CN114456408A - Preparation method of fungus fruiting body ionic liquid - Google Patents

Preparation method of fungus fruiting body ionic liquid Download PDF

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Publication number
CN114456408A
CN114456408A CN202210115948.6A CN202210115948A CN114456408A CN 114456408 A CN114456408 A CN 114456408A CN 202210115948 A CN202210115948 A CN 202210115948A CN 114456408 A CN114456408 A CN 114456408A
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fruiting body
ionic liquid
macrofungi
fungus
preparation
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CN114456408B (en
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袁久刚
徐进
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Jiangnan University
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Jiangnan University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/09Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
    • C08J3/091Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
    • C08J3/096Nitrogen containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2499/00Characterised by the use of natural macromolecular compounds or of derivatives thereof not provided for in groups C08J2401/00 - C08J2407/00 or C08J2489/00 - C08J2497/00

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Preparation Of Fruits And Vegetables (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention discloses a preparation method of fungus fruiting body ionic liquid, which comprises the following steps: (1) pretreating the fruiting body of the macrofungi to obtain powder of the fruiting body of the macrofungi; (2) and (2) mixing the ionic liquid, caustic soda and the large fungus fruiting body powder prepared in the step (1) under stirring, heating, removing water, and filtering to obtain the fungus fruiting body ionic liquid. The invention can dissolve macromolecular protein, dietary fiber and glycoprotein compound contained in the fruiting body, thereby realizing the full element dissolution of the fruiting body, having high utilization rate and being beneficial to expanding the application range of the fruiting body of the macrofungi.

