectic solvent is efficiently extracted, the procambarus clarkia shell chitin with higher purity is obtained by a one-pot method through heating and ultrasonic microwave treatment, strong acid is not used for desalting, the production cost can be obviously reduced, chemical reagents in the purification process can be stopped, the environmental pollution is reduced, and the extraction rate of the chitin can be greatly improved.
Description
Technical Field
The invention belongs to the technical field of natural product extraction, and relates to a ternary eutectic solvent for natural product extraction, in particular to a ternary eutectic solvent and application thereof in procambarus clarkia shell chitin extraction.
Background
Procambarus clarkia (L.) KidneyProcambarus clarkii) The growth adaptability is high, the propagation speed is high, the procambarus clarkii is an important economic class in the freshwater shrimp industry, the development of the procambarus clarkii industry is rapid in recent years, the culture yield of procambarus clarkii in China is 239.37 ten thousand tons according to statistics in 2020, and the industry drives the local property development and the social progress. However, at the same time, because the non-edible parts of the procambarus clarkia occupy a relatively high proportion, most of the shell is discarded or utilized with a low value.
The procambarus clarkia shell contains a large amount of chitin, is a natural high molecular compound, is insoluble in water, has various characteristics of no toxicity, biodegradability, biocompatibility, chemical stability, thermal stability and the like, and therefore, the biopolymer is attractive in various industrial and research fields of agriculture, medicine, food, textile and the like. However, the molecular structure is difficult to be dissolved in most solvents, and in practice, the extraction effect is limited because the solvent is only dissolved in a few strong acid solutions.
In recent years, with the deep preparation and deep utilization of procambarus clarkia chitin, the chitin product is more widely utilized in industries such as agriculture, food, biological medicine, chemical industry, cosmetics and the like. For a long time, the industrial extraction of chitin adopts strong acid to remove calcium carbonate and alkali to remove protein. The method has large demand for strong acid and strong alkali, high subsequent wastewater treatment cost, and is easy to generate serious environmental load, thereby being unfavorable for the sustainable development of industry. In recent years, various new green solvents are used in chitin extraction, wherein the Deep-eutect solvent (DES) has a certain application, and the Deep-eutect solvent is a liquid compound which has a melting point lower than that of any component thereof and is always in a liquid state in a room temperature state due to the fact that the melting point is lower than that of any component thereof, and the Deep-eutect solvent has the characteristics of good dissolution performance, abundant component sources, low price and the like, but a solution system formed by combining a conventional Hydrogen bond acceptor and a Hydrogen bond donor in the research of chitin extraction has great difficulty in extraction efficiency, and different Hydrogen bond donors and Hydrogen bond acceptors are influenced by factors such as acid property, compound chain length, functional group property, molar ratio composition, preparation condition and the like when the Deep-eutect solvent is prepared, so that the Deep-eutect solvent has great difference in terms of the properties such as crust, dissolution performance, acid property and the like, therefore, the Deep-eutect solvent is a significant important factor in the current preparation of the Deep-eutect solvent. The eutectic solvent exhibits remarkable advantages in terms of extraction efficiency and extraction effect compared with the common solvent extraction method in the field of natural product extraction, but more importantly than improving the extraction efficiency, the obtained extract can maintain its biological activity and is harmless to human beings, and is a further development direction for developing and utilizing natural products in the fields of foods, biology, catalysis and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a ternary eutectic solvent, which is applied to the extraction of procambarus clarkia shell chitin, fully dissolves shrimp shell powder and the eutectic solvent under the treatment of ultrasound and microwaves, and can remove impurities and calcium in the shrimp shell powder, thereby finally obtaining the chitin with high extraction rate and high purity.
The invention is realized by the following technical scheme:
the ternary eutectic solvent is prepared by mixing choline chloride, lactic acid and acetic acid, wherein the molar ratio of the choline chloride to the lactic acid to the acetic acid is 1:1-1:3:3. Wherein, choline chloride is hydrogen bond acceptor, lactic acid and acetic acid are hydrogen bond donor, and the process of mixing preparation is as follows: heating at a certain temperature, and continuously stirring by magnetic force for a period of time until uniform transparent liquid is generated, thus obtaining the ternary eutectic solvent.
Further, when the choline chloride, the lactic acid and the acetic acid are mixed to prepare the ternary eutectic solvent, the temperature is 90-150 ℃ and the time is 8-24 hours.
The invention further improves the scheme as follows:
the ternary eutectic solvent is applied to the extraction of procambarus clarkia shell chitin.
