CN103923051B - Industrial extracting method for ampelopsin - Google Patents

Abstract

The invention discloses an industrial extracting method for ampelopsin. The industrial extracting method comprises the steps of adding magnetized water into an extracting tank through a magnetizer until materials are immersed; circularly magnetizing the water, extracting under heating, and collecting an extracting solution after the extraction is ended; cooling the extracting solution, standing and extracting a clear solution to obtain a sediment; adding ethanol into the sediment, ultrasonically vibrating, extracting under heating, and extracting a supernatant liquid; carrying out vacuum concentration on the supernatant liquid to obtain a concentrated solution; adding hot water to dilute the concentrated solution, stirring, naturally cooling, separating the bottom sediment, further naturally cooling the residual clear solution to generate a yellowish white sediment, secondarily adding hot water into the yellowish white sediment, boiling, dissolving, repeating the steps many times, and drying the obtained high-purity ampelopsin. By using the industrial extracting method, the yield can be increased by more than 35%, and the extracting time can be shortened by 1/3; when ampelopsin is separated, fat-soluble impurities, part of water-soluble polyphenol and other impurities are removed; in addition, most of water-soluble polyphenols are removed through sectional sedimentation.

Description

A kind of industrial purifying process of ampelopsin

Technical field

The present invention relates to a kind of industrial purifying process of environmental protection of biological medicine ampelopsin.Only adopt ArsenazoⅢ level alcohol as Extraction solvent, through special method, obtain highly purified ampelopsin, also obtain polysaccharide compound and polyphenol complex product simultaneously.Toxic wastewater exhaust gas emission is not had, environmental protection in whole leaching process, with low cost, be applicable to suitability for industrialized production.

Background technology

Ampelopsin has protecting the liver, relieves the effect of alcohol, hypotensive, antitumor, promote the important pharmaceutical uses such as skin repair, be developed to various medicine, functional food or makeup in recent years.Therefore also cause the demand of ampelopsin huge, the industrial high efficiency Isolation and purification technology of ampelopsin is also subject to the extensive concern in industry.At present in the extraction process of natural product, adopt toxic organic solvents degreasing impurity elimination to extract natural drug or food ingredient is still widely used method.But toxic organic solvents remains and brings a lot of potential safety hazard to medicine or foodstuff production.In the extraction purification technology of ampelopsin, current bibliographical information and disclosed patented technology can be summed up as following basic skills: adopt the fat-soluble organic solvent such as sherwood oil or gasoline to dried material degreasing, then the material water heating after degreasing is boiled and boil extraction, then concentrating and precipitating or column chromatography are carried out to extracting solution, obtain the ampelopsin that purity is higher.There is a fatal weakness in this kind of technique: in skimming processes, have employed toxic organic solvents exactly, makes to remain with noxious solvent in the ampelopsin extracted.Therefore, study a kind of simple effectively, environmental protection and can the ampelopsin extracting method that uses of large-scale low-cost most important for the sound development of the sector.The present invention specifically solves following key technical problem: (1) adopts pure water and food grade alcohol as Extraction solvent, does not adopt any other solvent in addition; (2) controlled by the control of special temperature and alcohol concn, the impurity substep in extracting solution is removed.

The whole process of the inventive method does not also need column chromatography without the need for malicious solvent.Adopt rare alcohol (alcohol extract joins in ten times of water gagings and precipitates when alcohol extract precipitates, rare exactly alcohol) method of cooling reaches the object of degreasing, be precipitated simultaneously, water-soluble and specified temp cooling is heated again to precipitation, isolate polyphenol, then continue specified temp cooling, obtain highly purified ampelopsin.Present method realizes being separated based on the water-soluble difference of the fat-soluble component based on chlorophyll in total extracting solution, the various composition in vine tea polyphenol and ampelopsin.Because the major impurity in vine tea Aqueous extracts has: fat-soluble components such as fat, chlorophyll, protein, colloids, the water soluble components such as many sugar and starches, half water soluble component such as ampelopsin and various Polyphenols.Research report proves that in the flavonoid compound of vine tea, main component is ampelopsin, separately has a small amount of flavonoid impurity as poplar mycin, Quercetin, the second light industry bureau Quercetin, apigenin and kaempferol and micromolecular Polyphenols.In the Aqueous extracts of vine tea, because ampelopsin contains more hydroxyl (6 hydroxyls) and the three-dimensional arrangement of 3 '-position thereof, it is water-soluble far away higher than ampelopsin, Quercetin, the second light industry bureau Quercetin, apigenin and kaempferol, therefore we utilize this nature difference, by regulating precipitation temperature, realize effectively being separated of ampelopsin and other flavonoids and Polyphenols.

