Background technology
Lepidinm meyenii Walp (Maca) has another name called Peruvian ginseng, maka etc., the annual or 2 years raw herbaceous plant in South America, belong to Cruciferae (Cruciferae) separate row Vegetable spp (Lepidium L), concrete kind is also disputable, generally believe in the world, Lepidium meyenii Walp and Lepidium peruvianum Chacon two kinds almost do not have difference on growth and breeding, phytochemistry and health-care effect, are therefore collectively referred to as " Maca " (transliteration is " Lepidinm meyenii Walp ").Lepidinm meyenii Walp has had the cultivation history of several thousand in mountain area, Andean, South America. and be one of indispensable crop.There is good health-care effect.
Lepidinm meyenii Walp alkaloid can improve the quantity of the quantity of animal mature follicle corpusculum, the mobility of sperm and sperm, thus can significantly improve the fertility of mammal and Fish.And the alkaloid in Lepidinm meyenii Walp can act on hypothalamus and hypophysis cerebri, there is endocrine regulation gland as functions such as adrenal gland, thyroid, pancreas, ovaries, thus balance hormone, thus can with giving treatment female climacteric syndrome.
Common alkaloid extracting method has sour water direct extraction method, infusion process, oozes rumble method, hot cocurrent flow method, supersound extraction etc.At present, only have about the alkaloidal supersound extraction of Lepidinm meyenii Walp.Therefore, adopt conventional plant supercritical ultrasonics technology process Lepidinm meyenii Walp, the alkaloidal productive rate of Lepidinm meyenii Walp is lower, causes that existing Lepidinm meyenii Walp alkaloid cost is high and health-care effect is not obvious.
The ultrasound wave of prior art is lower to Maca reactive constituents extraction efficiency, and mainly because the wall mechanical intensity of Lepidinm meyenii Walp tuber cell is higher, the mechanical activation comminution breaking cellular wall efficiency of general cutting type is low, causes a large amount of cell inclusions to be intercepted by cell wall.First the present invention applies pressure-air to granule, and again at abrupt release pressure, make individual cells instantaneous expansion and cell wall is burst, cellular content ejects in a large number.Prior art has employing to be filled with ammonia to make raw material inflated with low pressure at a higher temperature and realize shell-broken effect, but for Lepidinm meyenii Walp raw material, high temperature likely makes active substance distortion wherein, also likely makes wherein volatile Lepidinm meyenii Walp alkene, Semen Sinapis wet goods substance escaping, loss.After tested, pass into the unstability that ammonia contributes to improving cell wall, it is more violent that the expansion made it bursts process, also contributes to the volatilization efficiency reducing Lepidinm meyenii Walp alkene, mustard oil, improve the productive rate of Lepidinm meyenii Walp alkene and Semen Sinapis wet goods.Sodium citrate can ensure breaking cellular wall product stand ammonia corrosion after stability, especially can avoid reactive protein inactivation wherein.Described sodium citrate-alcohol mixture is the mixture of the sodium citrate of 2 ~ 3 parts by weight and the ethanol of 60 ~ 90 parts.Grain (partly) footpath is that the granule of 0.2 ~ 0.5mm is easy to processing by prior art, and more cellulous cell wall can be made to expose in atmosphere.Described container can select the steam-explosion jar of prior art.Ultrasonic extraction in the present invention can select any one ultrasonic extraction equipment to realize, and common ultrasonic extraction also can be adopted to realize.Utilize repeated ultrasonic ripple to extract, obviously can promote the Maca reactive composition especially alkaloidal productive rate of Lepidinm meyenii Walp.Because the activity component concentration in different extraction time materials is different, sets different extraction conditions, can obtain the highest productive rate under minimum cost through multiple authentication the present invention, product has the highest biological activity simultaneously.Especially, the high pressure limit in container is decided to be 0.5 ~ 0.7Mpa of gauge pressure by the present invention.Upon discharge, volatile Lepidinm meyenii Walp alkene is by the loss of pressure along with release, and too low pressure cannot thorough fracturing cell walls for too high pressure.But in the present invention, the cell wall through ammonia process is easy to broken, thus is minimized the pressure in container, prevents the loss of volatile substances.The input quantity of ammonia can be preferably 1.3 ~ 2.5 times of vessel volume.