Further, the application of the ternary eutectic solvent in the extraction of procambarus clarkia shell chitin comprises the following specific steps:
s1: collecting the shrimp shells of procambarus clarkia, ultrasonically cleaning, removing foreign matters, soaking in the solution, heating and stirring for a period of time, then ultrasonically treating, washing with water, drying in a drying oven, crushing by a high-speed crusher, and sieving to obtain shrimp shell powder for later use;
s2: and (3) adding the shrimp shell powder prepared in the step (S1) into a ternary eutectic solvent, heating and stirring for a period of time under ultrasonic and microwave treatment until the shrimp shell powder tissue structure is fully dissociated and dissolved, adding a back extraction solvent deionized water at room temperature, centrifuging to neutrality to obtain a precipitate, decoloring the precipitate with hydrogen peroxide, and drying to obtain the chitin.
Further, the solution used for soaking in the S1 is 90% -100% ethanol solution, the heating and stirring temperature is 25 ℃ -40 ℃ and the time is 2-8 hours.
Further, the drying temperature in S1 is 90-100 ℃.
Further, the shrimp shell powder in the step S1 is filtered through a filter screen with 80-200 meshes.
Further, the mass ratio of the shrimp shell powder to the ternary eutectic solvent in the S2 is 1:5-1:20.
Further, the ultrasonic power of ultrasonic and microwave treatment in the step S2 is 50W/40kHz, the microwave heating temperature is 40-70 ℃, and the treatment time is 1-5 h.
Further, 10% H was used in S2 2 O 2 Decoloring, and drying at 50-90 deg.C.
The beneficial effects of the invention are as follows:
the invention takes choline chloride as a hydrogen bond acceptor, lactic acid and acetic acid as hydrogen bond donors, and prepares the ternary eutectic solvent which has obvious improvement effect on the extraction of procambarus clarkia chitin.
The acid in the eutectic solvent can react with mineral substances in the procambarus clarkia shrimp shell to generate a demineralization effect, so that a fibril structure combined by chitin and protein is loosened to generate a gap, chlorine in a hydrogen bond acceptor choline chloride has strong electronegativity and can form an anion, cation and neutral ion hydrogen bond, thereby being beneficial to the formation of hydrated ions, leading to ionization and protonation enhancement of the eutectic solvent, and further improving the demineralization effect. In addition, the eutectic solvent can form a new hydrogen bond with chitin and protein, so that the strong hydrogen bond action in the repeated unit of chitin is weakened, and the valence bond of the chitin connected with other macromolecules can be broken, so that the original microstructures of the chitin and the protein are broken, the eutectic solvent is favorable for further swelling in the structure, and the rich active functional group structure in the protein can form a new hydrogen bond with a hydrogen bond receptor, so that the hydrogen bonds in and among the fibril structure molecules are broken, the protein is separated from the structure, and the removal of the protein is accelerated. The intramolecular/intermolecular hydrogen bond in the chitin is blocked by the eutectic solvent, and a new hydrogen bond is formed between the chitin molecule and the eutectic solvent, so that the purpose of separating the chitin is achieved.
The ternary eutectic solvent is used for extracting procambarus clarkia shell chitin, and the mineral removal is mainly the effect of acid, but not all the acid or strong acid can reach the result of the application, when single acid is used as a hydrogen bond donor, the demineralization effect is relatively poor when the acid is weak, but the demineralization effect is good when the acid is strong, but the acid hydrolysis of chitin into disaccharide is also caused, the yield is obviously reduced, and the strong acid can increase the surface modification of chitin, and can also improve the esterification reaction between the hydroxyl of chitin and the carboxyl of acid in the hydrogen bond donor, thereby influencing the final extraction effect and quality. And when lactic acid and acetic acid are adopted as hydrogen bond donors, more hydrogen bonds with richer structures are formed, and the acid condition for maintaining buffer balance is more favorable for the exertion of the demineralization effect, the relationship between the acidity of the hydrogen bond donors and the yield and purity of chitin is not clear in the scientific community at present, but the combination and the proportion of the two hydrogen bond donors can promote the elimination of mineral substances, and the ternary eutectic solvent prepared by adopting the two acid hydrogen bond donors with different properties can achieve better deproteinization and chitin extraction effects.
The invention adopts the efficient extraction of ternary eutectic solvent, obtains the procambarus clarkia shell chitin with higher purity by a heating and ultrasonic microwave treatment one-pot method, does not use strong acid for desalting, can obviously reduce the production cost, can also put an end to chemical reagents in the purification process, reduces environmental pollution, and can greatly improve the extraction rate of the chitin.
Drawings
Fig. 1 is an SEM image of three-way eutectic solvent extracted chitin (a), commercial chitin (b) and shrimp shell (c).
As can be seen from fig. 1, the morphology and surface of the extracted chitin were significantly changed compared to the shrimp shells. The shrimp shell surface is rough and free of pores due to the presence of minerals and proteins. For the chitin extracted by eutectic melting, the surface is smooth and porous due to the removal of minerals and proteins.
