CN103919821A - Extraction method for cynomorium songaricum extract product - Google Patents

Abstract

The invention discloses a producing method for selenium-rich cynomorium songaricum extract products. The producing method is characterized by including steps as follows: step one: pretreating cynomorium songaricum, coarsely grinding the cynomorium songaricum and crushing the cynomorium songaricum in an ultramicro manner with an addition of seleninic acid to obtain a selenium-rich cynomorium songaricum ultramicro powder raw material; step two: preparing a cynomorium songaricum ultramicro raw material liquid; and step three: producing various extract products of high-purity micromolecular ester-soluble or semi-ester soluble nanocrystals or micron-sized crystals through a high speed centrifugal separation process and a vacuum drying process. The beneficial effects of the above producing method for the cynomorium songaricum extract products are that: a cynomorium songaricum crude raw material is subjected to deep processing by an ultramicro crushing process so that the cynomorium songaricum raw material is crushed finely with a particle size distribution being uniform. Any heat is not generated during the crushing process and original physical and chemical performance and biological availability of the cynomorium songaricum are substantially improved. Ultrasound wave which is generated during the ultramicro crushing process has a certain sterilizing and fresh-keeping function. Because a cynomorium songaricum liquid extractive is extracted through an organic solvent and is separated by the high speed centrifugal separation process and crystals of the cynomorium songaricum are produced through the vacuum freeze drying process, effective components in the cynomorium songaricum crude raw material is prevented from losing and active components in the cynomorium songaricum are saved furthest. Time of the process flow is shortened. The producing method is energy-saving, can save medicinal raw materials and reduces product costs.

Description

A kind of extracting method of Herba Cynomorii extract

Technical field

The present invention relates to a kind of extracting method of Chinese medicine extract, relate in particular to a kind of extracting method of Herba Cynomorii extract.

Background technology

Fleshy stem for the parasitic herbaceous plant Herba Cynomorii of Cynomoriaceae meat, main component herb is containing Herba Cynomorii terpene, the effective ingredient such as acyl ursolic acid, ursolic acid, Herba Cynomorii has yang invigorating functions, after salt is concocted, function to testis, epididymis and the preputial glands of normal and yang deficiency mice has obvious facilitation, in Herba Cynomorii water extract, the activity ratio of sperm strengthens, and is the common medicine for the treatment of male sterility.Herba Cynomorii extract is used as medicine conventionally, and the extracting mode of Herba Cynomorii extract has much such as having water distillation, formaldehyde, ether solvent extraction and supercritical extraction etc., and conventional extracting method extracts as raw material after due to the pretreatment that Herba Cynomorii raw medicinal material is carried out.Because raw materials of traditional Chinese medicinal materials is thick, the composition of medical material extracts and can not be extracted completely, and next present extracting method does not carry out molecular separation causes the Herba Cynomorii extract purity obtaining not high, and biological activity is low, and bioavailability is low, causes resource waste.In addition, in leaching process, also will add multiple other multi-solvents materials, the interpolation of these vehicle substances very easily causes the residual of Herba Cynomorii extract noxious substance and pollutes, and the difficult quality of the trace element existing in extract is reached to effective control.

At present Herba Cynomorii Chinese crude drug is at warehouse lay up period, easily by antibacterial, and the pollution of insect pest and microorganism mycete; Generally need to adopt the smoked sterilizing pesticide of sulfur.The contained trace element loss of Herba Cynomorii medical material after sulfur is smoked is very large, especially Herba Cynomorii terpene, the loss of the active substance such as acyl ursolic acid, ursolic acid element is larger, thereby reduced the pharmaceutical quality of medical material; Because leaching process has increased pre-treatment crude drug, smoked without sulfur when storing medical material, change into and adopt the storage steric course sterilizing of superpower ultraviolet air sterilization apparatus to Herba Cynomorii medical material; Adopt mildew-resistant to store the technology packing of vacuum bag packages Herba Cynomorii medical material; The processing of Herba Cynomorii Chinese crude drug is increased to micronized pulverization technique, make this extract easily by by micromolecule, improved the bioactive content of this product, improved and guarantee that the quality and yield of this extract is high: the innovation product has been the molten and molten extract of half ester of lyophilization micromolecule nanometer and 2 kinds of esters of micron.

