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CN-122010708-A - Curcumin preparation method and curcumin

CN122010708ACN 122010708 ACN122010708 ACN 122010708ACN-122010708-A

Abstract

The invention belongs to the technical field of natural product extraction, and in particular relates to a curcumin preparation method and curcumin, wherein the preparation method comprises the following steps of (1) turmeric pretreatment; the method comprises the steps of (1) primary flash extraction, (3) variable-frequency ultrasonic enzymolysis, (4) secondary flash enzyme deactivation, (5) macroporous resin purification, and (6) concentration and drying. The invention has the beneficial effects that the effective extraction (including wall breaking and enzymolysis) time is shortened to 20-30 minutes from 3-4 hours in the prior art through the cooperation of two-stage flash extraction and variable frequency ultrasonic enzymolysis. The data of the embodiment show that the curcumin extraction yield reaches 5.42-5.45%, the process time is short, the energy consumption is low, the enzyme consumption is low, the action time is short, the ethanol-water system is adopted, the safety and the low toxicity are realized, the use of strong acid, strong alkali or surfactant is avoided, the product is purer, and the post-treatment is simple.

Inventors

  • TIAN YUTING
  • Cheng Lujie
  • XIAO HANLIN
  • You Sizhe

Assignees

  • 福建农林大学

Dates

Publication Date
20260512
Application Date
20260115

Claims (10)

  1. 1. The preparation method of curcumin is characterized by comprising the following steps: (1) Pretreating turmeric, namely crushing turmeric, circularly flushing the turmeric with a mixed solvent of petroleum ether and normal hexane, centrifuging and drying to obtain defatted turmeric powder; (2) First-stage flash extraction, namely placing the defatted turmeric powder into a flash extractor, and adding ethanol for high-speed shearing extraction; (3) Performing variable-frequency ultrasonic enzymolysis, namely performing primary low-frequency ultrasonic treatment on the materials subjected to primary flash extraction, adding compound enzyme, and performing compound enzymolysis under a secondary high-frequency ultrasonic condition; (4) Secondary flash extraction and enzyme deactivation, namely performing secondary flash extraction on the material subjected to the frequency conversion ultrasonic enzymolysis, and simultaneously realizing enzyme deactivation and extraction, and centrifuging to obtain turmeric extract; (5) Macroporous resin purification, namely diluting the turmeric extract, loading the turmeric extract to a macroporous resin column, and carrying out adsorption, washing and elution to obtain curcumin eluent; (6) Concentrating and drying the curcumin eluent to obtain curcumin powder.
  2. 2. The method for preparing curcumin according to claim 1, wherein in the step (1), the volume ratio of petroleum ether to n-hexane is 8:2.
  3. 3. The method for preparing curcumin according to claim 1, wherein in the step (2), the ethanol is an aqueous solution with a volume fraction of 70-75%, and the feed liquid ratio of the defatted turmeric powder to the ethanol is 1 (30-40) g/mL.
  4. 4. The method for preparing curcumin according to claim 1, wherein the rotational speeds of flash extraction in the step (2) and the step (4) are 5000-6000 r/min and 7500-8500 r/min, respectively.
  5. 5. The method for preparing curcumin according to claim 1, wherein in the step (3), the frequency of the primary low-frequency ultrasonic wave is 20 kHz, the frequency of the secondary high-frequency ultrasonic wave is 80-180 kHz, the temperature of the composite enzymolysis is 40-45 ℃, and the pH value is 5.5.
  6. 6. The method for preparing curcumin according to claim 1, wherein in the step (3), the complex enzyme comprises cellulase, pectase and beta-glucanase, the mass ratio of the cellulase, pectase and beta-glucanase is (5-7): 1 (2-4): 1, and the total addition amount of the complex enzyme is 0.1-0.2% of the mass of the material.
  7. 7. The method for preparing curcumin according to claim 1, wherein in the step (5), before the macroporous resin is loaded and adsorbed, the turmeric extract is diluted with pure water to a volume content of ethanol of 16% or less.
  8. 8. The method for preparing curcumin according to claim 1, wherein in the step (5), the macroporous resin is D301 type weak-base anion exchange resin, and the eluent is 80-95% ethanol solution.
  9. 9. The method for preparing curcumin according to claim 1, wherein in the step (3), the total time of the variable-frequency ultrasonic enzymolysis is 20-30 minutes.
  10. 10. Curcumin prepared by the method for preparing curcumin according to any one of claims 1-9.