Description

Preparation method of fungus fruiting body ionic liquid
Technical Field
The invention relates to the technical field of natural edible fungus dissolution and regeneration, in particular to a method for preparing fungus fruiting body ionic liquid by dissolving all components of edible fungus fruiting body by taking the ionic liquid as a solvent.
Background
Fungi are neither plants nor animals, but are an independent biological group, the kingdom fungi. There are more than 6000 kinds of fungi which can form large-scale fruiting body or sclerotium tissue in nature, and in China, more than 50 kinds of edible mushrooms are 938 kinds and artificially cultivated. In 2019, the yield of edible fungi in China is about 4000 ten thousand tons, wherein 1115.94 ten thousand tons of shiitake mushrooms, 701.81 ten thousand tons of black fungus, 686.47 ten thousand tons of oyster mushrooms and 258.96 ten thousand tons of needle mushrooms are available. The large edible fungi not only have delicious taste, but also are rich in nutrients such as protein, sugar and dietary fiber, and therefore, the large edible fungi are widely accepted by consumers. Taking common shiitake mushroom as an example, each 100g of dry matter contains 26.5g of protein, 22.9g of carbohydrate and 39.8g of dietary fiber.
However, the efficiency of use of macrofungi is not high. Besides a part of the fungi can be used as food, some macrofungi, such as ganoderma lucidum, contain soluble micromolecular substances such as polysaccharide for improving immunity, and the like, and are also applied to the fields of medical treatment and health care products. The application of the part of fields is mainly to extract the contained fungal polysaccharide component by using water, alcohol or some aqueous two-phase systems. For example: yan Jingkun et al extracted and separated soluble polysaccharides and proteins from fungi using a two aqueous phase system of choline and water. However, these water-soluble polysaccharides or polypeptides are only a small part of the total components of the fungal fruiting body, and most of the high molecular weight proteins, polysaccharide-protein complexes and dietary fibers contained in the fungal fruiting body are not dissolved and cannot be effectively utilized, and are discarded in vain. Therefore, the efficiency of using the fruiting body of a macrofungus is too low from the viewpoint of the full-scale use of resources.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of fungus fruiting body ionic liquid. The fungus fruiting body ionic liquid is rich in components such as protein, polysaccharide, chitin and the like, can be applied to the field of material processing, and can be used for producing ultrafine powder, fibers, films, porous materials and the like by using a concentrated solution; it can be added into cosmetics and health products, and also can be used for improving the functionality and dyeability of textiles by using the coating, and the application prospect is immeasurable.
The technical scheme adopted by the invention is as follows:
the preparation method of the fungus fruiting body ionic liquid is characterized by comprising the following steps:
(1) pretreating the fruiting body of the macrofungi to obtain powder of the fruiting body of the macrofungi;
(2) and (2) mixing the ionic liquid, caustic soda and the large fungus fruiting body powder prepared in the step (1) under stirring, heating, removing water, and filtering to obtain the fungus fruiting body ionic liquid.
Preferably, in the step (1), the pretreatment method comprises the following steps: drying the fruiting body of the macrofungi, then mechanically crushing, extracting to remove grease, and drying to obtain the powder of the fruiting body of the macrofungi.
Preferably, the macro fungi is one or more of flammulina velutipes, agaricus bisporus, lucid ganoderma, shiitake mushrooms, straw mushrooms, coprinus comatus, agrocybe cylindracea, mushrooms, pholiota nameko, poria cocos, agaric, tremella, hericium erinaceus, dictyophora phalloidea, tricholoma matsutake, russula vinosa, cordyceps sinensis, truffle, pleurotus nebrodensis, bolete, morchella esculenta, saddle fungi and truffles.
Preferably, the water content of the fruiting body of the macrofungi is less than 10% after drying. More preferably, the water content of the fruiting body of the macrofungi is 0.5-5% after drying.
Preferably, the solvent used for extraction is acetone. More preferably, the fruit body powder after extraction contains less than 0.5% fat.
Preferably, in the step (2), the ionic liquid is one or more of 1-allyl-3-methylimidazole chloride salt, 1-butyl-3-methylimidazole chloride salt, 1-ethyl-3-methylimidazole chloride salt, 1-butyl-3-methylimidazole acetate and 1-ethyl-3-methylimidazole diethyl phosphate.
Preferably, in the step (2), the amount of the caustic soda is 1-5% of the mass of the ionic liquid; the dosage of the macrofungi fruiting body powder is 0.1-200% of the mass of the ionic liquid.
Further preferably, the using amount of the caustic soda is 0.1-10% of the mass of the ionic liquid; the dosage of the macrofungi fruiting body powder is 1-50% of the mass of the ionic liquid.
Further preferably, in the step (2), during the stirring and mixing process, the mixture is heated to 80-100 ℃ first, then heated to 100-140 ℃, and the dissolution is promoted by adopting a vacuum pumping mode.
An ionic liquid of fungus fruiting body prepared by the preparation method.
Application of the fungus fruiting body ionic liquid in preparation of ultrafine powder, spinning, coating or porous material.
The beneficial technical effects of the invention are as follows:
