CN103641870B - A kind of method extracting rutin from asparagus - Google Patents
A kind of method extracting rutin from asparagus Download PDFInfo
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- CN103641870B CN103641870B CN201310609225.2A CN201310609225A CN103641870B CN 103641870 B CN103641870 B CN 103641870B CN 201310609225 A CN201310609225 A CN 201310609225A CN 103641870 B CN103641870 B CN 103641870B
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Abstract
The present invention relates to the method extracting rutin from asparagus, be that to choose old stalk of asparagus be raw material, after soaking, clean, smashing to pieces, add ethanolic soln, extract flavonoid compound rutin wherein; Extraction of rutin liquid drips citric acid solution and carries out crystalline deposit after removing impurity after filtration; Precipitate and remove soluble impurity through washing, low-temperature vacuum drying, obtains rutin product.Present invention process is reasonable, and operation is simple and feasible, and production cost is low, and environmental pollution is little, and yield and the purity of rutin are high, greatly improve the added value of asparagus.
Description
Technical field
The present invention relates to the extraction of Flavonoid substances, especially a kind of method extracting rutin from asparagus.
Background technology
Rutin (Rutin), belongs to flavonoid compound, has another name called phytomelin, vitamin P, rutin; It not only has the effect reducing capillary permeability and fragility, can also keep and recover the normal elasticity of capillary vessel, can be used for the hemorrhage and purpura hemorrhagica of control hypertensive cerebral hemorrhage, diabetic retina etc., also can be used as food antioxidant and pigment, can also as the raw material of synthesis troxerutin.
Asparagus has another name called officinalis, Thallus Gracilariae, be rich in multiple amino acids, protein and VITAMIN, its content all higher than the l-asparagine in general fruits and vegetables, particularly asparagus and trace element-selenium, molybdenum, chromium, manganese etc., has adjustment organism metabolism, improve effect of body immunity, be that a kind of grade is held concurrently excellent famous and precious vegetables, there is abundant nutrition and higher pharmaceutical use, there is the laudatory title of " kings of vegetables ".Asparagus is mainly used in being processed into can and quick frozen product, and its processing period is annual 4 ~ June, and asparagus tissue fibrosis degree afterwards increases, and is not used further to processing, and allows its free growth, excavates in order to Second Year.China asparagus, after October, is just gathered in as bavin standing grain use, there is the deficiency that old stalk of asparagus utilization ratio is low.
According to the study, the rutin containing high-content in old stalk of asparagus.Research and develop a kind of method extracting rutin from asparagus, the production not being only rutin provides a new approach, and also for the utilization of old stalk of asparagus provides a new thinking, this has great importance for the added value improving old stalk of asparagus.
Summary of the invention
In order to overcome the deficiency that in prior art, old stalk of asparagus utilization ratio is low, the invention provides a kind of method extracting rutin from asparagus, this extracting method not only rational technology, operation is simple and feasible, production cost is low, and environmental pollution is little, the yield of rutin and purity high.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method extracting rutin from asparagus, is characterized in that: through following process steps:
A, raw material choose ripe, without disease and pest, the old stalk of asparagus of drying is raw material;
Old stalk of asparagus selected by step (a) is added the water soaking 3 ~ 4h of old stalk of asparagus quality 5 ~ 10 times by b, Feedstock treating, clear water is adopted to rinse well again, then send into the water that tissue mashing machine adds old stalk of asparagus quality 3 ~ 5 times and smash pulp to pieces, obtain asparagus slurries;
The asparagus slurries that step (b) obtains by c, alcohol extracting add old stalk of asparagus quality 10 ~ 15 times, concentration is the ethanolic soln of 65 ~ 75%, stir, be warming up to 70 ~ 80 DEG C, keep 3 ~ 4h, extract flavonoid compound rutin wherein, obtain Extraction of rutin liquid;
D, filter the Extraction of rutin liquid that step (c) obtained by 120 ~ 200 object filter clothes, remove asparagus small-particle and other insoluble impuritiess, obtain rutin filtered liquid;
Drip the citric acid solution that concentration is 0.3 ~ 0.5% gradually in e, heavy rutin filtered liquid step (d) obtained of acid, the pH value regulating rutin filtered liquid is 3.0 ~ 4.0, leaves standstill 2 ~ 3h, makes rutin crystallization wherein; Use 100 ~ 200 order filtered through gauze again, collect and obtain rutin precipitation;
F, wash and wash rutin that step (e) obtains precipitation with water 2 ~ 3 times, remove the impurity of solubility wherein, obtain highly purified rutin precipitation;
G, dry rutin precipitation step (f) obtained are sent in Vacuumdrier, and vacuum tightness-0.09 ~ 0.03kpa in the machine that keeps dry, temperature 35 ~ 60 DEG C, carries out low-temperature vacuum drying, obtains rutin product.
