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CN-117899520-B - Hydrophilic convertible ternary eutectic solvent and preparation method and application thereof

CN117899520BCN 117899520 BCN117899520 BCN 117899520BCN-117899520-B

Abstract

The invention discloses a hydrophilic convertible ternary eutectic solvent, a preparation method and application thereof, and belongs to the technical field of extraction of plant active substances. According to the invention, tetrabutyl ammonium chloride, dichloroacetic acid and ethylene glycol are used as raw materials to prepare the hydrophilic convertible ternary eutectic solvent, the eutectic solvent can be used as an extraction reagent for extracting polyphenol components in sorghum bran, and compared with 70% ethanol and 70% methanol of the traditional extraction reagent, the ternary eutectic solvent is used for extracting polyphenol in sorghum bran, so that the yield of polyphenol in sorghum bran is greatly improved.

Inventors

  • SU JING
  • JING XU
  • LI JIERU
  • Mi xue
  • WU YIZHEN
  • PAN MEIMEI

Assignees

  • 山西农业大学

Dates

Publication Date
20260508
Application Date
20240116

Claims (5)

  1. 1. The method for extracting polyphenol in sorghum bran by using hydrophilic convertible ternary eutectic solvent is characterized by comprising the following steps of: Crushing and sieving sorghum bran to obtain sorghum bran powder; adding the sorghum bran powder into a hydrophilic convertible ternary eutectic solvent, and performing ultrasonic treatment to obtain an extracting solution; centrifuging the extracting solution to separate two phases, wherein the upper layer is an aqueous phase containing sorghum bran polyphenol, the lower layer is a hydrophobic eutectic solvent phase, and the upper layer aqueous phase is the sorghum bran polyphenol extracting solution after being absorbed; The temperature of the centrifugal treatment is 0 ℃ to-12 ℃; the hydrophilic convertible ternary eutectic solvent is formed by mixing tetrabutyl ammonium chloride, dichloroacetic acid and ethylene glycol, and the dosage ratio is (4-4.5) g to (2-2.5) g to 1mL; The preparation method of the hydrophilic convertible ternary eutectic solvent comprises the steps of mixing tetrabutyl ammonium chloride, dichloroacetic acid and ethylene glycol, heating and stirring to obtain uniform transparent clear viscous liquid, mixing the viscous liquid with ultrapure water to obtain the hydrophilic convertible ternary eutectic solvent, wherein the water content of the hydrophilic convertible ternary eutectic solvent is 0-35% and is not 0.
  2. 2. The method of claim 1, wherein the ratio of the sorghum bran powder to the hydrophilic convertible ternary eutectic solvent is 1g to (10-50) mL.
  3. 3. The method according to claim 1, wherein the ultrasonic treatment is carried out at a power of 250W, a temperature of 20-60 ℃ and a time of 20-60min.
  4. 4. The method according to claim 1, wherein the centrifugation is carried out at a speed of 3000-5000rpm for a period of 5-15min.
  5. 5. The method according to claim 1, wherein ultra-pure water is added to the hydrophobic eutectic solvent phase and is heated and stirred to be converted into a hydrophilic convertible ternary eutectic solvent.

Description

Hydrophilic convertible ternary eutectic solvent and preparation method and application thereof Technical Field The invention belongs to the technical field of extraction of plant active substances, and particularly relates to a hydrophilic convertible ternary eutectic solvent, a preparation method and application thereof. Background Sorghum is the fifth largest grain crop of the world next to rice, wheat, corn and barley. Bran is one of the components of sorghum, has various phenolic substances, flavonoid compounds and procyanidins, and the phenolic substance content in the bran is six times that of grains. Because the sorghum bran contains the anti-nutritional factor tannin, not only the taste is affected, but also the utilization rate of the organism to the nutrients is reduced, so that the sorghum bran is often discarded in production, and waste is caused. Therefore, the utilization of the sorghum bran is promoted, and the method has important significance. In the extraction of active substances, conventional organic solvents such as methanol and ethanol are often used as extractant. However, the traditional organic solvent is used for extracting the sorghum bran polyphenol with low yield, high toxicity, poor biodegradability and low utilization rate, and a large amount of use can cause environmental pollution, so that the technical problem to be solved is how to extract the sorghum bran polyphenol with high efficiency and no toxicity. The eutectic solvent (DES) is a new generation of extraction solvent that can replace the extraction solvent in the traditional extraction process. The eutectic solvent consists of halide salt (i.e. hydrogen bond acceptor) and one or two hydrogen bond donors, has the advantages of biodegradability, low toxicity, low cost and the like, and is a high-quality solvent in the fields of separation, material science, biocatalysis and organic synthesis. The hydrogen bonding between the eutectic solvent donor and acceptor can also generate intermolecular interaction force with the target analyte, thereby achieving the extraction purpose. At present, DES is widely applied to extraction of components such as polyphenols, flavonoids, polysaccharides, proteins and the like in different raw materials. However, since the conventional eutectic solvent cannot be reused, and thus a great amount of waste is caused, it is important to develop a simple, rapid and efficient recovery of the eutectic solvent as an extractant. Disclosure of Invention The invention provides a hydrophilic convertible ternary eutectic solvent and a preparation method and application thereof, and aims to solve the problems that an existing extractant is low in extraction yield, high in toxicity, poor in biodegradability, likely to cause environmental pollution, difficult to recover an extract from the extractant and the like. Provides a new idea for the polyphenol extraction process. In order to achieve the above purpose, the present invention provides the following technical solutions: The invention aims at providing a hydrophilic convertible ternary eutectic solvent which is formed by mixing tetrabutyl ammonium chloride, dichloroacetic acid and ethylene glycol, wherein the dosage ratio is (4-4.5) g to (2-2.5) g to 1mL. The second purpose of the invention is to provide a preparation method of the hydrophilic convertible ternary eutectic solvent, which comprises the following steps of mixing tetrabutyl ammonium chloride, dichloroacetic acid and ethylene glycol, heating and stirring to obtain uniform transparent clear viscous liquid, and mixing the viscous liquid with ultrapure water to obtain the hydrophilic convertible ternary eutectic solvent. Further, the ultra-pure water is added in an amount such that the water content of the resulting hydrophilic convertible ternary eutectic solvent is 0 to 35% and not 0. Further, the heating and stirring are performed at 45-80 ℃ for 20-50min. The invention further provides an application of the hydrophilic convertible ternary eutectic solvent in extracting polyphenol components in plants. The invention provides a method for extracting polyphenol in sorghum bran by applying the hydrophilic convertible ternary eutectic solvent, which comprises the following steps: Crushing and sieving sorghum bran to obtain sorghum bran powder; Adding the sorghum bran powder into the hydrophilic convertible ternary eutectic solvent, and performing ultrasonic treatment to obtain an extracting solution; and (3) centrifuging the extracting solution to separate two phases, wherein the upper layer is an aqueous phase containing sorghum bran polyphenol, the lower layer is a hydrophobic eutectic solvent phase, and the upper layer aqueous phase is the sorghum bran polyphenol extracting solution after being absorbed. Further, the sieving is through an 80 mesh screen. Further, the dosage ratio of the sorghum bran powder to the hydrophilic convertible ternary eutectic solvent is 1g to (10-50) mL. Further,