CN100560578C - A kind ofly be used to prevent and treat asthenopic plant milk extract and preparation and preparation method - Google Patents
A kind ofly be used to prevent and treat asthenopic plant milk extract and preparation and preparation method Download PDFInfo
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Abstract
The invention provides a kind of preparation method who is used to prevent and treat asthenopic plant milk extract preparation.Its main technical points is to reach more than 50% with the efficient part content that grape waste residue (Semen Vitis viniferae, Pericarpium Vitis viniferae and stem of Fructus Vitis viniferae or their mixture) prepares Semen Vitis viniferae, and wherein monomer effective constituent catechin content is the preparation of feedstock production in the 0.5-20% scope.The present invention with the grape waste residue be that efficient part that raw material obtains Semen Vitis viniferae makes that preparation, cost are low, technology advantages of simple, the original structure that has kept efficient part and activity, the extract of Semen Vitis viniferae can be made into to be used to prevent and treat asthenopic any medicinal and healthcare products formulation, and it is applied to prevent and treat asthenopic medical treatment, healthcare field.
Description
Technical field:
The present invention relates to a kind of plant milk extract and preparation and preparation method, particularly a kind of control asthenopic grape waste residue extract and preparation and preparation method.
Technical background:
Asthenopia is to produce because of autonomous effort that visual organ attempts to obtain with insufficient adjusting clear vision, as blurring of vision, eye expand, syndromes such as ophthalmodynia, headache, aching shoulder and back and tired spirit.Along with the high speed development of information age and the quickening of rhythm of life, especially video display terminal (vdt)s (VDT) such as computer, TV, game machine, watch-dog incorporate in people's work, study and the family life gradually, asthenopia has become present ophthalmology common disease, has seriously influenced people's life.It is not a disease independently, but because one group of fatigue syndrome that a variety of causes causes claims the visual fatigue syndromes again.At present, the physiatrics of treatment has prism rectification, operative treatment, acupuncture etc.; Chemicals adopts neostigmine such as beta-blocker, vancomin etc. more, and neurotrophic agents and tranquilizer etc.But above treatment is all carried out at symptom, does not reach basic therapeutic purpose.Modern study finds, natural drug and Chinese medicine are should disease evident in efficacy, just progressively becomes patient's first-selected medicine.
The oligomeric procyanidolics that is rich in the grape (Oligomeric Proanthocyanidins, be called for short OPCs) is the polyphenols that monomer, dimer, the tripolymer by catechin is formed by combining.As far back as the seventies French scientist just find that Semen Vitis viniferae is a best resource of extracting pycnogenols, procyanidin content can be up to 95% in its extract.The grape resource of China is abundant, tankage grape waste residue after the annual only brew grape wine is about 8000t just, and in recent years the cultivated area of grape also in a large amount of increases, yet domestic only with it as simple raisin seed oil, feed, fertilizer and the polyphenol raw material of extracting.Discover and have significant oxidation-resistance by OPCs (its resistance of oxidation is V
C20 times, V
E50 times), remove interior free yl ability, improve unique effects such as microcirculation in human body obstacle, fields such as health care have been applied at present, especially can reduce retinopathy, control capillary hemorrhage aspect the eye health, it is the asthenopic desirable natural drug of treatment, its product is owing to meet the hope and the requirement of modern people's back to nature, and market outlook are very wide.
The method that is used to extract grape Central Plains anthocyan material at present has: the one, and chemical solvents method, the 2nd, supercritical fluid extraction, the 3rd, microwave extraction method.
Chinese patent such as CN03137933.8 adopt ethyl acetate, sherwood oil or the trichloromethane organic solvent method as the extraction solvent of Semen Vitis viniferae; CN00134314.9 is that cyanine oligomer has been invented a kind of water in the Semen Vitis viniferae, alcohol extracting is followed the example of; CN99111574.0 is raw material with the Semen Vitis viniferae, uses supercutical fluid method extraction of oil from grape seeds and cyanine oligomer; CN00120353.3 discloses a kind of novel method that adopts microwave method to extract the anthocyan material in the Semen Vitis viniferae.
Said extracted method or technology make moderate progress to the traditional preparation process method, but remaining in the improved problem that needs to be resolved hurrily aspect quality controlling means and the preparation technology, as exist impurity many, contain a large amount of carbohydrates and contain moisture absorption compositions such as a certain amount of inorganic salt and phlegmatic temperament; Organic solvents such as the acetone that uses in the leaching process, ethyl acetate, sherwood oil, not only cost height, dangerous big, contaminate environment, and cause the organic solvent residual excess, influence quality product and drug effect.Though CN00134314.9 has adopted free of contamination water and alcohol, efficient part is indeterminate, and yield is lower; And supercutical fluid method cost is higher, and treatment step is also comparatively loaded down with trivial details.