Summary of the invention

Problem for above-mentioned existence, the effective method that the object of this invention is to provide a kind of innovation leaching process of Herba Cynomorii crude drug extractive technique, be conducive to the micromolecule to Herba Cynomorii extract, be conducive to improve the purity of this extract, be conducive to improve the bioavailability of Herba Cynomorii extract, be conducive to control the volatility of Herba Cynomorii extract, improve the stability that has kept its content.

The object of the invention is to be achieved through the following technical solutions:

An extracting method for Herba Cynomorii extract, wherein, comprises the steps,

Step 1, cleans decontamination dried by medical material Herba Cynomorii; Roughly grind the order to 80-120, carry out again micronizing Herba Cynomorii raw material and make Herba Cynomorii raw material: with Herba Cynomorii coarse powder raw material, through micronizing unit, in pulverizing chamber, be subject to the dither that the high speed impact of grating disk and shearing and eddy current produce and pulverized, form powder body; Described powder body enters grading room be simultaneously subject to the effect of air force and centrifugal force to make 300-500 object micropowders under suction function, discharges after entering thereafter the pipeline that gathers materials, and collects and obtains Herba Cynomorii micropowders powder body;

Step 2, makes Herba Cynomorii raw material: the Herba Cynomorii ultrafine powder making in described step 1, with the alcohol-pickled 0.5-3 of 50%-90% hour, is obtained to immersion thereby filter; Gained immersion is poured to unsaturated common salt aqueous solution immersion and within 0.5-3 hour, through salt, soak and desalting processing, elimination sediment obtains filtrate; By gained filtrate pH value, be 5-6.5, under 55-115 ℃ of condition, carry out catalytic reaction 0.5-3 hour obtaining catalytic reaction solution; Adopt Ethanol-Acetic Acid ethyl ester-pure water to be mixed catalytic reaction solution, extract and obtain Herba Cynomorii extract; Gained Herba Cynomorii extract is made to Herba Cynomorii micromolecule ester type half ester type lyophilization crystalline solid raw material in vacuum lyophilization;

Step 3, adopt high speed centrifugation isolation technics to make Herba Cynomorii extracting solution: in extracting tank body, high speed centrifugation to be installed and to be fanned one group, during the operation of described high speed centrifugation fan, with the rotating speed of 3000-50000, the Herba Cynomorii raw material extracting solution making in described step 2 being carried out to sedimentation processes and obtains Herba Cynomorii extract liquid, and then via hole diameter be the micron-sized resin chromatographic column of 20-120 super consider separatedly concentratedly make Herba Cynomorii extract concentrated solution, after vacuum drying, make the micromolecule extracting solution of Herba Cynomorii nanometer and micron;

The extracting method of above-mentioned a kind of Herba Cynomorii extract wherein, is 3 times with the number of times of described ethyl acetate extraction in described step 2.

The extracting method of above-mentioned a kind of Herba Cynomorii extract, wherein, catalytic reaction solution described in described step 2 and described Ethanol-Acetic Acid ethyl ester-pure water volume ratio are 1:1-1:1.5; The material ratio degree of 0.05 Herba Cynomorii extracting solution is 1:40-50 times.

Compared with the prior art, beneficial effect of the present invention is: by Chinese crude drug Herba Cynomorii coarse powder raw material is carried out to the reprocessing of micronizing technique, make the meticulousr of Herba Cynomorii raw material pulverizing, even particle size distribution, crushing process does not produce heat, and the original physicochemical property of Herba Cynomorii raw material is constant, and bioavailability is enhanced, Herba Cynomorii raw material is had to fresh-keeping function, and the ultrasonic technology and the ultraviolet that have adopted crushing process to produce have certain sterilizing function that disappears simultaneously; By high speed centrifugation separation, make Herba Cynomorii extract, prevent the loss of effective ingredient in Herba Cynomorii raw material, preserve to greatest extent the active component of Herba Cynomorii, shortened technological process, energy savings and raw material, reduce costs, obtain the Herba Cynomorii extract of 2 kinds of highly purified micromolecule ester dissolubilities and half ester dissolubility nanometer and micron.