In addition, adopt extraction process by water efficiency lower, mainly because the viscosity of water is large, power of impregnation is weak, how to improve the penetration power of water, is the key of extraction process by water.Be that the water molecule number reducing water clusters is to improve the seepage force of water molecules about the penetration power key improving water, based on this, present invention employs magnetized water circulation method to extract, the aqueous solution of extractor is made constantly to circulate through magnetizing apparatus magnetization, can improve extraction efficiency more than 50%, extraction yield exceeds 20-30%.

Summary of the invention

The object of the invention is the industrial purifying process that there are provided a kind of ampelopsin.In whole purification process, only adopt pure water and food grade alcohol as Extraction solvent.Adopt the macromole water-soluble impurities such as alcohol extracting method Polysaccharide removing, starch, adopt rare alcohol (alcohol extract joins in ten times of water gagings and precipitates, and the is exactly rare alcohol precipitation) precipitator method to remove the oil-soluble impuritieses such as chlorophyll, adopt the temperature control precipitator method to remove impurity flavones and Polyphenols.Finally obtain high purity ampelopsin and byproduct Crude polysaccharides, total polyphenols.

In order to realize above-mentioned object, the present invention adopts following technical measures:

An industrial purifying process for ampelopsin, the steps include:

Step 1, pure water are join extractor to submergence material, the dry blade of material and Ampelopsis grossedentata or fresh Ampelopsis grossedentata blade after 2000-6000mT magnetizing apparatus magnetizes by Surface field intensity;

Step 2, then boil boil to 95 DEG C insulation 0.5-1 hour, while insulation, the extracting solution of material is the filter plate of 0.5-1 millimeter by aperture under the driving of recycle pump, entering Surface field intensity is get back in extractor by the mouth of pipe that adds water after the magnetizing apparatus of 2000-6000mT magnetizes, and collects extracting solution after extraction by the mouth of pipe;

Step 3, adopt artificial cooling or naturally cooling that temperature is cooled to less than 10 DEG C to extracting solution, staticly settle 5-8 hour, after extracting clear liquid, remaining precipitation takes out most moisture to without water droplet;

Step 4, then to step 3 collect precipitation in add the food-grade ethanol (high-tech Treatment of Industrial Water Chemical Co., Ltd. of Jining of Shandong Province city) that concentration is not less than 95%, ultrasonic vibration (40KHz, 500W, the clean safe PS-40 in Shenzhen) and 50-60 DEG C of heating and thermal insulation extracts 0.5-1 hour, then suction filtration supernatant liquid while hot, the mixture being precipitated as polysaccharide, protein, starch and colloid of gained after extraction clear liquid, can directly use as functional food, its polysaccharide content is at about 20-50%;

Step 5, to step 4 extract supernatant liquid carry out vacuum concentration to evaporator wall occurring white crystals with industrial rotatory evaporator time collect concentrated solution;

Step 6, by the concentrated solution of step 5 according to concentrated solution: hot water is the hot water that the mass ratio of 1:10-20 is injected into that temperature is 70-90 DEG C, and stirs, until after naturally cooling to room temperature leave standstill 12-24 hour, then extract out upper strata be suspended thing and clear liquid, collecting precipitation;

Step 7, the water of 5-10 times of quality is added to the precipitation that step 6 is collected,

Step 8, heated and stirred until precipitation is all dissolved to 95 DEG C, then stop heating, naturally cool to 50-60 DEG C;

Step 9, be separated bottom tan precipitate when step 8 naturally cools to 50-60 DEG C, this tan precipitate is vine tea Polyphenols impurity, can directly use as foodstuff additive;

The supernatant liquid of step 10, step 9 continues naturally cooling or refrigeration is cooled to less than 10 DEG C rear leaving standstill to produce yellow-white precipitation after 12-24 hour;

The yellow-white of step 11, collection step 10 precipitates 80 DEG C of oven dry, can obtain the ampelopsin of more than 90% purity;

Step 12, as improved purity, the ampelopsin obtained step 11 adds the water of 5-10 times of quality, adopts step 8 can obtain the ampelopsin of more than 98% for 2-3 time to the method re-treatment of step 11.