OPCs improves microcirculation in human body, removes free radical, anti-oxidant be the basic substance of its disease-prevention health effect, be widely used in every field as the product that has much DEVELOPMENT PROSPECT.Chinese patent such as CN00121388.1 disclose a kind of grape seed extract OPC s strong anti-oxidative composite capsule and manufacture method thereof, are to have the complex health care product that delays senility, regulates body's immunity; CN02159540.2 is to be anti-ageing, anticancer, anti-oxidant, as to improve the capsule of aspects such as the cardiovascular and cerebrovascular patent that is used for of raw material with the Semen Vitis viniferae extract, does not have clear and definite single-minded therapeutic purpose.As seen, also do not use modern extraction technique and quality controlling means at present and the grape waste residue is made the patented invention that is used to prevent and treat (standard extract) pharmaceutical preparation of asthenopic modern times.
Summary of the invention:
The objective of the invention is, shortcoming such as efficient part indeterminate and mechanism unclear, no crude drug, intermediate and final product quality control method big, a kind of control asthenopic grape waste residue extract and preparation and preparation method are provided at the taking dose that exists in the above-mentioned technology.Is standard extract with OPCs content in the grape waste residue greater than 50% efficient part, and make and be used to prevent and treat asthenopic modern preparation, it can solve the medium-term and long-term insoluble technical field problem of grape waste residue preparation technology, has filled up that grape waste residue extract OPC s is developed to the domestic blank that is used for the treatment of asthenopic preparation.
The object of the present invention is achieved like this: the efficient part of grape waste residue extract is the flavones of grape waste residue and Polyphenols composition through the effect experiment screening, oligopolymer comprising flavanol compound and pycnogenols, total content is at 50%-99%, through the further preferred efficient part of effect experiment is OPCs, and its content is at 50%-99%.Through the preferred effective constituent of effect experiment is wherein catechin, and its content is in the 0.5-20% scope.
The technical problem to be solved in the present invention provides a kind of employing resin absorption technology, extracts the OPCs method from the grape waste residue.
The preparation method of efficient part of the present invention, step is as follows:
(1) with grape waste residue extracting in water 1-10 time, the 2-20 that each consumption is respectively medicinal material weight doubly, extraction time is 0.5-10 hour, extracting temperature is 10-100 ℃, united extraction liquid.
(2) with the grape waste residue with 5-95% alcohol reflux 1-10 time, the 2-20 that each consumption is respectively medicinal material weight doubly, extraction time is 0.5-10 hour, united extraction liquid filters, and reclaims ethanol, concentrated medicinal extract.
(3) with the extracting solution of (1) or (2) medicinal extract after adding water 1-200 and doubly diluting, last resin column absorption, the volume ratio of raw material weight and resin is 1: 0.5-10, resin column footpath is 1 with the post height ratio: 1-30, with the pH value be water washing, the concentration of 2-8 be 5-95% ethanolic soln wash-out, flow velocity be 0.5-3.5 column volume/hour.
(4) collect ethanol eluate, in the ratio adding discoloring agent of effluent volume 1-30%, reflux 0.1-10 hour, filter, concentrating under reduced pressure, vacuum-drying, promptly.OPCs content can reach more than 50% in employing this law grape waste residue.
OPCs resin extraction process of the present invention is compared with traditional technology, and following 3 advantages are arranged:
1. dwindle dosage, improve bulk drug inner quality and preparation level.The refining thing that obtains after RAT handles can make effective component highly enriched, and impurity is few, and extraction yield only is the 2-5% of crude drug in whole (decocting method is about 20-30%, and alcohol deposition method is about 15%), helps making the Chinese medicine of modern formulation, also is convenient to quality control.This technology has once been finished removal of impurities and concentrated two procedures.
2. reduce the moisture absorption of product.The medicine major part of traditional technology preparation has stronger moisture absorption, is the medium-term and long-term difficult problem that exists of products production and storage.And after RAT handles, can remove moisture absorption compositions such as carbohydrates a large amount of in the decocting liquid, inorganic salt, lymphatic temperament effectively, and help the production of multiple formulation, strengthen the stability of product.
