Method for enriching and purifying procyanidin in pine bark

Abstract

The invention belongs to the field of natural organic chemistry, relating to a method for enriching and purifying procyanidin in pine bark. The method is characterized in that an intermittent distillation and macropore adsorbent resin coupling technology is used to separate and purify the procyanidin, and the technology is good for absorption selectivity of the procyanidin; and by using the intermittent distillation and macropore adsorbent resin coupling technology, absorption is quick and deabsorption is also quick, absorption capacity is large, extraction is convenient and quick, raw material source is rich, production cost is low, separation effect is obvious, extraction purity is high, above 50% of semi-finished product procyanidin and above 95% of final product procyanidin can be achieved, and the defects of low conventional extraction rate and low extraction purity are overcome. In the method, the macropore adsorbent resin which has the advantages of stable physicochemical property, large surface area, fast exchange speed, high mechanical strength, strong pollution resistance capability and good heat stability is selected, the procyanidin is selectively absorbed from solution through physical absorption, absorption is quick and deabsorption is also quick, and absorption capacity is large.

Description

Technical field:

[0001] The invention belongs to the field of natural organic chemistry and relates to a method for purifying proanthocyanidins, in particular to a method for enriching and purifying proanthocyanidins in pine bark by using a batch distillation-macroporous adsorption resin coupling method. Background technique:

[0002] Pine bark extract is a class of substances extracted from pine bark. The pine bark stripped from the trees is collected, flattened and extracted. It contains a large amount of compounds called OPCs (proanthocyanidin oligomers). A large number of studies have proved that OPCs are effective antioxidants, non-toxic, non-mutagenic, non-carcinogenic and have no side effects. It is very safe to use. Pine bark has been proven to be a new source of OPCs. The OPCs extracted from pine bark have no difference in quality and function, but there are some slight differences in appearance.

[0003] The English name of Proanthocyanidins is Oligomeric Proan...

Examples

Embodiment 1

[0026] Embodiment 1: A kind of method that utilizes batch distillation-macroporous adsorption resin coupling method to enrich and purify proanthocyanidins in pine bark, its steps are as follows:

[0027] (1) Pass through a 60-mesh sieve after the dried pine bark is crushed, and extract by heating and refluxing with 10 times the volume of pine bark powder under reflux for 3 times, each for 2 hours;

[0028] (2) Suction filtration of the pine bark extract treated in step (1) to obtain the extract and reclaim the initial extract of the solvent under reduced pressure;

[0029] (3) Heat and dissolve the obtained primary extract with ethanol, add purified water with a volume 20 times the volume of the extract alcohol solution for extraction, then adjust its pH value to 2.0 with acid, leave it to stand, suction filter, and recover the solvent under reduced pressure Obtain the crude extract of proanthocyanidins;

[0030] (4) The obtained proanthocyanidin extract is adsorbed on a macr...

Embodiment example 2

[0035] Implementation case 2: a method for enriching and purifying proanthocyanidins in pine bark by means of batch distillation-macroporous adsorption resin coupling method, the steps are as follows:

[0036] (1) After the dry pine bark is pulverized, cross a 10-mesh sieve, and extract by heating and refluxing with 20 times the volume of pine bark powder under reflux for 4 hours;

[0037] (2) Suction filtration of the pine bark extract treated in step (1) to obtain the extract and reclaim the initial extract of the solvent under reduced pressure;

[0038] (3) Heat and dissolve the obtained initial extract with ethanol, add purified water whose volume is 10 times the volume of the extract alcohol solution for extraction, then adjust its pH value to 2.3 with acid, leave it to stand, suction filter, and recover the solvent under reduced pressure Obtain the crude extract of proanthocyanidins;

[0039] (4) The obtained proanthocyanidin crude extract is adsorbed with a macroporous...