The present invention is that to choose old stalk of asparagus be raw material, adds ethanolic soln, is dissolved in ethanolic soln fully, up hill and dale by the rutin in raw material, the yield of rutin is improved after soaking, clean, smashing to pieces; Drip citric acid solution after removing impurity after filtration again and carry out crystalline deposit, precipitate and remove soluble impurity through washing, to improve its purity, after drying, obtain rutin product.Through measuring: the purity adopting this technical process to obtain rutin can reach more than 95%, the extraction yield of rutin is more than 4.5%.Present invention process is reasonable, and operation is simple and feasible, and production cost is low, and environmental pollution is little, and yield and the purity of rutin are high, greatly improve the added value of asparagus, and the utilization for old stalk of asparagus provides a new way.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details.
embodiment one
From asparagus, extract a method for rutin, it is characterized in that: through following process steps:
A, raw material choose ripe, without disease and pest, the old stalk of asparagus 100kg of drying is raw material, for subsequent use;
Old stalk of asparagus selected by step (a) is added the water soaking 3.5h of old stalk of asparagus quality 8 times by b, Feedstock treating, clear water is adopted to rinse well again, then send into the water that tissue mashing machine adds old stalk of asparagus quality 4 times and smash pulp to pieces, obtain asparagus slurries;
The asparagus slurries that step (b) obtains by c, alcohol extracting add old stalk of asparagus quality 12 times, concentration is the ethanolic soln of 70%, stirs, is warming up to 75 DEG C, keeps 3.5h, extract flavonoid compound rutin wherein, obtain Extraction of rutin liquid;
D, filter the Extraction of rutin liquid that step (c) obtained by 150 object filter clothes, remove asparagus small-particle and other insoluble impuritiess, obtain rutin filtered liquid;
Drip the citric acid solution that concentration is 0.4% gradually in e, heavy rutin filtered liquid step (d) obtained of acid, the pH value regulating rutin filtered liquid is 3.5, leaves standstill 2.5h, makes rutin crystallization wherein; Use 150 order filtered through gauze again, collect and obtain rutin precipitation;
F, wash and wash rutin that step (e) obtains precipitation with water 3 times, remove the impurity of solubility wherein, obtain highly purified rutin precipitation;
G, dry rutin precipitation step (f) obtained are sent in Vacuumdrier, and vacuum tightness 0.01kpa in the machine that keeps dry, temperature 50 C, carries out low-temperature vacuum drying, obtains rutin 4.86kg.After measured, the purity of this rutin reaches 96.83%.
embodiment two
From asparagus, extract a method for rutin, it is characterized in that: through following process steps:
A, raw material choose ripe, without disease and pest, the old stalk of asparagus 200kg of drying as raw material, for subsequent use;
Old stalk of asparagus selected by step (a) is added the water soaking 3h of old stalk of asparagus quality 10 times by b, Feedstock treating, then adopts clear water to rinse well, then sends into the water that tissue mashing machine adds old stalk of asparagus quality 5 times and smashs pulp to pieces, obtain asparagus slurries;
The asparagus slurries that step (b) obtains by c, alcohol extracting add old stalk of asparagus quality 15 times, concentration is the ethanolic soln of 65%, stirs, is warming up to 70 DEG C, keeps 4h, extract flavonoid compound rutin wherein, obtain Extraction of rutin liquid;
D, filter the Extraction of rutin liquid that step (c) obtained by 200 object filter clothes, remove asparagus small-particle and other insoluble impuritiess, obtain rutin filtered liquid;
Drip the citric acid solution that concentration is 0.5% gradually in e, heavy rutin filtered liquid step (d) obtained of acid, the pH value regulating rutin filtered liquid is 3.0, leaves standstill 2h, makes rutin crystallization wherein; Use 200 order filtered through gauze again, collect and obtain rutin precipitation;
F, wash and wash rutin that step (e) obtains precipitation with water 2 times, remove the impurity of solubility wherein, obtain highly purified rutin precipitation;
G, dry rutin precipitation step (f) obtained are sent in Vacuumdrier, and vacuum tightness 0.03kpa in the machine that keeps dry, temperature 60 C, carries out low-temperature vacuum drying, obtains rutin product 9.12kg.After measured, the purity of this rutin reaches 95.44%.