Further, Aging storage in described S6 adds 1 ~ 6 part of Aloe root system suspension in the filtrate pointing to 50 ~ 70 parts by weight, add 2 ~ 8 parts of vitamin Cs, 10 ~ 17 parts of glucoses, 2 ~ 15 parts of ethanol simultaneously, in sealed container, within 5th ~ 21, obtain Lepidinm meyenii Walp bioactive ingredients product afterwards with 35 ~ 45 DEG C of anoxybiotic process.After-ripening step can improve the biological activity of product, improves the Lepidinm meyenii Walp aromatic odor in product.The secretions of Aloe root system and microorganism contribute to the carrying out of after-ripening step.
Further, described Aloe root system suspension is the Radix of Aloe of 10 ~ 19 parts by weight, pulverizing is that the segment of 1 ~ 3mm is immersed in 20 ~ 40 parts of sterilized water and 2 ~ 15 parts of particle diameters are in the bead of 1mm, filters the filtrate of acquisition after adopting rotary shaker to vibrate 6 minutes under the speed of 200 ~ 250 turns/min.
Radix of Aloe be cut into segment and adopt bead to extrude, contributing to the release of above-mentioned secretions.
Described Radix of Aloe is the fresh aloe root of prior art, and its weight is fresh weight.
Particularly preferred, described operation S1 pre-treatment Lepidinm meyenii Walp tuber refers to and carries out 5 brittle operations of low temperature cell wall to Lepidinm meyenii Walp tuber; The brittle operation of described low temperature cell wall is specially is down to-9 ~-5 DEG C by the temperature of Lepidinm meyenii Walp tuber in 60s, after maintenance 30min, the mass fraction be immersed in containing 30 ~ 40 DEG C of constant temperature is 60min in the sodium chloride solution of 0.01%, and it is the acetic acid solution of 6% that every kilogram of Lepidinm meyenii Walp tuber sprays 3 ~ 6g mass fraction.
Under cryogenic, intracellular Free water will condense into trickle ice crystal and puncture cell membrane and cell wall.And without the materials such as cholesterol plant cell membrane at low temperatures mobility decline, brittle, easily broken.Especially, after acetic acid and sodium chloride process, also and easily damaged under low temperature repeatedly, the stress making cell wall occur that slight crack fills bears some the cell wall of Lepidinm meyenii Walp, is conducive to the thorough fragmentation of cell wall in follow-up breaking cellular wall operation.
Summary of the invention
In view of this, the present invention discloses a kind of extraction process that significantly can improve Lepidinm meyenii Walp alkaloid productive rate, reduce Maca reactive composition production cost, strengthen Lepidinm meyenii Walp bioactive ingredients physiological function.
Object of the present invention is achieved through the following technical solutions:
Based on the method for ultrasonic extraction Lepidinm meyenii Walp bioactive ingredients, comprise following operation:
S1. pre-treatment Lepidinm meyenii Walp tuber;
S2. described Lepidinm meyenii Walp tuber is pulverized for granule;
S3. broken wall treatment is carried out to described granule, obtain breaking cellular wall product;
S4. ultrasonic extraction process breaking cellular wall product is adopted; Collecting by filtration filtrate, obtains the first filtrate;
S5. collect filtering residue, and adopt purified water lixiviate 90 ~ 150min, collecting by filtration filtrate, obtain the second filtrate;
S6. mix described first filtrate and the second filtrate, obtain Lepidinm meyenii Walp bioactive ingredients product through Aging storage.