Embodiment example 3

[0044] Implementation case 3: a method for enriching and purifying proanthocyanidins in pine bark by means of batch distillation-macroporous adsorption resin coupling method, the steps are as follows:

[0045] (1) Pass 80 mesh sieves after the dried pine bark is pulverized, and extract by heating and refluxing with 75% ethanol with 15 times the volume of pine bark powder for 6 hours;

[0046] (2) Suction filtration of the pine bark extract treated in step (1) to obtain the extract and reclaim the initial extract of the solvent under reduced pressure;

[0047] (3) heating and dissolving the obtained initial extract with ethanol, adding purified water whose volume is 15 times the volume of the extract alcohol solution for extraction, then adjusting its pH value to 2.5 with acid, standing, suction filtration, and recovering the solvent under reduced pressure Obtain the crude extract of proanthocyanidins;

[0048] (4) The obtained proanthocyanidin crude extract is adsorbed on a m...

Technical field:

[0001] The invention belongs to the field of natural organic chemistry and relates to a method for purifying proanthocyanidins, in particular to a method for enriching and purifying proanthocyanidins in pine bark by using a batch distillation-macroporous adsorption resin coupling method. Background technique:

[0002] Pine bark extract is a class of substances extracted from pine bark. The pine bark stripped from the trees is collected, flattened and extracted. It contains a large amount of compounds called OPCs (proanthocyanidin oligomers). A large number of studies have proved that OPCs are effective antioxidants, non-toxic, non-mutagenic, non-carcinogenic and have no side effects. It is very safe to use. Pine bark has been proven to be a new source of OPCs. The OPCs extracted from pine bark have no difference in quality and function, but there are some slight differences in appearance.

[0003] The English name of Proanthocyanidins is Oligomeric Proan...

Examples

Embodiment 1

[0026] Embodiment 1: A kind of method that utilizes batch distillation-macroporous adsorption resin coupling method to enrich and purify proanthocyanidins in pine bark, its steps are as follows:

[0027] (1) Pass through a 60-mesh sieve after the dried pine bark is crushed, and extract by heating and refluxing with 10 times the volume of pine bark powder under reflux for 3 times, each for 2 hours;

[0028] (2) Suction filtration of the pine bark extract treated in step (1) to obtain the extract and reclaim the initial extract of the solvent under reduced pressure;

[0029] (3) Heat and dissolve the obtained primary extract with ethanol, add purified water with a volume 20 times the volume of the extract alcohol solution for extraction, then adjust its pH value to 2.0 with acid, leave it to stand, suction filter, and recover the solvent under reduced pressure Obtain the crude extract of proanthocyanidins;

[0030] (4) The obtained proanthocyanidin extract is adsorbed on a macr...

Embodiment example 2

[0035] Implementation case 2: a method for enriching and purifying proanthocyanidins in pine bark by means of batch distillation-macroporous adsorption resin coupling method, the steps are as follows:

[0036] (1) After the dry pine bark is pulverized, cross a 10-mesh sieve, and extract by heating and refluxing with 20 times the volume of pine bark powder under reflux for 4 hours;

[0037] (2) Suction filtration of the pine bark extract treated in step (1) to obtain the extract and reclaim the initial extract of the solvent under reduced pressure;

[0038] (3) Heat and dissolve the obtained initial extract with ethanol, add purified water whose volume is 10 times the volume of the extract alcohol solution for extraction, then adjust its pH value to 2.3 with acid, leave it to stand, suction filter, and recover the solvent under reduced pressure Obtain the crude extract of proanthocyanidins;

[0039] (4) The obtained proanthocyanidin crude extract is adsorbed with a macroporous...

Embodiment example 3

[0044] Implementation case 3: a method for enriching and purifying proanthocyanidins in pine bark by means of batch distillation-macroporous adsorption resin coupling method, the steps are as follows:

[0045] (1) Pass 80 mesh sieves after the dried pine bark is pulverized, and extract by heating and refluxing with 75% ethanol with 15 times the volume of pine bark powder for 6 hours;

[0046] (2) Suction filtration of the pine bark extract treated in step (1) to obtain the extract and reclaim the initial extract of the solvent under reduced pressure;

[0047] (3) heating and dissolving the obtained initial extract with ethanol, adding purified water whose volume is 15 times the volume of the extract alcohol solution for extraction, then adjusting its pH value to 2.5 with acid, standing, suction filtration, and recovering the solvent under reduced pressure Obtain the crude extract of proanthocyanidins;

[0048] (4) The obtained proanthocyanidin crude extract is adsorbed on a m...