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 inconvenient operation, high temperature and high pressure, and high reaction requirements, and achieves good auxiliary effects, low energy consumption, and high product purity.
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Embodiment 1
[0022] Add high-poly proanthocyanidins (polymerization degree: 6.8) to 3% sodium sulfite aqueous solution, 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
[0024] Add high-poly proanthocyanidin (polymerization degree is 8.2), add sodium sulfite aqueous solution with a mass percentage of 6%, control the mass concentration of high-poly proanthocyanidin to 12%, and control the temperature at 50°C, 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
[0026] Add high-poly proanthocyanidins (polymerization degree is 8.2), add sodium sulfite aqueous solution with a mass percentage of 1%, control the mass concentration of high-poly proanthocyanidins to 10%, and control the temperature at 40°C, 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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