CN109806295A - A kind of resin adsorption technology for extracting oligomeric pyrroles alkane carboxylic acid from fig - Google Patents

Abstract

The present invention provides a kind of resin adsorption technologies that oligomeric pyrroles alkane carboxylic acid is extracted from fig.Its main technical points is that the active component content that fig seed is prepared with fig waste residue (fig seed, fig skin and fig stalk or their mixture) reaches 50% or more, and wherein monomer effective component catechin content is the preparation of raw material preparation within the scope of 0.5-20%.The present invention using fig waste residue as the active component that raw material obtains fig seed be made preparation, at low cost, simple process rationally, maintain the original structure and activity of active component, the extract of fig seed can be made for any medicinal and health care product dosage form of prevention and treatment asthenopia, be applied to medical treatment, the healthcare field of prevention and treatment asthenopia.

Description

A kind of resin adsorption technology for extracting oligomeric pyrroles alkane carboxylic acid from fig

Technical field

The present invention relates to a Plant Extracts and preparation and preparation methods, especially a kind of to extract oligomeric pyrrole from fig Cough up the resin adsorption technology of alkane carboxylic acid.

Background technique

The oligomeric pyrroles alkane carboxylic acid (Oligomeric Proanthocyanidins, abbreviation PCA) being rich in fig is The polyphenols being formed by combining by the monomer, dimer, tripolymer of catechin.Early in the seventies French scientist find that Fig seed is the best resource for extracting pyrrolidine carboxylic acid, and extract procyanidins content may be up to 95%.The nothing in China Flowers and fruits are resourceful, be often only the leftover bits and pieces fig waste residue just about 8000t after brewing fig wine, and fig in recent years Cultivated area is also largely increasing, however it is domestic only it is used as simple extract fig seed oil, feed, fertilizer and more Phenol raw material.Research finds that (its oxidation resistance is V to PCA with significant inoxidizability_C20 times, V_E50 times), remove it is internal The ability of free radical improves the unique effects such as microcirculation in human body obstacle, has been applied to the fields such as health care at present, especially in eye Portion health aspect can reduce retinopathy, prevention and treatment capillary hemorrhage, be treat visual fatigue ideal natural drug, product due to Meet the hope and requirement of modern people's back to nature, market prospects are very wide.

Method currently used for extracting pyrrolidine carboxylic acid's substance in fig has: first is that chemical-solvent method, second is that super face Boundary's fluids extraction, third is that microwave loss mechanisms.

Chinese patent such as CN03137933.8, using ethyl acetate, petroleum ether or chloroform mentioning as fig seed Take the organic solvent method of solvent；CN00134314.9 is that pyrrolidine carboxylic acid's oligomer has invented a kind of water, alcohol extracting in fig seed It follows the example of；CN99111574.0 is using fig seed as raw material, using supercritical fluid method extraction fig seed oil and pyrrolidine carboxylic acid Oligomer；CN00120353.3 discloses a kind of new method using the anthocyan substance in multistage microwave amplifier grape pip.

Said extracted method or technique make moderate progress to traditional preparation methods, but in method of quality control and preparation process side Face still has the problem of improvement urgently to be resolved, such as there is that impurity is more, containing a large amount of carbohydrates and contains a certain amount of inorganic salts and viscous The moisture absorptions composition such as liquid matter；The organic solvents such as acetone, ethyl acetate used in extraction process, petroleum ether, it is not only at high cost, dangerous Greatly, environment is polluted, and causes organic solvent residual excess, influences product quality and drug effect.Although CN00134314.9 is used Free of contamination water and alcohol, but active component is indefinite, and yield is lower；And supercritical fluid method cost is higher, processing step It is rapid also relatively complicated.

PCA improve microcirculation in human body, remove free radical, it is anti-oxidant be its disease-prevention health effect material base, as quite The product of tool development prospect is widely used to every field.Chinese patent such as CN00121388.1 discloses a kind of fig seed Extract PCA strong anti-oxidative composite capsule and its manufacturing method are that the compound with the body's immunity that delays senescence, adjusts is protected Strong product；It is raw material for anti-aging, anticancer, anti-oxidant, improvement heart and brain blood that CN02159540.2, which is using fig seed extract, The patent of the capsule of pipe etc., not clearly single-minded therapeutic purposes.As it can be seen that there is presently no apply modern extraction technique Fig waste residue is made to the patent for being used to prevent and treat modern times (standard extract) pharmaceutical preparation of asthenopia with method of quality control Invention.

