CN103923051A - 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 extracting solvent, through special method, obtain highly purified ampelopsin, also obtain polysaccharide compound and polyphenol complex product simultaneously.In whole leaching process, there is no toxic wastewater exhaust gas emission, environmental protection, 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 in recent years various medicines, functional food or makeup.Therefore also cause the demand of ampelopsin huge, the industrial high efficiency of ampelopsin extracts and purification technique is also subject to the extensive concern in industry.In the extraction process of natural product, adopting poisonous organic solvent degreasing impurity elimination is still widely used method to extract natural drug or food ingredient at present.But poisonous organic solvent residual has brought a lot of potential safety hazards to medicine or foodstuff production.In the extraction purification technique of ampelopsin, current bibliographical information and disclosed patented technology can be summed up as following basic skills: adopt the fat-soluble organic solvents such as sherwood oil or gasoline to dried material degreasing, then the material water heating after degreasing is boiled and boiled extraction, then extracting solution is carried out to concentrating and precipitating or column chromatography, obtain the ampelopsin that purity is higher.There is a fatal weakness in this class technique: in skimming processes, adopt poisonous organic solvent exactly, and residual with noxious solvent in the ampelopsin that makes to extract.Therefore, study a kind of simple effectively, environmental protection and the ampelopsin extracting method that can large-scale low-cost uses most important for the sound development of the sector.The following key technical problem of the concrete solution of the present invention: (1) adopts pure water and food grade alcohol as extracting solvent, does not adopt in addition any other solvent; (2), by special temperature control and alcohol concn control, the impurity substep in extracting solution is removed.

The whole process of the inventive method does not need column chromatography without the need for malicious solvent yet.(alcohol extract joins in ten times of water gagings and precipitates in the time that alcohol extract precipitates, to adopt rare alcohol, rare exactly alcohol) method of cooling reaches the object of degreasing, be precipitated simultaneously, precipitation is heated again water-soluble cooling with specified temp, isolate polyphenol, then continue specified temp cooling, obtain highly purified ampelopsin.Present method is that various compositions in main fat-soluble component, vine tea polyphenol taking chlorophyll based in total extracting solution and the water-soluble difference of ampelopsin realize separation.Because the major impurity in vine tea water extraction liquid has: the fat-soluble components such as fat, chlorophyll, protein, colloid, the water soluble components such as many sugar and starches, half water soluble components such as ampelopsin and various Polyphenols.In the flavonoid compound of research report proof 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 water extraction liquid of vine tea, the three-dimensional arrangement that contains more hydroxyl (6 hydroxyls) and 3 '-position due to ampelopsin, 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 ampelopsin and separate with other flavonoids and the effective of Polyphenols.

In addition, adopting extraction process by water efficiency lower, is mainly because the viscosity of water is large, a little less than power of impregnation, how to improve the penetration power of water, is the key of extraction process by water.Be that about the penetration power key that improves water the water molecule number that reduces water clusters is to improve the seepage force of water molecules, based on this, the present invention has adopted magnetized water circulation method to extract, the aqueous solution of extractor is constantly circulated to be magnetized through magnetizing apparatus, can improve extraction efficiency more than 50%, extraction yield exceeds 20-30%.

Summary of the invention

The object of the invention is to be to provide a kind of industrial purifying process of ampelopsin.In whole purification process, only adopt pure water and food grade alcohol as extracting 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 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 to join extractor to submergence material after 2000-6000mT magnetizing apparatus magnetizes by Surface field intensity, and material is the dry blade of Ampelopsis grossedentata or fresh Ampelopsis grossedentata blade;

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

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

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

Step 5, the industrial rotatory evaporator of supernatant liquid that step 4 is extracted carry out vacuum concentration and collect concentrated solution when there is white crystals in evaporator wall;

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

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

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

Step 9, when step 8 naturally cools to 50-60 DEG C, separate bottom brown precipitation, this brown is precipitated as 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 10 DEG C of following rear leaving standstill after 12-24 hour, to produce yellow-white precipitation;

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

Step 12, as need improve purity, the ampelopsin that step 11 is obtained adds the water of 5-10 times of quality, adopts step 8 ampelopsin that can obtain 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.

Extract because present method adopts magnetized water, in order to improve the penetration power of water, thereby improve extraction efficiency, the present invention has designed magnetized water extractor, meanwhile, concentrate and be deposited in setting tank bottom center according to the singularity of precipitin reaction in this extracting method-----polyphenol, designed special setting tank.