Detailed Description
Example 1
Preparing shrimp shell powder: collecting the shrimp shells of procambarus clarkia, carrying out ultrasonic cleaning, removing foreign matters, soaking in a 90% -100% ethanol solution, heating and stirring at 25-40 ℃ for 2-8 hours, carrying out ultrasonic treatment, washing with water, drying at 90-100 ℃ in a drying box, crushing by a high-speed crusher, and sieving by a 120-mesh filter screen to obtain shrimp shell powder for later use.
Preparing a ternary eutectic solvent: and (3) weighing choline chloride, acetic acid and lactic acid according to a molar ratio of 1:1:1, sequentially adding the choline chloride, the acetic acid and the lactic acid into a beaker, and placing the beaker in an oil bath pot at 100 ℃ and continuously stirring the oil bath pot to form transparent liquid, thus obtaining the ternary eutectic solvent.
Extracting chitin: weighing shrimp shell powder according to the mass ratio of 1:8, mixing with the ternary eutectic solvent, and reacting in an ultrasonic-microwave extraction container with the temperature set at 50 ℃ for 2 hours to obtain a reaction product. Adding distilled water into the reactant cooled to room temperature, cooling, centrifuging on a high-speed centrifuge, repeatedly washing until the reactant is nearly neutral, and drying the precipitate to obtain white flakes, thus obtaining the chitin. The extraction rate of the chitin after weighing is 28.06 percent, the ash content is 0.25 percent, and the protein content is 3.51 percent.
Example 2
Preparing shrimp shell powder: collecting the shrimp shells of procambarus clarkia, carrying out ultrasonic cleaning, removing foreign matters, soaking in a 90% -100% ethanol solution, heating and stirring at 30-35 ℃ for 2-8 hours, carrying out ultrasonic treatment, washing with water, drying at 90-100 ℃ in a drying box, crushing by a high-speed crusher, and sieving by a 200-mesh filter screen to obtain shrimp shell powder for later use.
Preparing a ternary eutectic solvent: and (3) weighing choline chloride, acetic acid and lactic acid according to a molar ratio of 1:3:1, sequentially adding the choline chloride, the acetic acid and the lactic acid into a beaker, and placing the beaker in an oil bath pot at 100 ℃ and continuously stirring the oil bath pot to form transparent liquid, thus obtaining the ternary eutectic solvent.
Extracting chitin: weighing shrimp shell powder according to the mass ratio of 1:10, mixing with the ternary eutectic solvent, and reacting for 4 hours in an ultrasonic microwave extraction container with the temperature set to 55 ℃ to obtain a reaction product. Adding distilled water into the reactant cooled to room temperature, cooling, centrifuging on a high-speed centrifuge, repeatedly washing until the reactant is nearly neutral, and drying the precipitate to obtain white flakes, thus obtaining the chitin. The extraction rate of the chitin after weighing is 31.26 percent, the ash content is 0.30 percent, and the protein content is 3.40 percent.
Example 3
Preparing shrimp shell powder: collecting the shrimp shells of procambarus clarkia, carrying out ultrasonic cleaning, removing foreign matters, soaking in a 90% -100% ethanol solution, heating and stirring at 25-30 ℃ for 2-8 hours, carrying out ultrasonic treatment, washing with water, drying at 90-100 ℃ in a drying box, crushing by a high-speed crusher, and sieving by a 120-mesh filter screen to obtain shrimp shell powder for later use.
Preparing a ternary eutectic solvent: and (3) weighing choline chloride, acetic acid and lactic acid according to a molar ratio of 1:3:3, sequentially adding the choline chloride, the acetic acid and the lactic acid into a beaker, and placing the beaker in an oil bath pot at 100 ℃ and continuously stirring the oil bath pot to form transparent liquid, thus obtaining the ternary eutectic solvent.
Extracting chitin: weighing shrimp shell powder according to the mass ratio of 1:8, mixing with the ternary eutectic solvent, and stirring and reacting for 3 hours in an ultrasonic-microwave extraction container with the temperature set at 60 ℃ to obtain a reaction product. Adding distilled water into the reactant cooled to room temperature, cooling, centrifuging on a high-speed centrifuge, repeatedly washing until the reactant is nearly neutral, and drying the precipitate to obtain white flakes, thus obtaining the chitin. The extraction rate of the chitin after weighing is calculated to be 30.46%, the ash content is 0.28%, and the protein content is 3.70%.
Example 4
Preparing shrimp shell powder: collecting the shrimp shells of procambarus clarkia, carrying out ultrasonic cleaning, removing foreign matters, soaking in a 90% -100% ethanol solution, heating and stirring at 30-40 ℃ for 2-8 hours, carrying out ultrasonic treatment, washing with water, drying at 90-100 ℃ in a drying box, crushing by a high-speed crusher, and sieving by a 200-mesh filter screen to obtain shrimp shell powder for later use.