Above extracting method obtains three kinds of products: polysaccharide compound, vine tea polyphenol complex and high purity ampelopsin.

Because present method adopts magnetized water to extract, in order to improve the penetration power of water, thus improve extraction efficiency, the present invention devises magnetized water extractor, meanwhile, concentrate according to the singularity of precipitin reaction in this extracting method-----polyphenol and be deposited in setting tank bottom center, devise special setting tank.

The present invention compared with prior art, has following beneficial effect:

(1) utilize rare alcohol to precipitate the lipid such as ampelopsin and suspension chlorophyll, the lipid such as ampelopsin and chlorophyll is separated, reach the object removing oil-soluble impurities, remove part water-soluble polyphenols class simultaneously; (2) adopt 95% alcohol extraction to go out total flavones and a small amount of polyphenol to ampelopsin and the precipitation mixture such as polysaccharide, starch, reach the impurity such as Polysaccharide removing, protein, starch; (3) fix cooling temperature (50-60 DEG C) stagnation point, within the scope of this stagnation point, ampelopsin is still dissolved in the hot water, other flavones of major part, as the then Precipitation such as ampelopsin, Quercetin, the second light industry bureau Quercetin, apigenin and kaempferol, adopt the flavones beyond this method separation ampelopsin and Polyphenols; (4) adopt magnetized water circulation method to extract the ampelopsin in material, and do not adopt compared with magnetized water circulation method, general extractive yield improves more than 30%, and ampelopsin yield can improve more than 5%; (5) adopt the settling tank of special band underseal structure, carry out collection Polyphenols precipitation, improve work efficiency.

Accompanying drawing explanation

Fig. 1 is the structural representation of extractor;

Fig. 2 is setting tank side-view;

Fig. 3 is that the first state graph (underseal is opened) overlooked by setting tank;

Fig. 4 is that the second state graph (underseal closes) overlooked by setting tank;

In figure: 1-extractor; 2-magnetizing apparatus; 3-water pump; 4-setting tank; 5-underseal; 5-1-first fans underseal; 5-2-second fans underseal; 6-ampelopsin precipitates; 7-Polyphenols precipitation (comprising the flavones precipitation except ampelopsin); 8-supernatant liquor; 9-controls motor; 10-transmission shaft; 11-polyphenol precipitates; 12-filter plate; The 13-mouth of pipe.

Embodiment

embodiment 1:

Extractor 1 is with the magnetizing apparatus 2 on the water-circulating pump 3 of bidirectional circulating function and water circulating pipe, and its using method is: after adding material, injects pure water by the mouth of pipe 13, then opens reverse cycle pump 3, starts heating cycle and extracts; The bottom of extractor 1 is provided with filter plate 12.Liquid extracting bottom extractor 1 is also magnetized by recycle pump 3 and magnetizing apparatus 2 top being promoted to extractor 1 by the bottom of extractor 1 successively.

Setting tank 4 bottom center is provided with the polyphenol settling tank 11 that a layer height is to ten/20ths 1/5th of setting tank height, the top of this polyphenol settling tank also has a underseal 5, this underseal is two semicircle flabellum (5-1,5-2) composition and automatic open-close the effect played when closed at the bottom of sealed can, described two semicircle flabellum (5-1,5-2) drive folding by transmission shaft 10, the power of this transmission shaft 10 is controlled by motor 9.