3.RAT can shorten the production cycle, required equipment is simple, has removed many operations consuming time such as staticly settling, concentrate from.Not only saved packing, reduced cost, also created condition for Chinese medicine enters the world market.
The present invention compares with traditional solvent extration, supercutical fluid method, technology is simple, do not use the volatile organic solvent of toxicity in the technical process, safe and reliable, production cost is low, environmentally safe.
Standard extract of the present invention is to make medicinal various clinical acceptable forms, comprise capsule, tablet, powder, granule, oral liquid, vina, pill, pellet, capsule and pill, ointment, mixture, tincture, injection etc., wherein preparations such as soft capsule, pill, oral liquid, eye drop preferably.
The standard extract that grape waste residue of the present invention obtains according to its preparation method can directly be made preparation or be mixed and made into preparation with the medicine acceptable carrier.Described medicine acceptable carrier can be: starch, sucrose, lactose, mannitol, silicon derivative, cellulose family and derivative, alginate, gelatin, polyvinylpyrrolidone, glycerine, tween-80, agar, lime carbonate, Calcium hydrogen carbonate, tensio-active agent, polyoxyethylene glycol, cyclodextrin, dextrin, phospholipid material, kaolin, talcum powder, calcium stearate, Magnesium Stearate etc.
Standard extract of the present invention and composition are to have functions such as microcirculation improvement, oxidation-resistance, elimination interior free yl, enhancing body immunizing power, are applied in preparation asthenopic medicine of control and healthcare products.
Embodiment:
The present invention will be further described below in conjunction with embodiment
Embodiment 1: a kind of RAT preparation method of grape waste residue
Raw material adopts the grape waste residue, and with 50% alcohol reflux 2 times, each consumption is 7,5 times of crude drug weight, and extraction time is 2,1 hours, and united extraction liquid filters, and reclaims ethanol, concentrated medicinal extract.Medicinal extract is added 120 times of dilutions of water, the absorption of last resin column, the volume ratio of raw material weight and resin is 1: 3, resin column footpath and post height ratio are 1: 15, water washing, the 50% ethanolic soln wash-out of usefulness pH=6, flow velocity be 1 column volume/hour.
Collect ethanol eluate, press effluent volume 5% and add discoloring agent, reflux 3 hours filters, concentrating under reduced pressure, and vacuum-drying, promptly.OPCs content can reach more than 50% in employing this law grape waste residue.
Embodiment 2: a kind of RAT preparation method of grape waste residue
Raw material adopts the grape waste residue, and with 60% alcohol reflux 3 times, each consumption is 8,6,4 times of raw medicinal herbs weight, and extraction time is 60,45,30min, and united extraction liquid filters, and reclaims ethanol, concentrated medicinal extract.Medicinal extract is added 150 times of dilutions of water, the absorption of last resin column, raw material heavy with volume ratio resin be 1: 5, resin column through with the post height ratio be 1: 20, with water washing, the 60% ethanolic soln wash-out of pH=8, flow velocity be 2 column volumes/hour.Elutriant is through concentrating under reduced pressure, vacuum-drying, promptly.OPCs content can reach more than 50% in employing this law grape waste residue.
Embodiment 3:OPCs is greater than 50% grape waste residue extract (standard extract) soft capsule and the preparation of dripping pill
Get OPCs greater than the capsule material that 50% grape waste residue extract and gelatin make, adopt pressing pill, typing, drying, select ball, wash ball, make soft capsule; Adopt the dropping method pill, through typing, dry, select ball, wash ball, make dripping pill.Soft capsule that makes and dropping pill formulation OPCs content should be more than 50%.
The toxicity clinical trial
Below further prove the curative effect and the security of standard extract of the present invention and composition by clinical and toxicological test.
The experimental drug thing: standard extract of the present invention does not add the preparation that auxiliary material directly makes and is called in test OPCs.
Test example 1: the asthenopic clinical observation I of the treatment of pharmaceutical composition of the present invention
Treatment is divided into 2 groups owing to accommodative asthenopia patient 156 examples of long-term close eye, each 78 people.One winding is subjected to OPCs pharmacological agent, a course of treatment (one month); Another group only adopts composite treatment such as correction of refractive errors, the treatment of Pilocarpin eye drop eye droppings etc. for control group, efficiently is respectively 92%, 36%.