Pre-treatment alleged by S1 comprises the conventional pre-treatment step of prior art, as clean, dry etc.Lepidinm meyenii Walp tuber alleged by the present invention is the commercially available prod of water content at 50wt% ~ 75wt%.S2 can adopt any one existing techniques in realizing, as existing beater grinder.Pulverize raw-material tuber for granule, be conducive to the specific surface area increasing raw material, in follow-up broken wall treatment, having larger area bears the rising of pressure and reduces instantaneously, thus improves breaking cellular wall efficiency.Through the raw material of broken wall treatment, the Lepidinm meyenii Walp alkaloid of ultrasonic extraction, macamide, activated protein productive rate are far above the ultrasonic extraction of prior art.And the filtering residue after ultrasonic extraction uses hydro-thermal method lixiviate further, active component remaining in filtering residue thoroughly can be extracted under lower-cost prerequisite, improve the utilization rate of raw material, waste can be reduced and effectively control the production cost of Maca reactive composition in large-scale production and application.Aging storage can be leave standstill, lucifuge preservation 20 ~ 30 days.Broken wall treatment also can adopt any one plant wall breaking technology to realize.
Further, described broken wall treatment refers to the container described granule being placed in sealing, passes into the ammonia equal with vessel volume, and heating container maintains 3 ~ 5min to container Nei Wenduda 60 ~ 65 DEG C; Stop ammonia, and be 0.5 ~ 0.7Mpa to inputting gauge pressure in pressure-air to container in container and maintain 60 ~ 130 seconds, in 0.5 ~ 1 second, the gauge pressure in container is reduced to 0pa; Adopt volume to be vessel volume 40% ~ 80% sodium citrate and alcohol mixture eluant container, collect flushing thing and be described breaking cellular wall product;
The particle diameter of described granule is 0.2 ~ 0.5mm;
Further, adopt ultrasonic extraction process breaking cellular wall product to refer to described breaking cellular wall product and quality to be that its ethanol of 2 ~ 5 times mixes, after being heated to 30 ~ 40 DEG C, adopt the ultrasonic extraction 30 ~ 50min of 80KHz, after filtration, three multiple extractions are carried out to filtering residue; Described multiple extract refer to adopt quality be the ethanol of filtering residue 3 ~ 5 times at 50 ~ 80 DEG C with the ultrasonic extraction 90 ~ 140min of 60KHz; Merging filtrate obtains described first filtrate.
Detailed description of the invention
The present invention to be described in further detail below in conjunction with embodiment for the ease of it will be appreciated by those skilled in the art that:
Embodiment 1
The present embodiment provides a kind of method based on ultrasonic extraction Lepidinm meyenii Walp bioactive ingredients, comprises following operation:
S1. pre-treatment Lepidinm meyenii Walp tuber;
S2. above-mentioned Lepidinm meyenii Walp tuber is pulverized for granule;
S3. broken wall treatment is carried out to above-mentioned granule, obtain breaking cellular wall product;
S4. ultrasonic extraction process breaking cellular wall product is adopted; Collecting by filtration filtrate, obtains the first filtrate;
S5. collect filtering residue, and adopt purified water lixiviate 125min, collecting by filtration filtrate, obtain the second filtrate;
S6. mix above-mentioned first filtrate and the second filtrate, obtain Lepidinm meyenii Walp bioactive ingredients product through Aging storage.
Above-mentioned broken wall treatment refers to the container above-mentioned granule being placed in sealing, passes into ammonia, and heating container maintains 4min to container Nei Wenduda 60 DEG C; Stop input ammonia, and be 0.6Mpa to inputting gauge pressure in pressure-air to container in container and maintain 90 seconds, in 0.5 second, the gauge pressure in container is reduced to 0pa; Adopt alcohol flushing container, collect flushing thing and be above-mentioned breaking cellular wall product;
The particle diameter of above-mentioned granule is 0.4mm;
Adopt ultrasonic extraction process breaking cellular wall product to refer to above-mentioned breaking cellular wall product and quality to be that its ethanol of 3 times mixes, after being heated to 35 DEG C, adopt the ultrasonic extraction 45min of 80KHz, after filtration, three multiple extractions are carried out to filtering residue; Above-mentioned multiple extract refer to adopt quality be the ethanol of filtering residue 4 times at 60 DEG C with the ultrasonic extraction 100min of 60KHz; Merging filtrate obtains above-mentioned first filtrate.