An industrial purifying process for ampelopsin, the steps include:

Step 1,50 kilograms, the dry blade of Ampelopsis grossedentata to be rendered in the middle of extractor 1, opens water pump 3, by the interface 10 of water pipe pure water be added to extractor (in) do not have material to water logging,

Step 2, heating are boiled and are boiled to 95 DEG C of insulations 1 hour, while insulation, reversion water pump starts circulation by the water in extractor, water is the filter plate 12 of 0.5-1 millimeter by extractor bottom part aperture diameter and is the magnetizing apparatus of 6000mT by Surface field intensity in working cycle, the penetration power of water is strengthened, the constituents extraction ability of vine tea leaf is strengthened, then extracting extracting solution out from the mouth of pipe 13 turns back to extractor, extracts extracting solution out and put in cooling pool after extraction

Step 3, again extracting in water, return step 2 and repeatedly extract 3 times, put into cooling pool and collect extracting solution;

Step 4, in cooling pool, reduce the temperature to 10 DEG C to extracting solution naturally cooling, staticly settle 5 hours, then extract the supernatant liquid in cooling pool out, after extracting clear liquid, remaining precipitation is placed on gauze and is filtered dry moisture;

Add the food-grade ethanol that concentration is 95% in step 5, the precipitation of then collecting in step 4, ultrasonic vibration (40KHz, 500W, PS-40) heating and thermal insulation extract 1 hour at 60 DEG C, then take advantage of hot suction filtration supernatant liquid,

Step 6, return step 5 until suction filtration 3 supernatant liquids repeatedly, the mixture being precipitated as polysaccharide, protein, starch and colloid of gained after extraction clear liquid, can directly use as functional food, wherein main component is polysaccharide, and its polysaccharide content is about 40%;

Concentrated solution is collected when step 7, the clear liquid extracted step 6 again carry out vacuum concentration to evaporator wall there is yellow-white crystalline with industrial rotatory evaporator;

Step 8, the concentrated solution collected step 7 to be injected into according to the mass ratio of 1:20 in the water of 90 DEG C and slowly to stir, and naturally cool to room temperature, leave standstill 20 hours, then extract supernatant liquor out, collecting precipitation;

Step 9, to step 8 collect precipitation add 5 times of quality water,

Step 10, heated and stirred are to 95 DEG C until precipitation is all dissolved, and then stop heating, transferred to by solution in setting tank 4, open two flabellums (5-1,5-2) of underseal 5, then solution naturally cools to 60 DEG C;

Closing two flabellums (5-1,5-2) of underseal 5 time step 11, solution temperature in step 10 drop to 50 DEG C, be tan precipitate inside underseal 5, and this tan precipitate is vine tea Polyphenols and precipitates;

Step 12, continuation naturally cooling or refrigeration are cooled to less than 10 DEG C, leave standstill and produce yellow-white precipitation after 20 hours;

Step 13, collection yellow-white are deposited in the ampelopsin that 80 DEG C of oven dry can obtain more than 90% purity, step 14,5 times of quality water are added again to the ampelopsin that step 13 obtains, return step 10 can obtain more than 95% for 2-3 time ampelopsin to the method re-treatment of step 13.

embodiment 2:

Extractor 1 is with the magnetizing apparatus 2 on the water-circulating pump 3 of bidirectional circulating function and water circulating pipe, and its using method is: after adding material, injects pure water by the mouth of pipe 13, then opens reverse cycle pump 3, starts heating cycle and extracts; The bottom of extractor 1 is provided with filter plate 12.Liquid extracting bottom extractor 1 is also magnetized by recycle pump 3 and magnetizing apparatus 2 top being promoted to extractor 1 by the bottom of extractor 1 successively.

Setting tank 4 bottom center is provided with the polyphenol settling tank 11 that a layer height is to ten/20ths 1/5th of setting tank height, the top of this polyphenol settling tank also has a underseal 5, this underseal is two semicircle flabellum (5-1,5-2) composition and automatic open-close the effect played when closed at the bottom of sealed can, described two semicircle flabellum (5-1,5-2) drive folding by transmission shaft 10, the power of this transmission shaft 10 is controlled by motor 9.

An industrial purifying process for ampelopsin, the steps include:

Step 1,50 kilograms, the dry blade of Ampelopsis grossedentata to be rendered in the middle of extractor 1, opens water pump 3, by the interface 10 of water pipe pure water be added to extractor (in) do not have material to water logging,

Step 2, heating are boiled and are boiled to 98 DEG C of insulations 1 hour, while insulation, reversion water pump starts circulation by the water in extractor, water is the filter plate 12 of 0.5-1 millimeter by extractor bottom part aperture diameter and is the magnetizing apparatus of 6000mT by Surface field intensity in working cycle, the penetration power of water is strengthened, the constituents extraction ability of vine tea leaf is strengthened, then extracting extracting solution out from the mouth of pipe 13 turns back to extractor, extracts extracting solution out and put in cooling pool and be cooled to room temperature after extraction.