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

(1) utilize the lipids such as rare alcohol precipitation ampelopsin and suspension chlorophyll, the lipid such as ampelopsin and chlorophyll is separated, reach the object of removing oil-soluble impurities, remove the water-soluble Polyphenols of part simultaneously; (2) adopt 95% alcohol extraction to go out total flavones and a small amount of polyphenol to the precipitation mixture such as ampelopsin and 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 hot water, most of other flavones, as the Precipitation such as ampelopsin, Quercetin, the second light industry bureau Quercetin, apigenin and kaempferol, adopt this method to separate ampelopsin flavones and Polyphenols in addition; (4) adopt magnetized water circulation method to extract the ampelopsin in material, compare with not adopting magnetized water circulation method, general extractive yield improves more than 30%, and ampelopsin yield can improve more than 5%; (5) adopt the special settling tank with underseal structure, collect Polyphenols precipitation, improve work efficiency.

Brief description of the drawings

Fig. 1 is the structural representation of extractor;

Fig. 2 is setting tank side-view;

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

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

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 precipitation; 7-Polyphenols precipitation (comprising the flavones precipitation except ampelopsin); 8-supernatant liquor; 9-controls motor; 10-transmission shaft; 11-polyphenol precipitation; 12-filter plate; The 13-mouth of pipe.

Embodiment

embodiment 1:

Extractor 1 is with the magnetizing apparatus 2 on water-circulating pump 3 and the water circulating pipe of bidirectional circulating function, and its using method is: add after material, inject pure water by the mouth of pipe 13, then open reversion recycle pump 3, start heating cycle and extract; The bottom of extractor 1 is provided with filter plate 12.The bottom of extractor 1 is promoted to the Liquid extracting of extractor 1 bottom magnetization by recycle pump 3 and magnetizing apparatus 2 top of extractor 1 successively.

Setting tank 4 bottom center are provided with 1/20th to 1/15th the polyphenol settling tank 11 that a layer height is 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 and in the time of closure, play sealed can at the bottom of effect, two described 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 is rendered in the middle of extractor 1, is opened water pump 3, the interface 10 by 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, the water pump that reverses in insulation starts circulation by the water in extractor, water is the filter plate 12 of 0.5-1 millimeter the magnetizing apparatus that is 6000mT by Surface field intensity by extractor bottom part aperture diameter in working cycle, the penetration power of water is strengthened, the composition extractability of vine tea leaf is strengthened, then extract extracting solution out from the mouth of pipe 13 and turn back to extractor, after extraction, extract extracting solution out and put in cooling pool

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

Step 4, in cooling pool, extracting solution naturally cooling is reduced the temperature to 10 DEG C, staticly settle 5 hours, then extract the supernatant liquid in cooling pool out, extract after clear liquid remaining precipitation and be placed on gauze upward filtration solid carbon dioxide and divide;

Step 5, be then 95% food grade ethanol to adding concentration in the precipitation of 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 to step 5 until 3 supernatant liquids of suction filtration repeatedly, the mixture that is 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 in 40% left and right;

Step 7, the industrial rotatory evaporator of clear liquid that step 6 is extracted carries out vacuum concentration and collects concentrated solution when having yellow-white crystallization in evaporator wall again;

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

Step 9, the precipitation that step 8 is collected add 5 times of quality water,

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

Step 11, solution temperature in step 10 drop to two flabellums (5-1,5-2) of closing underseal 5 in 50 DEG C, and underseal 5 the insides are brown precipitation, and this brown precipitation is vine tea Polyphenols precipitation;

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

Step 13, collect yellow-white and be deposited in 80 DEG C of oven dry and can obtain the ampelopsin of 90% above purity, step 14, the ampelopsin that step 13 is obtained add 5 times of quality water again, return to the ampelopsin that step 10 can obtain more than 95% for 2-3 time to the method re-treatment of step 13.

embodiment 2:

Extractor 1 is with the magnetizing apparatus 2 on water-circulating pump 3 and the water circulating pipe of bidirectional circulating function, and its using method is: add after material, inject pure water by the mouth of pipe 13, then open reversion recycle pump 3, start heating cycle and extract; The bottom of extractor 1 is provided with filter plate 12.The bottom of extractor 1 is promoted to the Liquid extracting of extractor 1 bottom magnetization by recycle pump 3 and magnetizing apparatus 2 top of extractor 1 successively.