Aging storage in above-mentioned S6 adds 3 parts of Aloe root system suspensions in the filtrate pointing to 55 parts by weight, add 7 parts of vitamin Cs, 12 parts of glucoses, 9 parts of ethanol simultaneously, in sealed container, within 14th, obtain Lepidinm meyenii Walp bioactive ingredients product afterwards with 40 DEG C of anoxybiotic process.
Above-mentioned Aloe root system suspension is the Radix of Aloe of 17 parts by weight, and the segment pulverized as 3mm is immersed in 30 parts of sterilized water and 8 parts of particle diameters are in the bead of 1mm, filters the filtrate of acquisition after adopting rotary shaker to vibrate 6 minutes under the speed of 250 turns/min.Above-mentioned operation S1 pre-treatment Lepidinm meyenii Walp tuber refers to and carries out 5 brittle operations of low temperature cell wall to Lepidinm meyenii Walp tuber; The brittle operation of above-mentioned low temperature cell wall is specially is down to-9 ~-5 DEG C by the temperature of Lepidinm meyenii Walp tuber in 60s, after maintenance 30min, the mass fraction be immersed in containing 30 ~ 40 DEG C of constant temperature is 60min in the sodium chloride solution of 0.01%, and it is the acetic acid solution of 6% that every kilogram of Lepidinm meyenii Walp tuber sprays 3 ~ 6g mass fraction.
In the present embodiment, 1 part is 1kg.Adopt the Lepidinm meyenii Walp tuber (water content 70wt%) of 60 parts, through the concentrated product finally preparing 73.25kg, wherein Lepidinm meyenii Walp alkaloid is 327g after measured, and Lepidinm meyenii Walp alkene content is 109g, and macamide is 0.999g, polysaccharide 538.39g, glucosinolate 981g.
Embodiment 2
The present embodiment provides a kind of method based on ultrasonic extraction Lepidinm meyenii Walp bioactive ingredients, comprises following operation:
S1. pre-treatment Lepidinm meyenii Walp tuber;
S2. above-mentioned Lepidinm meyenii Walp tuber is pulverized for granule;
S3. broken wall treatment is carried out to above-mentioned granule, obtain breaking cellular wall product;
S4. ultrasonic extraction process breaking cellular wall product is adopted; Collecting by filtration filtrate, obtains the first filtrate;
S5. collect filtering residue, and adopt purified water lixiviate 150min, collecting by filtration filtrate, obtain the second filtrate;
S6. mix above-mentioned first filtrate and the second filtrate, obtain Lepidinm meyenii Walp bioactive ingredients product through Aging storage.
Above-mentioned broken wall treatment refers to the container above-mentioned granule being placed in sealing, passes into ammonia, and heating container maintains 5min to container Nei Wenduda 60 DEG C; Stop input ammonia, and be 0.5Mpa to inputting gauge pressure in pressure-air to container in container and maintain 130 seconds, in 0.5 second, the gauge pressure in container is reduced to 0pa; Adopt alcohol flushing container, collect flushing thing and be above-mentioned breaking cellular wall product;
The particle diameter of above-mentioned granule is 0.5mm;
Adopt ultrasonic extraction process breaking cellular wall product to refer to above-mentioned breaking cellular wall product and quality to be that its ethanol of 2 times mixes, after being heated to 40 DEG C, adopt the ultrasonic extraction 30min of 80KHz, after filtration, three multiple extractions are carried out to filtering residue; Above-mentioned multiple extract refer to adopt quality be the ethanol of filtering residue 5 times at 50 DEG C with the ultrasonic extraction 140min of 60KHz; Merging filtrate obtains above-mentioned first filtrate.
Aging storage in above-mentioned S6 adds 6 parts of Aloe root system suspensions in the filtrate pointing to 50 parts by weight, add 2 parts of vitamin Cs, 17 parts of glucoses, 2 parts of ethanol simultaneously, in sealed container, within 5th, obtain Lepidinm meyenii Walp bioactive ingredients product afterwards with 45 DEG C of anoxybiotic process.
Above-mentioned Aloe root system suspension is the Radix of Aloe of 19 parts by weight, and the segment pulverized as 1mm is immersed in 40 parts of sterilized water and 2 parts of particle diameters are in the bead of 1mm, filters the filtrate of acquisition after adopting rotary shaker to vibrate 6 minutes under the speed of 250 turns/min.