Test example 2: the asthenopic clinical observation II of the treatment of pharmaceutical composition of the present invention
Treatment is engaged in computer operation, is surfed the Net, sees TV for a long time, VDT asthenopia disease patient 90 examples such as play games, and is equally divided into 2 groups, and a winding is subjected to the treatment of OPCs, and another group is control group, adopts general treatement.After 60 days, the contrast susceptibility of 45 patient's eyes of treatment group has clear improvement than control group, cures 42 examples, 3 examples that take a turn for the better, efficient 93%.
Test example 3: the safety evaluation of pharmaceutical composition of the present invention
Get 42 of Wistar kind rat, mouse respectively, body weight 85-120g, oral OPCs50mg/kgd, continuous 6 months.Observe general drug reaction, detect indexs such as hematology, blood biochemical and histopathology.After 6 months, compare through every inspection and physiology and to have no significant change, without any side effects, and tolerance is good, no teratogenesis, mutagenesis, LD
50All more than 4500.
The result of the standard extract of grape waste residue and clinical observation of composition for preventing and controlling asthenopia and safety evaluation shows, standard extract of the present invention and preparation determined curative effect, mechanism is clear, have no adverse reaction, and proves that standard extract and preparation that the present invention makes are effective, safe and reliable.
Claims (4)
1, a kind of preparation method who is used to prevent and treat asthenopic plant milk extract, it is characterized in that: this method steps is as follows:
(1) with grape waste residue extracting in water 1-10 time, the 2-20 that each consumption is respectively medicinal material weight doubly, extraction time is 0.5-10 hour, extracting temperature is 10-100 ℃, united extraction liquid;
Or with the grape waste residue with 5-95% alcohol reflux 1-10 time, the 2-20 that each consumption is respectively medicinal material weight doubly, extraction time is 0.5-10 hour, united extraction liquid filters, and reclaims ethanol, concentrated medicinal extract;
(2) with the extracting solution of (1) or add medicinal extract after water 1-200 doubly dilutes, last resin column absorption, the volume ratio of raw material weight and resin is 1: 0.5-10, the resin column footpath is 1 with the post height ratio: 1-30, with the pH value be water washing, the concentration of 2-8 be 5-95% ethanolic soln wash-out, flow velocity be 0.5-3.5 column volume/hour, described resin is the resin by the polystyrene series of polystyrene series, modification and iso-butylene series synthetic opposed polarity, different model;
(3) collect ethanol eluate, in the ratio adding discoloring agent of effluent volume 1-30%, reflux 0.1-10 hour, filter, concentrating under reduced pressure, vacuum-drying, promptly; OPCs content reaches more than 50% in employing this law grape waste residue.
2, the preparation method who is used to prevent and treat asthenopic plant milk extract according to claim 1 is characterized in that: prepared extract directly or with pharmaceutically acceptable carrier is mixed and made into preparation.
3, a kind of preparation method who is used to prevent and treat asthenopic plant milk extract according to claim 2, it is characterized in that: described preparation is capsule, tablet, powder, granule, oral liquid, vina, pill, ointment, mixture, tincture, injection.
4, a kind of preparation method who is used to prevent and treat asthenopic plant milk extract according to claim 3, it is characterized in that: described pill comprises pellet and capsule and pill.
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| CN100560578C true CN100560578C (en) | 2009-11-18 |
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Families Citing this family (7)
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| CN102086185B (en) * | 2009-12-02 | 2013-05-08 | 中国科学院生物物理研究所 | Oligomeric proanthocyanidins and method for extracting same |
| CN101703635B (en) * | 2009-12-03 | 2012-08-08 | 应维强 | Production technology of grape pip and grape skin extract |
| CN101999493B (en) * | 2010-12-08 | 2013-07-31 | 费维来 | Preparation method of plant health-care cool tea |
| CN105669780A (en) * | 2016-01-14 | 2016-06-15 | 张敬明 | Method for raising polyphenol content and water-solubility of grape seed extract |
| CN108618137A (en) * | 2018-07-18 | 2018-10-09 | 深圳极醇健康产业股份有限公司 | A kind of lycopene capsules and preparation method thereof |
| CN108887678A (en) * | 2018-07-18 | 2018-11-27 | 深圳极醇健康产业股份有限公司 | A kind of tomato red plain piece and preparation method thereof |
| CN113712957A (en) * | 2021-08-19 | 2021-11-30 | 温州医科大学附属眼视光医院 | Preparation method and application of oligomeric proanthocyanidins ophthalmic product |
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| CN1506362A (en) * | 2002-12-06 | 2004-06-23 | 沈阳中科药业公司 | Resin process of extracting proanthocyanidin from graup seed |
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