Preparing a ternary eutectic solvent: and (3) weighing choline chloride, acetic acid and lactic acid according to a molar ratio of 1:1:3, sequentially adding the choline chloride, the acetic acid and the lactic acid into a beaker, and placing the beaker in an oil bath pot at 100 ℃ and continuously stirring the oil bath pot to form transparent liquid, thus obtaining the ternary eutectic solvent.
Extracting chitin: weighing shrimp shell powder according to the mass ratio of 1:10, mixing with the ternary eutectic solvent, and stirring and reacting for 2 hours in an ultrasonic-microwave extraction container with the temperature set at 60 ℃ to obtain a reaction product. Adding distilled water into the reactant cooled to room temperature, cooling, centrifuging on a high-speed centrifuge, repeatedly washing until the reactant is nearly neutral, and drying the precipitate to obtain white flakes, thus obtaining the chitin. The extraction rate of the chitin after weighing is calculated to be 29.86%, the ash content is 0.31%, and the protein content is 3.45%.
Comparative example 1
The binary eutectic solvent prepared by choline chloride and lactic acid with the molar ratio of 1:3 is adopted to replace the ternary eutectic solvent of the invention, other operations are the same as those of example 1, and the calculated extraction rate of the chitin after weighing is 25.78%, the ash content is 0.58% and the protein content is 4.62%.
Comparative example 2
The binary eutectic solvent prepared by choline chloride and acetic acid with the molar ratio of 1:3 is adopted to replace the ternary eutectic solvent of the invention, other operations are the same as those of example 1, and the calculated extraction rate of the chitin after weighing is 26.12%, the ash content is 0.63% and the protein content is 4.69%.
Claims (8)
1. The application of the ternary eutectic solvent in the extraction of procambarus clarkia shell chitin is characterized in that the ternary eutectic solvent is prepared by mixing choline chloride, lactic acid and acetic acid, and the molar ratio of the choline chloride to the lactic acid to the acetic acid is 1:1:1-1:3:3;
the specific steps for extracting the chitin of the procambarus clarkia shell are as follows:
s1: collecting the shrimp shells of procambarus clarkia, ultrasonically cleaning, removing foreign matters, soaking in the solution, heating and stirring for a period of time, then ultrasonically treating, washing with water, drying in a drying oven, crushing by a high-speed crusher, and sieving to obtain shrimp shell powder for later use;
s2: and (3) adding the shrimp shell powder prepared in the step (S1) into a ternary eutectic solvent, heating and stirring for a period of time under ultrasonic and microwave treatment until the shrimp shell powder tissue structure is fully dissociated and dissolved, adding a back extraction solvent deionized water at room temperature, centrifuging to neutrality to obtain a precipitate, decoloring the precipitate with hydrogen peroxide, and drying to obtain the chitin.
2. The use of a ternary eutectic solvent in the extraction of procambarus clarkia shell chitin as claimed in claim 1, characterized in that: when the choline chloride, the lactic acid and the acetic acid are mixed to prepare the ternary eutectic solvent, the temperature is 90-150 ℃ and the time is 8-24 hours.
3. The use of a ternary eutectic solvent in the extraction of procambarus clarkia shell chitin as claimed in claim 1, characterized in that: the solution used for soaking in the S1 is 90% -100% ethanol solution, the heating and stirring temperature is 25 ℃ -40 ℃ and the time is 2-8 hours.
4. The use of a ternary eutectic solvent in the extraction of procambarus clarkia shell chitin as claimed in claim 1, characterized in that: and in S1, the drying temperature is 90-100 ℃.
5. The use of a ternary eutectic solvent in the extraction of procambarus clarkia shell chitin as claimed in claim 1, characterized in that: and S1, screening the shrimp shell powder by a filtering screen with 80-200 meshes.
6. The use of a ternary eutectic solvent in the extraction of procambarus clarkia shell chitin as claimed in claim 1, characterized in that: and S2, the mass ratio of the shrimp shell powder to the ternary eutectic solvent is 1:5-1:20.
7. The use of a ternary eutectic solvent in the extraction of procambarus clarkia shell chitin as claimed in claim 1, characterized in that: and S2, the ultrasonic power of ultrasonic and microwave treatment is 50W/40kHz, the microwave heating temperature is 40-70 ℃, and the treatment time is 1-5 h.
8. The use of a ternary eutectic solvent in the extraction of procambarus clarkia shell chitin as claimed in claim 1, characterized in that: s2 is 10% H 2 O 2 Decoloring, and drying at 50-90 deg.C.
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| CN112726253A (en) * | 2021-01-21 | 2021-04-30 | 天津科技大学 | Method for efficiently separating plant fibers by acidic eutectic solvent/metal salt multi-component system |
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