In the present embodiment, 1 part is 1kg.Adopt the Lepidinm meyenii Walp tuber (water content 70wt%) of 60 parts, through the concentrated product finally preparing 75.69kg, wherein Lepidinm meyenii Walp alkaloid (total alkali after measured, acetic acid titration) content is 277.20g, Lepidinm meyenii Walp alkene content is 98.11g, macamide is 1.237g, polysaccharide 529.82g, glucosinolate 997.83g.
Embodiment 3
The present embodiment provides a kind of method based on ultrasonic extraction Lepidinm meyenii Walp bioactive ingredients, comprises following operation:
S1. pre-treatment Lepidinm meyenii Walp tuber;
S2. above-mentioned Lepidinm meyenii Walp tuber is pulverized for granule;
S3. broken wall treatment is carried out to above-mentioned granule, obtain breaking cellular wall product;
S4. ultrasonic extraction process breaking cellular wall product is adopted; Collecting by filtration filtrate, obtains the first filtrate;
S5. collect filtering residue, and adopt purified water lixiviate 90min, collecting by filtration filtrate, obtain the second filtrate;
S6. mix above-mentioned first filtrate and the second filtrate, obtain Lepidinm meyenii Walp bioactive ingredients product through Aging storage.
Above-mentioned broken wall treatment refers to the container above-mentioned granule being placed in sealing, passes into ammonia, and heating container maintains 3min to container Nei Wenduda 65 DEG C; Stop input ammonia, and be 0.7Mpa to inputting gauge pressure in pressure-air to container in container and maintain 60 seconds, in 1 second, the gauge pressure in container is reduced to 0pa; Adopt alcohol flushing container, collect flushing thing and be above-mentioned breaking cellular wall product;
The particle diameter of above-mentioned granule is 0.2mm;
Adopt ultrasonic extraction process breaking cellular wall product to refer to above-mentioned breaking cellular wall product and quality to be that its ethanol of 5 times mixes, after being heated to 30 DEG C, adopt the ultrasonic extraction 50min of 80KHz, after filtration, three multiple extractions are carried out to filtering residue; Above-mentioned multiple extract refer to adopt quality be the ethanol of filtering residue 3 times at 80 DEG C with the ultrasonic extraction 90min of 60KHz; Merging filtrate obtains above-mentioned first filtrate.
Aging storage in above-mentioned S6 adds 1 part of Aloe root system suspension in the filtrate pointing to 70 parts by weight, add 8 parts of vitamin Cs, 10 parts of glucoses, 15 parts of ethanol simultaneously, in sealed container, within 21st, obtain Lepidinm meyenii Walp bioactive ingredients product afterwards with 35 DEG C of anoxybiotic process.
Above-mentioned Aloe root system suspension is the Radix of Aloe of 10 parts by weight, and the segment pulverized as 3mm is immersed in 20 parts of sterilized water and 15 parts of particle diameters are in the bead of 1mm, filters the filtrate of acquisition after adopting rotary shaker to vibrate 6 minutes under the speed of 200 turns/min.
In the present embodiment, 1 part is 1kg.Adopt the Lepidinm meyenii Walp tuber (water content 70wt%) of 60 parts, through the concentrated product finally preparing 74.75kg, wherein Lepidinm meyenii Walp alkaloid is 309g after measured, and Lepidinm meyenii Walp alkene content is 87g, and macamide is 0.952g, polysaccharide 511.47g, glucosinolate 961g.
Embodiment 4
The present embodiment provides a kind of method based on ultrasonic extraction Lepidinm meyenii Walp bioactive ingredients, comprises following operation:
S1. pre-treatment Lepidinm meyenii Walp tuber;
S2. above-mentioned Lepidinm meyenii Walp tuber is pulverized for granule;
S3. broken wall treatment is carried out to above-mentioned granule, obtain breaking cellular wall product;
S4. ultrasonic extraction process breaking cellular wall product is adopted; Collecting by filtration filtrate, obtains the first filtrate;
S5. collect filtering residue, and adopt purified water lixiviate 125min, collecting by filtration filtrate, obtain the second filtrate;
S6. mix above-mentioned first filtrate and the second filtrate, obtain Lepidinm meyenii Walp bioactive ingredients product through Aging storage.