Accompanying drawing explanation

Fig. 1 is the extracting method process flow diagram of a kind of Herba Cynomorii extract of the present invention.

The specific embodiment

Below in conjunction with schematic diagram and concrete operations embodiment, the invention will be further described.

As shown in Figure 1, the extracting method of a kind of Herba Cynomorii extract of the present invention, first, take Herba Cynomorii as raw material, first upper corase grind is ground to 80-120 order, adopt again micronizing unit to carry out micronizing, be crushed to 300-500 order, add sodium selenite, when Herba Cynomorii coarse granule is sent in pulverizing chamber by spiral through charging aperture, be subject to high speed impact and the shearing of grating disk, the while is also subject to the dither of eddy current generation and is pulverized.Powder body after pulverizing is crossed spreader and is covered into grading room under suction function.Due to the high speed rotating of grading wheel, powder body is subject to the effect of air force and centrifugal force simultaneously.When centrifugal force > air force, illustrate that powder body is greater than predefined Cut size particle size, powder body is got rid of to be returned to pulverizing chamber to tapered sleeve and continues to pulverize, and the qualified powder body of the pulverizing that meets the standard of setting in advance, now air force > centrifugal force is subject to dynamic action, after entering the pipeline that gathers materials, to subsidiary engine, be discharged from, after collection, become Herba Cynomorii ultrafine powder.Secondly, above-mentioned gained Herba Cynomorii ultrafine powder, with after the alcohol-pickled 0.5-3 of 50%-90% hour, is obtained to immersion; Gained immersion is poured to unsaturated common salt aqueous solution immersion and within 0.5-3 hour, through salt, soak and desalting processing, elimination sediment obtains filtrate; Adjust pH value to be adjusted to acidity gained filtrate simultaneously, be approximately 5-6.5, then at 55-115 ℃, carry out catalytic reaction 0.5-3 hour; The solution 1:1 adopting during catalytic reaction ,-1:1, the proportioning of 2 Ethanol-Acetic Acid ethyl ester; 1:40-50 times of thing than the condition of degree under extraction repeatedly, extract and obtain Herba Cynomorii liquid charging stock for 2-3 time.

Next, transformation extraction pot; Vertical shaft upper end in extracting tank body is installed high speed centrifugation and is fanned one group, under the transmission of vertical shaft, drives high speed centrifugation to fan centrifugal operation; High speed rotating speed by described high speed centrifugation fan with 3000-10000, prepared Herba Cynomorii liquid charging stock is carried out to high speed settling processing, obtain micromolecule Herba Cynomorii extract liquid, and then make Herba Cynomorii extract concentrated solution through large aperture resin and chromatography post, through making Herba Cynomorii extract liquid after cooling rapidly.

The Herba Cynomorii extract making according to said method, owing to adopting molecular sieve to control the molecule Quality Control of Herba Cynomorii extract, therefore, this Herba Cynomorii extract can reach the quality standard of molecular level, is beneficial to the component and the trace element total amount that improve this extract, and Quality Control is clearer and more definite, biological activity is high, safety, purity is high, and bioavailability is high; The Herba Cynomorii extract that the said method of take makes is as the medicine making as raw material, and cosmetics, when flavorant and other products, are more conducive to absorption and the absorption of human body, and result of use can be better.

Above specific embodiments of the invention be have been described in detail, but the present invention is not restricted to specific embodiment described above, it is just as example.To those skilled in the art, any equivalent modifications that this is carried out and alternative also all among category of the present invention.Therefore, do not depart from of the present invention

Equalization conversion and the modification under spirit and scope, done, all should contain within the scope of the invention.