the invention solves the problem that most dry substances can not be effectively utilized except for partially edible and partially extracted fungal polysaccharide or polypeptide substances of the fruiting body of the large fungus in the prior art, can dissolve the fungal polysaccharide extracted from the fruiting body and can dissolve macromolecular protein, dietary fiber and glycoprotein compounds contained in the fruiting body, thereby realizing the complete element dissolution of the fruiting body, having high utilization rate and being beneficial to expanding the application range of the fruiting body of the large fungus.
The ionic liquid adopted by the invention is a substance with extremely high polarity, has extremely strong dissolving capacity on protein, cellulose and polysaccharide, and can obtain a sporophore ionic liquid solution with the mass fraction of more than 50 percent by further dissolving in vacuum with the assistance of pretreatment of the invention.
The ionic liquid in the invention has the characteristics of high temperature resistance, non-volatility, no pungent smell, recoverability and the like, so the preparation process is simple and convenient, and meets the requirements of green mass production.
Detailed Description
The present invention will be described in detail with reference to examples.
1. Measurement of dissolution mass fraction
Taking 1 support, plugging the colorimetric tube, respectively adding 10g of ionic liquid, then respectively adding a certain mass of fruit body powder, filtering the solution when the system is dissolved to be in a clear and transparent state, drying filter residues to be absolutely dry, and weighing.
The dissolution mass fraction is (fruiting body powder mass-filter residue mass)/ionic liquid mass is 100%
2. Determination of fat content
The measurement was carried out according to GB5512-85 standard using a fat tester.
Example 1
A preparation method of fungus fruiting body ionic liquid comprises the following steps:
(1) drying Ganoderma fruiting body to water content of 5%, pulverizing Ganoderma fruiting body with ball mill, extracting with acetone for 24 hr to remove fat, and making into Ganoderma fruiting body powder;
(2) adding 2 wt% of caustic soda into 1-butyl-3-methylimidazolyl acetate ionic liquid, heating to 90 ℃, adding the ganoderma lucidum fruiting body powder prepared in the step (1) into the ionic liquid according to the mass ratio of 10%, stirring and mixing uniformly, heating the system to 100 ℃, vacuumizing, removing water contained in the system, continuously stirring until the system is dissolved to be amber, and finally filtering to remove a small amount of insoluble substances to obtain the ionic liquid solution containing the ganoderma lucidum fruiting body, wherein the mass fraction of the solution is 85 wt%.
Example 2
A preparation method of fungus fruiting body ionic liquid comprises the following steps:
(1) drying the fruiting body of Lentinus Edodes to water content of 1.0%, pulverizing by ball mill, extracting with acetone for 12 hr to remove fat, and making the fat content lower than 0.5% to obtain fruiting body powder of Lentinus Edodes;
(2) adding 5 wt% of caustic soda into 1-butyl-3-methylimidazolium chloride ionic liquid, heating to 90 ℃, adding the lentinus edodes fruiting body powder prepared in the step (1) into the ionic liquid according to the mass ratio of 100%, uniformly stirring and mixing, heating the system to 140 ℃, vacuumizing, removing water contained in the system, continuously stirring until the system is dissolved to be amber, and finally filtering to remove a small amount of insoluble substances to obtain the ionic liquid solution containing the lentinus edodes fruiting bodies, wherein the mass fraction of the solution is 72 wt%.
Example 3
A preparation method of fungus fruiting body ionic liquid comprises the following steps:
(1) drying oyster mushroom fruiting bodies to the water content of 10%, crushing the oyster mushroom fruiting bodies by using a ball mill, extracting the crushed oyster mushroom fruiting bodies for 20 hours by using acetone to remove fat, and enabling the fat content to be lower than 0.5% to obtain oyster mushroom fruiting body powder;
(2) adding 10 wt% of caustic soda into 1-ethyl-3-methylimidazolium chloride ionic liquid, heating to 100 ℃, adding 200 wt% of oyster mushroom fruiting body powder prepared in the step (1) into the ionic liquid, uniformly stirring and mixing, heating the system to 130 ℃, vacuumizing, removing water contained in the system, continuously stirring until the system is dissolved to be amber, and finally filtering to remove a small amount of insoluble substances to obtain an ionic liquid solution containing oyster mushroom fruiting bodies, wherein the mass fraction of the solution is 95 wt%.
Comparative example 1
A preparation method of fungus fruiting body ionic liquid comprises the following steps:
(1) drying Ganoderma fruiting body to water content of 5%, pulverizing Ganoderma fruiting body with ball mill, extracting with acetone for 24 hr to remove fat, and making into Ganoderma fruiting body powder;
(2) in choline chloride/K3PO4Adding 2 wt% of caustic soda into a system consisting of distilled water, heating to 90 ℃, adding the ganoderma lucidum fruiting body powder prepared in the step (1) into the system according to the mass ratio of 10%, stirring and mixing uniformly, heating the system to 100 ℃, and then continuously stirring. Wherein, choline chloride/K3PO4The mass ratio of the distilled water to the distilled water is 0.5:0.5: 1;
in comparison with example 1, comparative example 1 cannot be vacuumized because it contains a large amount of water, and choline chloride/K is visible to the naked eye after stirring for 24 hours3PO4The system consisting of distilled water can not completely dissolve all components of the fruiting body, and the dissolution rate is only 35% by testing, which shows that the choline chloride ionic liquid aqueous two-phase system can not dissolve most of the components of the fruiting body of the fungus, but only extract micromolecular polysaccharide and partial water-soluble protein of the fungus.