Step 3, again the supernatant liquid cooled in step 2 cooling pool is joined in extractor, return step 2 and repeatedly extract 3 times, extracting solution is put into cooling pool and is cooled to room temperature;

Step 4, in cooling pool, reduce the temperature to 10 DEG C to extracting solution artificial cooling, staticly settling 10 hours, then extract the supernatant liquid in cooling pool out, after extracting clear liquid, remaining precipitation is placed on gauze and is filtered dry moisture;

Add the food-grade ethanol that concentration is 90% in step 5, the precipitation of then collecting in step 4, ultrasonic vibration (40KHz, 500W, PS-40) heating and thermal insulation extract 1 hour at 60 DEG C, then take advantage of hot suction filtration supernatant liquid,

Step 6, return step 5 until suction filtration 3 supernatant liquids repeatedly, the mixture being precipitated as polysaccharide, protein, starch and colloid of gained after extraction clear liquid, can directly use as functional food, wherein main component is polysaccharide, and its polysaccharide content is about 35%;

Concentrated solution is collected when step 7, the clear liquid extracted step 6 again carry out vacuum concentration to evaporator wall there is yellow-white crystalline with industrial rotatory evaporator;

Step 8, the concentrated solution collected step 7 to be injected into according to the mass ratio of 1:18 in the water of 80 DEG C and slowly to stir, and naturally cool to room temperature, leave standstill 24 hours, then extract supernatant liquor out, collecting precipitation;

Step 9, add 6 times of quality water to the precipitation that step 8 is collected, be heated to 98 DEG C, stir until precipitation is all dissolved, then stop heating, transferred to by solution in setting tank 4, open two flabellums (5-1,5-2) of underseal 5, then solution naturally cools to 60 DEG C;

Closing two flabellums (5-1,5-2) of underseal 5 time step 10, solution temperature in step 10 drop to 50 DEG C, be tan precipitate inside underseal 5, and this tan precipitate is vine tea Polyphenols and precipitates;

Step 11, continuation refrigeration are cooled to less than 10 DEG C, leave standstill and produce yellow-white precipitation after 20 hours;

Step 12, collection yellow-white are deposited in the ampelopsin that 80 DEG C of oven dry can obtain more than 90% purity, step 13, again add 6 times of quality water to the ampelopsin that step 12 obtains, the method re-treatment returning step 9 to 12 can obtain the ampelopsin of more than 97% for 2-3 time.

embodiment 3

Extractor 1 is with the magnetizing apparatus 2 on the water-circulating pump 3 of bidirectional circulating function and water circulating pipe, and its using method is: after adding material, injects pure water by the mouth of pipe 13, then opens reverse cycle pump 3, starts heating cycle and extracts; The bottom of extractor 1 is provided with filter plate 12.Liquid extracting bottom extractor 1 is also magnetized by recycle pump 3 and magnetizing apparatus 2 top being promoted to extractor 1 by the bottom of extractor 1 successively.

Setting tank 4 bottom center is provided with the polyphenol settling tank 11 that a layer height is to ten/20ths 1/5th of setting tank height, the top of this polyphenol settling tank also has a underseal 5, this underseal is two semicircle flabellum (5-1,5-2) composition and automatic open-close the effect played when closed at the bottom of sealed can, described two semicircle flabellum (5-1,5-2) drive folding by transmission shaft 10, the power of this transmission shaft 10 is controlled by motor 9.