Claims (3)

1. this technological invention relates to a kind of extracting method of Chinese medicine Herba Cynomorii extract, relates to extractive technique and the product of the fat-soluble and half fat-soluble organic molecule natural chemical substance of Chinese crude drug Herba Cynomorii, and its technological invention right characteristic is, comprises the following steps;

Step 1, micronizing Herba Cynomorii make superfine powder raw produce: Chinese crude drug Herba Cynomorii rhizome portion is screened, removing clean-air dry of impurity-water dries, with pressure pneumatic hammer machine, smash to pieces, enter electric rough grinding machine and be crushed to 80-120 order, add trace element-selenium again this coarse powder to be entered to micronizing unit and carry out micronized pulverization to 300-500 order, make rich selenium ultra micro Herba Cynomorii powder; Under the dither that during micronized pulverization operation, Herba Cynomorii coarse powder raw material and trace element-selenium produce in the indoor high speed impact that is subject to micronizing dish of airtight micronizing and shearing and swirl pneumatic power and pressure, by micronizing, form the rich selenium ultrafine powder integrally combining; Described powder body enters singulizing disc chamber and is repeatedly subject to after the effect of air force and centrifugal pressure handkerchief under suction function, discharges after entering the pipeline that gathers materials, and collects, and through packing, makes the rich selenium ultrafine powder of 300-500 object raw produce;

Step 2, make Herba Cynomorii raw material liq: by the Herba Cynomorii ultrafine powder making in described step 1 with 50%-90% soak with ethanol 0.5-3 hour, then obtain Herba Cynomorii immersion through ultrafiltration; Gained immersion is poured to unsaturated common salt aqueous solution, then soak and through salt, soak and desalting processing for 0.5-3 hour, elimination Herba Cynomorii sediment, obtains Herba Cynomorii filtrate; The pH value of gained Herba Cynomorii filtrate is adjusted to 5-6.5, under the temperature conditions of 55-115 ℃, carries out catalytic reaction 0.5-3 hour, obtain catalytic reaction solution; Catalytic reaction solution adopts ethyl acetate and ethanol and micromolecule pure water mixed solvent, and proportioning is 1:1-1:1.5:0.1 concentration, through catalytic reaction extraction, obtains Herba Cynomorii extract;

Step 3, high speed centrifugation separation make Herba Cynomorii extract and through vacuum drying, make nanometer and micron ester type half ester type Herba Cynomorii ester is molten and the white light yellow complexion crystalline solid of half ester dissolubility Coumarins again; In extracting tank body, high speed centrifugation is installed and is fanned 1 group, gradient rotating speed that can 3000-5000 during the operation of described high speed centrifugation fan, the Herba Cynomorii extract liquor body raw material making in described step 2 is carried out settlement separate, collect respectively 2 kinds of liquid of the Herba Cynomorii small molecular extract obtain nanometer and micron different scale; Via hole diameter is the different micron-sized resins of 20-120 and chromatography column separating purification respectively again, make 2 kinds of Herba Cynomorii purified extract micromolecule concentrated solutions, dry through frozen vacuum dryer, reclaim solvent, make Herba Cynomorii coumarin lyophilizing crystalline solid, total content is dried 2 kinds of things higher than ester type and the white light yellow complexion small molecule active of the half ester type Herba Cynomorii crystallization freezing of 0.4%-0.5% content.

2. the extracting method of a kind of Herba Cynomorii extract according to claim 1, is characterized in that, in described step 2 with the matching method of described ethyl acetate and ethanol and pure water mixed solvent and proportioning 1:1 and 1:1.5 and 1:0.05; The temperature conditions of extraction is 55-115 degree, and ph is 5-6.5, and the number of times that decompression is extracted in reflux course is 2-3 time.

3. the extracting method of a kind of Chinese medicine Herba Cynomorii extract according to claim 1 and 2, is characterized in that, catalytic reaction solution described in described step 2 and described ethyl acetate volume ratio are 1:1-1:1,5; 1; The ratio degree of 0,05 reaction solution and Herba Cynomorii material is 1:40-1:50 times, and temperature conditions is 55-115 degree.