Above-mentioned pre-treatment is carry out conventional cleaning, be dried to water content being 70wt% to fresh Lepidinm meyenii Walp tuber.Above-mentioned broken wall treatment refers to the container above-mentioned granule being placed in sealing, passes into ammonia, and heating container maintains 4min to container Nei Wenduda 60 DEG C; Stop input ammonia, and be 0.6Mpa to inputting gauge pressure in pressure-air to container in container and maintain 90 seconds, in 0.5 second, the gauge pressure in container is reduced to 0pa; Adopt alcohol flushing container, collect flushing thing and be above-mentioned breaking cellular wall product;
The particle diameter of above-mentioned granule is 0.4mm;
Adopt ultrasonic extraction process breaking cellular wall product to refer to above-mentioned breaking cellular wall product and quality to be that its ethanol of 3 times mixes, after being heated to 35 DEG C, adopt the ultrasonic extraction 45min of 80KHz, after filtration, three multiple extractions are carried out to filtering residue; Above-mentioned multiple extract refer to adopt quality be the ethanol of filtering residue 4 times at 60 DEG C with the ultrasonic extraction 100min of 60KHz; Merging filtrate obtains above-mentioned first filtrate.
In the present embodiment, 1 part is 1kg.Adopt the Lepidinm meyenii Walp tuber (water content 70wt%) of 60 parts, through the concentrated product finally preparing 73.25kg, wherein Lepidinm meyenii Walp alkaloid is 265g after measured, and Lepidinm meyenii Walp alkene content is 65g, and macamide is 0.907g, polysaccharide 458.39g, glucosinolate 710g.
Embodiment 5
The present embodiment provides a kind of method based on ultrasonic extraction Lepidinm meyenii Walp bioactive ingredients, comprises following operation:
S1. pre-treatment Lepidinm meyenii Walp tuber;
S2. above-mentioned Lepidinm meyenii Walp tuber is pulverized for granule;
S3. broken wall treatment is carried out to above-mentioned granule, obtain breaking cellular wall product;
S4. ultrasonic extraction process breaking cellular wall product is adopted; Collecting by filtration filtrate, obtains the first filtrate;
S5. collect filtering residue, and adopt purified water lixiviate 125min, collecting by filtration filtrate, obtain the second filtrate;
S6. mix above-mentioned first filtrate and the second filtrate, obtain Lepidinm meyenii Walp bioactive ingredients product through Aging storage.
Above-mentioned broken wall treatment is that pressure-air is pulverized.
Aging storage in above-mentioned S6 adds 3 parts of Aloe root system suspensions in the filtrate pointing to 55 parts by weight, add 7 parts of vitamin Cs, 12 parts of glucoses, 9 parts of ethanol simultaneously, in sealed container, within 14th, obtain Lepidinm meyenii Walp bioactive ingredients product afterwards with 40 DEG C of anoxybiotic process.
Above-mentioned Aloe root system suspension is the Radix of Aloe of 17 parts by weight, and the segment pulverized as 3mm is immersed in 30 parts of sterilized water and 8 parts of particle diameters are in the bead of 1mm, filters the filtrate of acquisition after adopting rotary shaker to vibrate 6 minutes under the speed of 250 turns/min.
Adult male mice (body weight 113.11 ± 5.72g) is divided into 6 groups, often organizes 50, often group gavage feeding embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 and normal saline respectively, feeding dosage is 0.5g.Feeding process lasts 50 days.Mice takes food food and water since the childhood.
Often group chooses 30 mices, orders about its swimming, test mouse blood sugar concentration after 120min in being gone in off the deep end.And test the rate of increase of Mouse Weight in 50 days.Its result is as shown in table 1.
Table 1 mouse test results
Be more than wherein specific implementation of the present invention, it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these apparent replacement forms all belong to protection scope of the present invention.