Summary of the invention

The purpose of the present invention is taking dose is big, active component is indefinite and mechanism is unclear present in view of the above technology Chu, without crude drug, intermediate and final product quality control method the disadvantages of, provide and a kind of extract oligomeric pyrroles alkane carboxylic acid from fig Resin adsorption technology.Active component using PCA content in fig waste residue greater than 50% is made and is used for as standard extract The Modern preparations of asthenopia are prevented and treated, it can solve long-term insoluble technical field in fig waste residue preparation process and asks Topic has filled up the domestic blank by fig waste residue extract PCA exploitation at the preparation for being used to treat asthenopia.

The object of the present invention is achieved like this: the active component of fig waste residue extract is nothing through effect experiment screening The flavones and polyphenol components of flowers and fruits waste residue, including the oligomer of flavanol compound and pyrrolidine carboxylic acid, total content is in 50%- 99%, it is PCA through the further preferred active component of effect experiment, content is in 50%-99%.It is preferred through effect experiment Effective component is catechin therein, and content is within the scope of 0.5-20%.

The technical problem to be solved in the present invention is to provide a kind of resin adsorption that oligomeric pyrroles alkane carboxylic acid is extracted from fig Technology.

The preparation method of active component of the invention, steps are as follows:

(1) by fig waste residue extracting in water 1-10 times, each dosage is respectively 2-20 times of medicinal material weight, extraction time It is 0.5-10 hours, Extracting temperature is 10-100 DEG C, combined extract.

(2) fig waste residue 5-95% reflow of alcohol is extracted 1-10 times, each dosage is respectively the 2- of medicinal material weight 20 times, extraction time is 0.5-10 hours, combined extract, filtering, and recovered alcohol is concentrated to give medicinal extract.

(3) by the extracting solution of (1) or add (2) medicinal extract after 1-200 times of water dilution, the absorption of upper resin column, raw material weight with The volume ratio of resin is 1: 0.5-10, and resin column diameter and pillar height ratio are 1: 1-30, with pH value be 2-8 water washing, concentration 5- The elution of 95% alcoholic solution, flow velocity are 0.5-3.5 column volume/hour.

(4) alcohol eluent is collected, decolorising agent is added in the ratio of effluent volume 1-30%, it is small to be heated to reflux 0.1-10 When, filter, be concentrated under reduced pressure, vacuum drying to get.Using PCA content in this law fig waste residue up to 50% or more.

PCA resin extraction process of the invention has following 3 advantages compared with traditional handicraft:

1. reducing dosage, bulk pharmaceutical chemicals inherent quality and preparation level are improved.The refined substance obtained after RAT is handled can make medicine Imitate that ingredient is highly enriched, and impurity is few, recovery rate is only that (decocting method is 20-30% or so, and alcohol deposition method is by the 2-5% of crude drug in whole 15% or so), be conducive to the Chinese medicine that modern formulation is made, be also convenient for quality control.The technique once completes removal of impurities and concentration Two procedures.

2. reducing the moisture absorption of product.The drug of traditional handicraft preparation largely has stronger moisture absorption, is that product is raw Long-term existing problem in producing and storing.And after RAT is handled, can be effectively removed in decocting liquid a large amount of carbohydrate, inorganic salts, The moisture absorbing components such as lymphatic temperament are conducive to the production of a variety of dosage forms, enhance the stability of product.

3.RAT can be shortened the production cycle, and required equipment is simple, eliminate the process staticly settle, be concentrated etc. more than time-consuming.No But packaging is saved, cost is reduced, has also entered international market for Chinese medicine and creates condition.

The present invention is compared with traditional solvent extraction, supercritical fluid method, without using poison in simple process, process flow Property volatile organic solvent, safe and reliable, production cost is low, no pollution to the environment.

Standard extract of the invention be can be made into medicinal various clinically-acceptable dosage forms, including capsule, tablet, Powder, granule, oral solution, vina, pill, micropill preparation, capsule and pill, ointment, mixture, tincture, injection etc., wherein preferably For preparations such as soft capsule, pill, oral solution, eye drops.