Setting tank 4 bottom center are provided with 1/20th to 1/15th the polyphenol settling tank 11 that a layer height is 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 and in the time of closure, play sealed can at the bottom of effect, two described 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 is rendered in the middle of extractor 1, is opened water pump 3, the interface 10 by 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, the water pump that reverses in insulation starts circulation by the water in extractor, water is the filter plate 12 of 0.5-1 millimeter the magnetizing apparatus that is 6000mT by Surface field intensity by extractor bottom part aperture diameter in working cycle, the penetration power of water is strengthened, the composition extractability of vine tea leaf is strengthened, then extract extracting solution out from the mouth of pipe 13 and turn back to extractor, after extraction, extract extracting solution out and put into and in cooling pool, be cooled to room temperature.

Step 3, supernatant liquid cooling in step 2 cooling pool is joined in extractor again, return to 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, extracting solution artificial cooling is reduced the temperature to 10 DEG C, staticly settling 10 hours, then extract the supernatant liquid in cooling pool out, extract after clear liquid remaining precipitation and be placed on gauze upward filtration solid carbon dioxide and divide;

Step 5, be then 90% food grade ethanol to adding concentration in the precipitation of 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 to step 5 until 3 supernatant liquids of suction filtration repeatedly, the mixture that is 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 in 35% left and right;

Step 7, the industrial rotatory evaporator of clear liquid that step 6 is extracted carries out vacuum concentration and collects concentrated solution when having yellow-white crystallization in evaporator wall again;

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

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

Step 10, solution temperature in step 10 drop to two flabellums (5-1,5-2) of closing underseal 5 in 50 DEG C, and underseal 5 the insides are brown precipitation, and this brown precipitation is vine tea Polyphenols precipitation;

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

Step 12, collect yellow-white and be deposited in 80 DEG C of oven dry and can obtain the ampelopsin of 90% above purity, step 13, the ampelopsin that step 12 is obtained add 6 times of quality water again, return to the ampelopsin that the method re-treatment of step 9 to 12 can obtain more than 97% for 2-3 time.

embodiment 3

Extractor 1 is with the magnetizing apparatus 2 on water-circulating pump 3 and the water circulating pipe of bidirectional circulating function, and its using method is: add after material, inject pure water by the mouth of pipe 13, then open reversion recycle pump 3, start heating cycle and extract; The bottom of extractor 1 is provided with filter plate 12.The bottom of extractor 1 is promoted to the Liquid extracting of extractor 1 bottom magnetization by recycle pump 3 and magnetizing apparatus 2 top of extractor 1 successively.

Setting tank 4 bottom center are provided with 1/20th to 1/15th the polyphenol settling tank 11 that a layer height is 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 and in the time of closure, play sealed can at the bottom of effect, two described 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 to join extractor to submergence material after 2000-6000mT magnetizing apparatus magnetizes by Surface field intensity, and material is the dry blade of Ampelopsis grossedentata or fresh Ampelopsis grossedentata blade;

Step 2, then boil boil to 95 DEG C insulation 1 hour, in 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, after the magnetizing apparatus 2 that enters Surface field intensity and be 2000-6000mT magnetizes, gets back in extractor, collects extracting solution;

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

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

Step 5, the industrial rotatory evaporator of supernatant liquid that step 4 is extracted carry out vacuum concentration and collect concentrated solution when there is white crystals in evaporator wall;

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

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

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

Step 9, when naturally cooling to 50 DEG C, step 8 isolates bottom brown precipitation;

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

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

Step 12, the ampelopsin that step 11 is obtained add the water of 5-10 times of quality, the ampelopsin that adopts step 8 can obtain 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 amendments or supplement or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.

Claims (1)

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

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

Step 2, then boil boil to 95 DEG C insulation 0.5-1 hour, in 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), enter after the magnetizing apparatus that Surface field intensity is 2000-6000mT (2) magnetizes and get back in extractor, after extraction, collect extracting solution;

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

Step 4, then in the precipitation of collecting to step 3, add concentration to be not less than 95% food grade ethanol, 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, the industrial rotatory evaporator of supernatant liquid that step 4 is extracted carry out vacuum concentration and collect concentrated solution when there is white crystals in evaporator wall;

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

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

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

Step 9, when naturally cooling to 50-60 DEG C, step 8 separates bottom brown precipitation;

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

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

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