A kind of method of extracting pycnogenols in the seed of Fructus Hippophae
Technical field
The present invention relates to the process for extracting of pycnogenols in the seed of Fructus Hippophae
Background technology
Pycnogenols is the general name of the extensive one big type of polyphenolic substance that exists in the vegetable kingdom.20 middle of century, French scientist Maas chief reins in and has at first found pycnogenols.Through nearly 50 years research, people improve constantly the understanding of pycnogenols pharmacological action.In recent years, a host of facts prove that pycnogenols is not only a kind of good antioxidant, and can regulate the crucial biological approach of body, participate in the many redox chain reaction process in the basic vital process.Experiment confirm, oligomeric procyanidolics has direct or indirect prevention, therapeutic action to nearly hundred kinds of damages and disease, has extensive use in fields such as healthcare products, medicine and makeup.
In numerous plants, grape is unfailing research topic always, at present, still is that raw material extracts pycnogenols both at home and abroad with the Semen Vitis viniferae.Research shows that seed of Fructus Hippophae is better pycnogenols source, because its extract contains more dimer, tripolymer, and dimer, the more single aggressiveness of tripolymer and polymer have stronger oxidation-resistance.The Semen Vitis viniferae extract composition is a pycnogenols, and monomer whose is a catechin, and mean polymerisation degree is lower.The sea buckthorn seed proanthocyanidins significantly different from the chemical structure of grape seed proanthocyanidins, mainly for the original prodelphinidin (monomer epigallocatechin), with an average degree of polymerization of 12.8.The effect of seed of Fructus Hippophae pycnogenols inhibited oxidation is better than grape pip procyanidin.
Summary of the invention
Technical problem to be solved by this invention is to unite to use the supercritical CO 2 abstraction technique to extract Seabuckthorm Seed Oil; Its seed dregs of rice adopt ultrasonic method to extract the seed of Fructus Hippophae procyanidin extract, adopt the dry three technology of microwave drying technology to extract the method for the pycnogenols in the sea-buckthorn seed cake.
For addressing the above problem, a kind of method of extracting pycnogenols in the seed of Fructus Hippophae of the present invention comprises the steps:
1. after the seed of Fructus Hippophae removal of impurities fragmentation, adopt supercritical CO
2Abstraction technique obtains the sea-buckthorn seed cake in low temperature (50 ℃) production process after extracting Seabuckthorm Seed Oil, and no solvent residue.
2. adopt ultrasonic method (50 ℃) to extract sea-buckthorn seed cake, get seed of Fructus Hippophae pycnogenols ethanol extract.
3. negative pressure low temperature reclaims edible ethanol, gets the pycnogenols aqueous solution.
4. promptly get the seed of Fructus Hippophae procyanidin extract after adopting vacuum microwave with pycnogenols aqueous solution drying, its procyanidin content can reach 50%.
The present invention compared with prior art has following advantage:
1, extract Seabuckthorm Seed Oil with solvent method, circumfluence method is extracted the pycnogenols in the sea-buckthorn seed cake, and the refining several situation of crude extract of spraying drying pycnogenols extracting solution and resin absorption are compared, and the present invention is an associating use supercritical CO
2Abstraction technique, ultrasonic method extractive technique, vacuum microwave drying technology; Its production process is in more all the time carries out under the low temperature; Avoided the influence of high temperature to the heat-sensitive substance pycnogenols as far as possible, simultaneously, supersound extraction and vacuum microwave drying not only carry out at low temperatures; Also shorten the time of production process greatly, also obviously reduced the loss of pycnogenols.The inventive method has been evaded the toxic action that resin possibly come off and bring fully without the refining crude extract of resin absorption.The real no solvent residue of seed of Fructus Hippophae procyanidin extract, high-content, high-quality that the inventive method obtains.And application for a patent for invention number: the method for 200810176033.6 method and " international sea-buckthorn research and development " the 8th volume the 3rd phase P11 page or leaf September in 2010; Procyanidin content all about 30%, can only adopt further refining its content that improves of resin again in the resulting seed of Fructus Hippophae procyanidin extract crude extract.Increase its production cost undoubtedly, also the risk of toxicity that resin wear brings possibly occur.
2, the present invention adopts vacuum microwave drying pycnogenols extracting solution, temperature low (below 50 ℃), time short (in 2 hours), and the quality product that obtains is fully suitable with cryodesiccated quality.And the spraying drying of application for a patent for invention numbers 200810176033.6, because temperature is high, the pycnogenols of thermo-sensitivity will inevitably significantly sacrificing; And the cryodesiccated time (extracting liquid measure on an equal basis) is more than 20 times of microwave drying time, and its production cost is more than 2.7 times of microwave drying production cost.
Embodiment
Embodiment 1: a kind of method of extracting pycnogenols in the seed of Fructus Hippophae comprises the steps:
1. adopt supercritical CO
2The sea-buckthorn seed cake 1kg of extraction behind the Seabuckthorm Seed Oil extracts 3 times through ultrasonic method down at 30 ℃ with 8L, 30% ethanolic soln, at every turn 0.35 hour extraction time.Merge No. three times extracting solution, cross with 200 order filter clothes and filter filtrating.Negative pressure low temperature reclaims edible ethanol, gets the seed of Fructus Hippophae pycnogenols aqueous solution.
2. get powdery seed of Fructus Hippophae procyanidin extract product 82g after the seed of Fructus Hippophae pycnogenols aqueous solution being adopted the vacuum microwave cryodrying, its procyanidin content is 49.6%.
Wherein: the 24L supercritical CO that sea-buckthorn seed cake adopts Guangzhou light industry to be produced
2Seed oil in the extraction plant extraction seed of Fructus Hippophae, its parameter is extraction temperature 45-50 ℃, extracting pressure is 26-32MPa, extraction time 2.5-3.5h.
Embodiment 2: a kind of method of extracting pycnogenols in the seed of Fructus Hippophae comprises the steps:
1. adopt supercritical CO
2The sea-buckthorn seed cake 10kg of extraction behind the Seabuckthorm Seed Oil extracts 2 times through ultrasonic method down at 50 ℃ with 100L, 80% ethanolic soln, at every turn 0.5 hour extraction time.Merge secondary raffinate, cross with 200 order filter clothes and filter filtrating.Negative pressure low temperature reclaims edible ethanol, gets the seed of Fructus Hippophae pycnogenols aqueous solution.
2. get powdery seed of Fructus Hippophae procyanidin extract product 0.95kg after the seed of Fructus Hippophae pycnogenols aqueous solution being adopted the vacuum microwave cryodrying, its procyanidin content is 50.6%.
Wherein: the 24L supercritical CO that sea-buckthorn seed cake adopts Guangzhou light industry to be produced
2Seed oil in the extraction plant extraction seed of Fructus Hippophae, its parameter is extraction temperature 45-50 ℃, extracting pressure is 26-32MPa, extraction time 2.5-3.5h.
Description of drawings
Accompanying drawing is a process diagram of the present invention.