embodiment three
From asparagus, extract a method for rutin, it is characterized in that: through following process steps:
A, raw material choose ripe, without disease and pest, the old stalk of asparagus 100kg of drying as raw material, for subsequent use;
Old stalk of asparagus selected by step (a) is added the water soaking 4h of old stalk of asparagus quality 5 times by b, Feedstock treating, then adopts clear water to rinse well, then sends into the water that tissue mashing machine adds old stalk of asparagus quality 3 times and smashs pulp to pieces, obtain asparagus slurries;
The asparagus slurries that step (b) obtains by c, alcohol extracting add old stalk of asparagus quality 10 times, concentration is the ethanolic soln of 75%, stirs, is warming up to 80 DEG C, keeps 3h, extract flavonoid compound rutin wherein, obtain Extraction of rutin liquid;
D, filter the Extraction of rutin liquid that step (c) obtained by 120 object filter clothes, remove asparagus small-particle and other insoluble impuritiess, obtain rutin filtered liquid;
Drip the citric acid solution that concentration is 0.3% gradually in e, heavy rutin filtered liquid step (d) obtained of acid, the pH value regulating rutin filtered liquid is 4.0, leaves standstill 3h, makes rutin crystallization wherein; Use 100 order filtered through gauze again, collect and obtain rutin precipitation;
F, wash and wash rutin that step (e) obtains precipitation with water 3 times, remove the impurity of solubility wherein, obtain highly purified rutin precipitation;
G, dry rutin precipitation step (f) obtained are sent in Vacuumdrier, and vacuum tightness-0.09kpa in the machine that keeps dry, temperature 35 DEG C, carries out low-temperature vacuum drying, obtains rutin product 4.73kg.After measured, the purity of this rutin reaches 95.64%.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (1)
1. from asparagus, extract a method for rutin, it is characterized in that: through following process steps:
A, raw material choose ripe, without disease and pest, the old stalk of asparagus of drying is raw material;
Old stalk of asparagus selected by step (a) is added the water soaking 3 ~ 4h of old stalk of asparagus quality 5 ~ 10 times by b, Feedstock treating, clear water is adopted to rinse well again, then send into the water that tissue mashing machine adds old stalk of asparagus quality 3 ~ 5 times and smash pulp to pieces, obtain asparagus slurries;
The asparagus slurries that step (b) obtains by c, alcohol extracting add old stalk of asparagus quality 10 ~ 15 times, concentration is the ethanolic soln of 65 ~ 75%, stir, be warming up to 70 ~ 80 DEG C, keep 3 ~ 4h, extract flavonoid compound rutin wherein, obtain Extraction of rutin liquid;
D, filter the Extraction of rutin liquid that step (c) obtained by 120 ~ 200 object filter clothes, remove asparagus small-particle and other insoluble impuritiess, obtain rutin filtered liquid;
Drip the citric acid solution that concentration is 0.3 ~ 0.5% gradually in e, heavy rutin filtered liquid step (d) obtained of acid, the pH value regulating rutin filtered liquid is 3.0 ~ 4.0, leaves standstill 2 ~ 3h, makes rutin crystallization wherein; Use 100 ~ 200 order filtered through gauze again, collect and obtain rutin precipitation;
F, wash and wash rutin that step (e) obtains precipitation with water 2 ~ 3 times, remove the impurity of solubility wherein, obtain highly purified rutin precipitation;
G, dry rutin precipitation step (f) obtained are sent in Vacuumdrier, and vacuum tightness-0.09 ~ 0.03kpa in the machine that keeps dry, temperature 35 ~ 60 DEG C, carries out low-temperature vacuum drying, obtains rutin product.
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Citations (5)
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|---|---|---|---|---|
| DE19850282A1 (en) * | 1998-10-30 | 2000-05-04 | Merck Patent Gmbh | Preparation of new or known tris-hydroxyalkyl quercetin and isoquercetin derivatives by enzymatic cleavage of rutin derivatives, used e.g. as nutritional supplements, cosmetic UV filters or cardiovascular drugs |
| CN1546506A (en) * | 2003-12-04 | 2004-11-17 | 国家海洋局第一海洋研究所 | Method for preparing asparagus rutin |
| CN101422201A (en) * | 2008-11-18 | 2009-05-06 | 长春工业大学 | Natural compound antioxidant for fat-rich food |
| CN102532333A (en) * | 2011-09-30 | 2012-07-04 | 福建惠泽生物科技有限公司 | Method for comprehensively extracting active substances from asparagus scraps based on multi-stage membrane separation |
| CN102718820A (en) * | 2012-07-10 | 2012-10-10 | 刘志强 | Method for extracting and refining rutin |
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2013
- 2013-11-27 CN CN201310609225.2A patent/CN103641870B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19850282A1 (en) * | 1998-10-30 | 2000-05-04 | Merck Patent Gmbh | Preparation of new or known tris-hydroxyalkyl quercetin and isoquercetin derivatives by enzymatic cleavage of rutin derivatives, used e.g. as nutritional supplements, cosmetic UV filters or cardiovascular drugs |
| CN1546506A (en) * | 2003-12-04 | 2004-11-17 | 国家海洋局第一海洋研究所 | Method for preparing asparagus rutin |
| CN101422201A (en) * | 2008-11-18 | 2009-05-06 | 长春工业大学 | Natural compound antioxidant for fat-rich food |
| CN102532333A (en) * | 2011-09-30 | 2012-07-04 | 福建惠泽生物科技有限公司 | Method for comprehensively extracting active substances from asparagus scraps based on multi-stage membrane separation |
| CN102718820A (en) * | 2012-07-10 | 2012-10-10 | 刘志强 | Method for extracting and refining rutin |
Non-Patent Citations (2)
| Title |
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| 芦笋中芦丁的提取及其鉴定;刘树兴，等;《食品工业科技》;20010831;第22卷(第04期);39-41 * |
| 芦笋老茎中芦丁的提取工艺;刘树兴，等;《食品与发酵工业》;20051231;第31卷(第12期);143-145 * |
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