Description

Curcumin preparation method and curcumin Technical Field The invention belongs to the technical field of natural product extraction, and particularly relates to a preparation method of curcumin and curcumin. Background Turmeric is a dried rhizome of the plant Curcuma longa L (Curcuma longa L) of the genus Curcuma of the family Zingiberaceae, is a perennial herb, and is mainly distributed in Asia, mainly produced in China and India. Research shows that turmeric has wide pharmacological activities, including anti-tumor, anti-inflammatory, anti-oxidation, antiviral, immune-modulating, etc. The main active ingredient of the turmeric is curcumin, which can kill cancer cells and inhibit proliferation of the cancer cells, and has good anticancer effect. However, curcumin is contained in turmeric in a low amount (usually about 3 to 6%) and is encapsulated in dense cell walls and cell interstitium composed of cellulose, hemicellulose, pectin, lignin and lipids, resulting in low extraction efficiency, complex process and high energy consumption. The existing curcumin extraction method mainly comprises the following steps: the organic solvent extraction method is to reflux or extract with ethanol, acetone, etc. The method has simple operation, but low extraction rate, high solvent consumption, easy residue, and long-time extraction at high temperature can cause curcumin degradation. Enzyme-assisted extraction method comprises destroying cell wall with cellulase, pectase, etc. For example, the chinese patent application publication No. CN108147955A discloses a "flash extraction+complex enzymolysis" process, but the enzymolysis step is an independent static process (3 hours), and uses amylase and papain, which has no strong pertinence to the main components of turmeric cell wall, and still requires high temperature to inactivate enzyme (usually above 85 ℃) after enzymolysis, which may destroy thermosensitive curcumin, and the subsequent purification needs to rely on complex crystallization step. Ultrasonic assisted extraction, which utilizes ultrasonic cavitation and mechanical effect to promote mass transfer. For example, the Chinese patent application with publication number CN113387785A discloses "composite enzymolysis and continuous flow ultrasonic extraction", but the method relies on continuous flow and ultrasonic of solvent, does not adopt high-speed mechanical shearing to perform physical wall breaking, and the enzymolysis time is still 3-4 hours, so that the whole process time is longer. Flash extraction, which uses high-speed shearing force to break the cells instantaneously. However, the single use of the cell wall is often incomplete in breaking the wall, and the damage to the deep cell wall structure is limited. In summary, the prior art has the following problems that (1) a single physical wall breaking (such as flash extraction) or biological enzymolysis is difficult to completely destroy the complex cell wall structure of turmeric. (2) The static enzymolysis time is long, the mass transfer efficiency is low, and the enzyme system is not selected to be optimal for the turmeric cell wall. (3) The steps are serially connected, the total time is long, and the steps of enzyme deactivation and purification are complex. (4) High temperature enzyme deactivation or prolonged extraction may lead to degradation of curcumin. Therefore, an integrated process capable of efficiently, rapidly and mildly extracting high-purity and high-activity curcumin from turmeric is developed, and has important industrial value. Disclosure of Invention Aiming at the defects of the prior art, the invention aims to provide a high-efficiency curcumin preparation method, which realizes the synergistic effect of wall breaking, enzymolysis, enzyme deactivation and extraction by creatively deeply fusing two-stage flash extraction and variable-frequency ultrasonic coupling compound enzymolysis and designing a specific process sequence, thereby achieving the aims of shortening the time, improving the extraction rate and the product purity and protecting the biological activity of curcumin. In order to solve the technical problems, the invention adopts the technical scheme that the preparation method of curcumin comprises the following steps: (1) Pretreating turmeric, namely crushing turmeric, circularly flushing the turmeric with a mixed solvent of petroleum ether and normal hexane, centrifuging and drying to obtain defatted turmeric powder; (2) First-stage flash extraction, namely placing the defatted turmeric powder into a flash extractor, and adding ethanol for high-speed shearing extraction; (3) Performing variable-frequency ultrasonic enzymolysis, namely performing primary low-frequency ultrasonic treatment on the materials subjected to primary flash extraction, adding compound enzyme, and performing compound enzymolysis under a secondary high-frequency ultrasonic condition; (4) Secondary flash extraction and enzyme deactivation, namely