Application example 1
Directly pouring the ionic liquid solution containing the lucid ganoderma sporocarp prepared in the example 1 into ethanol with the volume being 3 times that of the solution, uniformly stirring, filtering to obtain superfine powder after the powder of the lucid ganoderma sporocarp is completely separated out, washing with ethanol for multiple times, and removing the attached ionic liquid to obtain the lucid ganoderma superfine powder. The superfine powder can be used as additive for health product or cosmetic.
Application example 2
The preparation method comprises the steps of defoaming and filtering the ionic liquid solution containing the lentinus edodes fruiting bodies prepared in the embodiment 2, adopting a dry-jet wet spinning process, enabling the ionic liquid solution to pass through a metering pump, passing through a spinneret plate, controlling the length of an air gap, finally enabling the ionic liquid solution to enter an ionic liquid aqueous solution for solidification and forming, stretching, washing and drying the ionic liquid aqueous solution to form fibers, and obtaining the lentinus edodes fibers, wherein the strength of the fibers can reach 0.2 cN/dT.
Application example 3
The ionic liquid solution containing the fruiting body of shiitake mushroom obtained in example 2 was defoamed, filtered, and cast into a film, and the ionic liquid was precipitated using ethanol as a coagulation bath to obtain a transparent hard film having a film strength of 3.1MPa and an elongation at break of 21.2%.
Application example 4
The ionic liquid solution containing the mushroom fruiting bodies prepared in the embodiment 2 is directly placed in a refrigerator with the temperature of minus 20 ℃, precooled for 24 hours, then placed in a refrigerator with the temperature of minus 80 ℃ for freeze-drying for 48 hours, and taken out and soaked in ethanol to obtain the porous material of the fungus fruiting bodies, wherein the porosity of the material is about 78%, the material has good adsorption performance, and the water absorption rate is 1.6 times.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. The preparation method of the fungus fruiting body ionic liquid is characterized by comprising the following steps:
(1) pretreating the fruiting body of the macrofungi to obtain powder of the fruiting body of the macrofungi;
(2) and (2) mixing the ionic liquid, caustic soda and the large fungus fruiting body powder prepared in the step (1) under stirring, heating, removing water, and filtering to obtain the fungus fruiting body ionic liquid.
2. The method according to claim 1, wherein in the step (1), the pretreatment is carried out by: drying the fruiting body of the macrofungi, then mechanically crushing, extracting to remove grease, and drying to obtain the powder of the fruiting body of the macrofungi.
3. The method according to claim 2, wherein the macro fungi is one or more of needle mushroom, agaricus bisporus, ganoderma lucidum, shiitake mushroom, straw mushroom, coprinus comatus, agrocybe aegerita, mushroom, pholiota nameko, poria cocos, agaric, tremella, hericium erinaceus, dictyophora phalloidea, matsutake, tricholoma matsutake, russula, cordyceps sinensis, truffle, pleurotus nebrodensis, boletus, morchella, saddlefungus and truffle.
4. The method according to claim 2, wherein the water content of the fruiting body of the macrofungi after drying is less than 10%.
5. The method of claim 2, wherein the solvent used for extraction is acetone.
6. The method according to claim 1, wherein in the step (2), the ionic liquid is one or more of 1-allyl-3-methylimidazole chloride salt, 1-butyl-3-methylimidazole chloride salt, 1-ethyl-3-methylimidazole chloride salt, 1-butyl-3-methylimidazole acetate salt, and 1-ethyl-3-methylimidazole diethyl phosphate salt.
7. The preparation method according to claim 1, wherein in the step (2), the amount of the caustic soda is 1-5% of the mass of the ionic liquid; the dosage of the macrofungi fruiting body powder is 0.1-200% of the mass of the ionic liquid.
8. The preparation method according to claim 7, wherein the amount of the caustic soda is 0.1-10% of the mass of the ionic liquid; the dosage of the macrofungi fruiting body powder is 1-50% of the mass of the ionic liquid.
9. An ionic liquid of fungal fruiting body obtained by the method of claim 1.
10. Use of an ionic liquid of fungal fruiting bodies as claimed in claim 9 for the preparation of ultra fine powders, spun yarns, coatings or porous materials.
CN202210115948.6A 2022-02-07 2022-02-07 Preparation method of fungus fruiting body ionic liquid Active CN114456408B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103509133A (en) * 2013-10-10 2014-01-15 江苏大学 Method for rapidly separating lentinan
US20150099871A1 (en) * 2012-03-23 2015-04-09 K Hughes & Co., Ltd. Lentinan extraction process from mushrooms using ionic liquid
CN104861082A (en) * 2015-06-03 2015-08-26 江苏大学 Method for separating polysaccharide and protein by using choline ionic liquid two-phase aqueous system

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150099871A1 (en) * 2012-03-23 2015-04-09 K Hughes & Co., Ltd. Lentinan extraction process from mushrooms using ionic liquid
CN103509133A (en) * 2013-10-10 2014-01-15 江苏大学 Method for rapidly separating lentinan
CN104861082A (en) * 2015-06-03 2015-08-26 江苏大学 Method for separating polysaccharide and protein by using choline ionic liquid two-phase aqueous system

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
PARUSHI NARGOTRA等: ""Application of ionic liquid and alkali pretreatment for enhancing saccharification of sunflower stalk biomass for potential biofuel-ethanol production"", 《BIORESOURCE TECHNOLOGY》, vol. 267, pages 560 - 568, XP085444254, DOI: 10.1016/j.biortech.2018.07.070 *

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