An industrial purifying process for ampelopsin, the steps include:

Step 1, pure water are join extractor to submergence material, the dry blade of material and Ampelopsis grossedentata or fresh Ampelopsis grossedentata blade after 2000-6000mT magnetizing apparatus magnetizes by Surface field intensity;

Step 2, then boil boil to 95 DEG C insulation 1 hour, while insulation, the extracting solution of material is the filter plate 12 of 0.5-1 millimeter by aperture under the driving of recycle pump 3, and entering Surface field intensity is get back in extractor after the magnetizing apparatus 2 of 2000-6000mT magnetizes, and collects extracting solution;

Step 3, adopt artificial cooling or naturally cooling that temperature is cooled to less than 10 DEG C to extracting solution, staticly settle 5-8 hour, after extracting clear liquid, remaining precipitation takes out most moisture to without water droplet;

Add the food-grade ethanol that concentration is not less than 95% in step 4, the precipitation of then collecting to step 3, ultrasonic vibration 60 DEG C of heating and thermal insulations extract 0.5 hour, then suction filtration supernatant liquid while hot,

Step 5, to step 4 extract supernatant liquid carry out vacuum concentration to evaporator wall occurring white crystals with industrial rotatory evaporator time collect concentrated solution;

Step 6, by the concentrated solution of step 5 according to concentrated solution: hot water is that the mass ratio of 1:19 to be injected in the water of 80 DEG C and to stir, and stirs, until leave standstill 20 hours after naturally cooling to room temperature, then extracts supernatant liquor out, collecting precipitation;

Step 7, the water of 10 times of quality is added to the precipitation that step 6 is collected;

Step 8, heated and stirred until precipitation is all dissolved to 95 DEG C, then stop heating, naturally cool to 50 DEG C;

Step 9, isolate bottom tan precipitate when step 8 naturally cools to 50 DEG C;

The supernatant liquid of step 10, step 9 continues naturally cooling or refrigeration is cooled to less than 10 DEG C rear leaving standstill to produce yellow-white precipitation after 20 hours;

The yellow-white of step 11, collection step 10 precipitates 80 DEG C of oven dry, can obtain the ampelopsin of more than 90% purity;

Step 12, the ampelopsin obtained step 11 add the water of 5-10 times of quality, adopt step 8 can obtain the ampelopsin of more than 98% for 2-3 time to the method re-treatment of step 11.

Specific embodiment described in this specification sheets is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.

Claims (1)

1. an industrial purifying process for ampelopsin, the steps include:

Step 1, pure water are join extractor to submergence material, the dry blade of material and Ampelopsis grossedentata or fresh Ampelopsis grossedentata blade after 2000-6000mT magnetizing apparatus (2) magnetizes by Surface field intensity;

Step 2, then boil boil to 95 DEG C insulation 0.5-1 hour, while insulation, the extracting solution of material is the filter plate (12) of 0.5-1 millimeter by aperture under the driving of recycle pump (3), entering after magnetizing apparatus (2) that Surface field intensity is 2000-6000mT magnetizes gets back in extractor, collects extracting solution after extraction;

Step 3, adopt artificial cooling or naturally cooling that temperature is cooled to less than 10 DEG C to extracting solution, staticly settle 5-8 hour, after extracting clear liquid, remaining precipitation takes out most moisture to without water droplet;

Add the food-grade ethanol that concentration is not less than 95% in step 4, the precipitation of then collecting to step 3, ultrasonic vibration also extracts 0.5-1 hour at 50-60 DEG C of heating and thermal insulation, then suction filtration supernatant liquid while hot;

Step 5, to step 4 extract supernatant liquid carry out vacuum concentration to evaporator wall occurring white crystals with industrial rotatory evaporator time collect concentrated solution;

Step 6, by the concentrated solution of step 5 according to concentrated solution: hot water is the hot water that the mass ratio of 1:10-20 is injected into that temperature is 70-90 DEG C, and stirs, until after naturally cooling to room temperature leave standstill 12-24 hour, then extract out upper strata be suspended thing and clear liquid, collecting precipitation;

Step 7, the water of 5-10 times of quality is added to the precipitation that step 6 is collected;

Step 8, heated and stirred until precipitation is all dissolved to 95 DEG C, then stop heating, naturally cool to 50-60 DEG C;

Step 9, when step 8 naturally cools to 50-60 DEG C be separated bottom tan precipitate;

The supernatant liquid of step 10, step 9 continues naturally cooling or refrigeration is cooled to less than 10 DEG C rear leaving standstill to produce yellow-white precipitation after 12-24 hour;

The yellow-white of step 11, collection step 10 precipitates 80 DEG C of oven dry;

Step 12, the ampelopsin obtained step 11 add the water of 5-10 times of quality, adopt step 8 to method re-treatment 2-3 time of step 11.