Method for preparing oligomeric proanthocyanidins by enhanced degradation under pulsed electric field

A technology of oligomeric proanthocyanidins and high polymer procyanidins, which is applied in the direction of organic chemistry, can solve the problems of high temperature and high pressure, inconvenient operation, and high reaction requirements, and achieves the effects of less energy consumption, good auxiliary effect and high product purity.

Active Publication Date: 2013-02-13
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) The oxidative degradation method is unstable and easy to decompose during use and storage, and it is easy to cause phenolic hydroxyl groups to be oxidized to carboxyl groups, resulting in product inactivation;
[0007] (2) acid or alkali degradation method, in

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add high-poly proanthocyanidins (polymerization degree is 6.8) to 3% sodium sulfite aqueous solution by mass, control the mass concentration of high-poly proanthocyanidins to 16%, and control the temperature at 50°C, and use a continuous constant-flow pump to pump the mixture Pump into the pulse electric field device, and at the same time adjust the electric field strength to 45kV / cm, pulse width 50μs, pulse frequency 3kHz, bipolar narrow pulse square waveform, pulse processing time 12ms, cooling, centrifugation, alcohol precipitation and impurity removal, D101 macropore Resin adsorption, 2 times column volume distilled water washing, 4 times column volume volume percentage concentration is 40% ethanol aqueous solution elution, collect eluate, concentrate under reduced pressure, freeze-dry to obtain oligomeric proanthocyanidins, after testing, the average of the obtained proanthocyanidins The degree of polymerization was 3.29, and the yield was 94%.

Embodiment 2

[0025] Add high-poly proanthocyanidins (polymerization degree is 8.2), add the sodium sulfite aqueous solution that the mass percent content is 6%, control the mass concentration of high-poly proanthocyanidins to be 12%, and control the temperature at 50 ℃, pump the mixture with a continuous constant flow pump Enter the pulse electric field device, and adjust the electric field intensity to 45kV / cm, pulse width 80μs, pulse frequency 1.08kHz, bipolar square waveform, pulse processing time 15ms, cooling, centrifugation, alcohol precipitation and impurity removal, D101 macroporous resin adsorption , washing with water, and the volume percentage concentration of 2 times the column volume is 70% ethanol aqueous solution to elute, collect the eluate, concentrate under reduced pressure, and freeze-dry to obtain oligomeric proanthocyanidins. After testing, the average degree of polymerization of the obtained proanthocyanidins is 2.47, and the yield is 95%.

Embodiment 3

[0027] Add high-poly proanthocyanidins (polymerization degree is 8.2), add the sodium sulfite aqueous solution that the mass percent content is 1%, control the mass concentration of high-poly proanthocyanidins to be 10%, and control the temperature at 40 ℃, pump the mixture with a continuous constant flow pump Enter the pulse electric field device, adjust the electric field intensity to 40kV / cm, pulse width 100μs, pulse frequency 800Hz, bipolar square waveform, pulse processing time 10ms, cooling, centrifugation, alcohol precipitation and impurity removal, D101 macroporous resin adsorption, Wash with distilled water for 3 times the column volume, elute with 60% ethanol aqueous solution for 3 times the column volume, collect the eluate, concentrate under reduced pressure, and freeze-dry to obtain oligomeric proanthocyanidins. After testing, the average degree of polymerization of the obtained proanthocyanidins is 3.67 , the yield was 93.8%.

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Abstract

The invention discloses a method for preparing oligomeric proanthocyanidins by enhanced degradation under a pulsed electric field. According to the method, polymeric proanthocyanidins serving as raw materials are degraded under the assistance of the pulsed electric field to prepare the oligomeric proanthocyanidins. The method comprises the following steps of: dissolving the polymeric proanthocyanidins, adding sulfite, treating by the pulsed electric field, separating, performing alcohol leaching to remove impurities, purifying, concentrating and drying to obtain the oligomeric proanthocyanidins, wherein in the step of treating by the pulsed electric field, a polymeric proanthocyanidin solution is pumped in a pulse treatment chamber and is treated for 3 to 20 milliseconds under the conditions that the electric field intensity is 40 to 60 kV/cm, the pulse width is 50 to 120 microseconds and the pulse frequency is 100 to 3,000 Hz, and a pulse waveform is a square wave. The method is feasible, short in treatment time of the electric field, high in practicality, energy-saving and environment-friendly, so that the application range of the polymeric proanthocyanidins in fields of medicines, food, cosmetics and health-card products is expanded.

Description

technical field [0001] The invention relates to a preparation method of oligomeric proanthocyanidins, in particular to a method for preparing oligomeric proanthocyanidins by high-intensity pulsed electric field treatment. Background technique [0002] Proanthocyanidins are flavan-3-ol monomers passed through C 4 -C 8 or C 4 -C 6 The proanthocyanidin molecules are connected to a certain degree of polymerization, and the basic units are mainly catechin, epicatechin and epicatechin gallate. According to the size of the degree of polymerization, two-pentamers are usually called oligomers (OPC), and pentamers and above are called high polymers (PPC). Widely present in grape seeds, cypress, pine, and ginkgo, because of its special physiological activities and functions, it has a wide range of uses in cosmetics, leather and other fields, among which the application in the pharmaceutical industry is the most prominent. In medicine, proanthocyanidins have antioxidant properties ...

Claims

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Application Information

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IPC IPC(8): C07D311/62
Inventor 曾新安赵丹孙大文韩忠
Owner SOUTH CHINA UNIV OF TECH
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