The standard extract that fig waste residue of the invention is obtained according to preparation method can be directly prepared into preparation or and drug Acceptable carrier is mixed and made into preparation.The pharmaceutically acceptable carrier may is that starch, sucrose, lactose, mannitol, Silicon derivative, cellulose family and derivative, alginates, gelatin, polyvinylpyrrolidone, glycerol, Tween-80, agar, carbonic acid Calcium, calcium bicarbonate, surfactant, polyethylene glycol, cyclodextrin, dextrin, phospholipid material, kaolin, talcum powder, stearic acid Calcium, magnesium stearate etc..

Standard extract and composition of the invention is that have improve microcirculation, inoxidizability, eliminate interior free yl, increase The functions such as strong immunity of organisms, applied in the drug and health care product of preparation prevention and treatment asthenopia.

Specific embodiment

Below with reference to embodiment, the present invention will be further described

A kind of embodiment 1: resin adsorption technology for extracting oligomeric pyrroles alkane carboxylic acid from fig

Raw material uses fig waste residue, is extracted 2 times with 50% reflow of alcohol, and each dosage is 7,5 times of crude drug weight, Extraction time is 2,1 hours, combined extract, filtering, and recovered alcohol is concentrated to give medicinal extract.Medicinal extract plus 120 times of water are diluted, on The volume ratio of resin column absorption, raw material weight and resin is 1: 3, and resin column diameter and pillar height ratio are 1: 15, with the washing of pH=6 It washs, the elution of 50% alcoholic solution, flow velocity is 1 column volume/hour.

Alcohol eluent is collected, decolorising agent is added by effluent volume 5%, is heated to reflux 3 hours, filters, is concentrated under reduced pressure, Vacuum drying to get.Using PCA content in this law fig waste residue up to 50% or more.

A kind of embodiment 2: resin adsorption technology for extracting oligomeric pyrroles alkane carboxylic acid from fig

Raw material uses fig waste residue, is extracted 3 times with 60% reflow of alcohol, and each dosage is 8,6, the 4 of raw medicinal herbs weight Times, extraction time 60,45,30min, combined extract filter, and recovered alcohol is concentrated to give medicinal extract.By medicinal extract plus 150 times of water The volume ratio of dilution, upper resin column absorption, raw material weight and resin is 1: 5, and it is 1: 20 that resin column, which is passed through with pillar height ratio, with pH=8's Water washing, the elution of 60% alcoholic solution, flow velocity are 2 column volume/hours.Eluent is concentrated under reduced pressure, vacuum drying to get. Using PCA content in this law fig waste residue up to 50% or more.

Claims (2)

1. a kind of resin adsorption technology that oligomeric pyrroles alkane carboxylic acid is extracted from fig, it is characterized in that: the method steps are as follows:

(1) by fig waste residue extracting in water 1-10 times, each dosage is respectively 2-20 times of medicinal material weight, and extraction time is 0.5-10 hours, Extracting temperature was 10-100 DEG C, combined extract；

Or extract fig waste residue 5-95% reflow of alcohol 1-10 times, each dosage is respectively 2-20 times of medicinal material weight, Extraction time is 0.5-10 hours, combined extract, filtering, and recovered alcohol is concentrated to give medicinal extract；

(2) by the extracting solution of (1) or add the medicinal extract after 1-200 times of water dilution, the absorption of upper resin column, the body of raw material weight and resin Product ratio is 1: 0.5-10, and resin column diameter and pillar height ratio are 1: 1-30, and the water washing for being 2-8 with pH value, concentration are 5-95% alcohol Solution elution, flow velocity are 0.5-3.5 column volume/hour, and the resin is by the polystyrene of polystyrene series, modification The resin of series and the opposed polarity of isobutene series synthesis, different model；

(3) alcohol eluent is collected, decolorising agent is added in the ratio of effluent volume 1-30%, is heated to reflux 0.1-10 hours, Filtration, be concentrated under reduced pressure, vacuum drying to get；Using PCA content in this law fig waste residue up to 50% or more.

2. it is according to claim 1 for preventing and treating the preparation method of the plant extracts of asthenopia, it is characterized in that: prepared Extract directly or be mixed and made into preparation with pharmaceutically acceptable carrier.