CN105832801A - Extraction and separation method for macaenes and maca amides - Google Patents
Extraction and separation method for macaenes and maca amides Download PDFInfo
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- CN105832801A CN105832801A CN201610337869.4A CN201610337869A CN105832801A CN 105832801 A CN105832801 A CN 105832801A CN 201610337869 A CN201610337869 A CN 201610337869A CN 105832801 A CN105832801 A CN 105832801A
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/31—Brassicaceae or Cruciferae (Mustard family), e.g. broccoli, cabbage or kohlrabi
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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Abstract
The invention belongs to the field of biological extraction, and discloses an extraction and separation method for macaenes and maca amides. The method comprises the following steps: (1) impregnation and ultraviolet irradiation; (2) uniform mixing; (3) critical CO2 extraction and concentration; (4) petroleum ether extraction; (5) elution; (6) decolorization, concentration and drying. The extraction and separation method comprises processes of impregnation, extraction, elution, decolorization, concentration and the like, and has the advantages of high yield, high product purity, simple operation process and the like.
Description
Technical field
The invention belongs to field of biological extraction, be specifically related to a kind of Maca alkene, the extraction separation method of macamides.
Background technology
Maca (formal name used at school: Lepidium meyenii Walp), (Spanish: Maca).Mainly produce in South America Andes normal pulse Chinese yunnan Lijing, be a kind of crucifer.Leaf is oval, rhizome likeness in form turnip radish, and edible is a kind of natural food, and nutrition is enriched.The hypocotyl of Maca may be in golden or faint yellow, red, purple, blueness, black or green.Flaxen most common, and shape, taste are preferably also.Maca, rich in high unit nutrient, has the function of nourishing and fit keeping function to human body.Black Maca is to be acknowledged as the Maca that effect is best, and yield is few.Maca originates in High aititude mountain area, suitably grows in High aititude, low latitudes, high day and night temperature, subacidity sandy loam, sun-drenched soil；Plantation area is distributed mainly on the Yulong Xueshan area of Andes, state, South America and Chinese yunnan Lijing, and there is suitable kind of soil of larger area this two big main producing region.And also there is a small amount of plantation in other areas of Chinese yunnan and the area such as Xinjiang, Tibet.
The distinctive two kinds of unique active substances of Maca that Maca Xi Shi U.S. foreign citizen of Chinese origin botanist Zheng B.L finds, it is mainly composed of: n-benzyl 16 phthalein amine, benzyl-(92) octadecylene amide, n-benzyl-(92,122)-diene 18 phthalein amine, benzyl-(92,122,152)-triolefin 18 phthalein amine, n-benzyl kemanide S, and n-benzyl caprylamide, n-benzyl-16-hydroxyl-9-aoxidize-10E 12E
14E-pungent certain herbaceous plants with big flowers three acrylamide, n-benzyl-16 hydroxyl-9,16-dioxy-10E 12E
17 homologues such as 14E-pungent certain herbaceous plants with big flowers three acrylamide.Macamides and Maca alkene content in Maca extract is 0.6%.Macamides and Maca alkene are the main matter causing improvement of sexual function, and abundant aminoacid can help human body to transmit information in nervus centralis, has important regulating and controlling effect especially to sexual activity.
At present, there are some researchs to do the extraction work of some macamides and Maca alkene, but mostly have that extraction efficiency is low, a defect such as purity difference and complex process, be not suitable for large-scale industrial production.
Summary of the invention
Present invention aim to address in prior art macamides and the defect such as Maca alkene extraction process extraction ratio is low, extraction cost is high and operating procedure is loaded down with trivial details, it is provided that a kind of Maca alkene, the extraction separation method of macamides.
The present invention is achieved by the following technical solution:
A kind of Maca alkene, the extraction separation method of macamides, it comprises the steps: that step 1) is soaked and ultra-vioket radiation, step 2) mixing, the critical CO of step 3)2Extraction and concentration, step 4) petroleum ether extraction, step 5) eluting, step 6) is decoloured, is concentrated and be dried.
Specifically, described extraction separation method comprises the steps:
Step 1) is soaked and ultra-vioket radiation: taking fresh of Maca be raw material, cleans, is immersed in 6%(w/w) sodium chloride solution in 6 hours, then take out, dry, be ground into the powder of 8-10 mesh, then with ultraviolet irradiation 15 minutes；
Step 2) mixing: the powder of step 1) is obtained mixture according to the quality of 1:1 than mixing homogeneously with kieselguhr；
The critical CO of step 3)2Extraction and concentration: use critical CO2Extraction mode, the ethanol with 95% is 27.5-29.5MPa as entrainer, control extracting pressure, and extraction time is 3-4 hour, and extraction temperature is 40 DEG C；Repeating to extract once, merge twice extract, be placed in vacuum evaporator, be 0.82MPa in vacuum, temperature is evaporated being concentrated to give concentrated solution under conditions of being 43 DEG C；
Step 4) petroleum ether extraction: add the petroleum ether of double weight in concentrated solution, at 60-90 DEG C of extraction, then stratification, collects the aqueous phase extraction for polysaccharose substance of lower floor；
Step 5) eluting: be evaporated under reduced pressure mutually by step 4) gained upper strata petroleum ether, reclaims petroleum ether, and debris compares mixing and stirring with alumina powder according to the quality of 1:1, dry, it is then added to aluminium oxide eluting post, carries out eluting with petroleum ether, collect eluent；
Step 6) decolouring, concentrate and be dried: toward eluent in, add 3%(w/w) activated carbon, keep decolouring 40min at reflux, filtration, concentrated filtrate, then dry 2 hours at 40-60 DEG C, obtain containing Maca alkene, the extract of macamides.
Preferably, the intensity of described ultraviolet is 2000uW/cm2。
Described diatomaceous particle diameter is 50-100 mesh.
The particle diameter of described alumina powder is 100-200 mesh.
The present invention obtain beneficial effect be primarily but not limited to following some:
Extraction process of the present invention, by immersion, extraction, eluting, decolours and the technique such as concentration, has the advantages such as yield height, good product purity, operating procedure are simple；
The present invention uses critical CO2The mode that extraction mode and petroleum ether combine, improves yield, it is to avoid the loss of effective components that single mode causes；
Extraction process use kieselguhr mix with Maca powder, diatomaceous adsorption can be passed through, cell wall stabilization is declined further, cell spalling process is aggravated, improving the leaching rate of active component, absorption affinity is less simultaneously, easily dissociates, and diatomaceous cost is less than adsorbing materials such as resins, alleviates business burden；
Maca cell, through salt environment and intensive ultraviolet environment stress, with the secretion of induced activity molecule, and can make cell wall play pendulum, and the leaching of the alkaloids such as Maca alkene, macamides increases accordingly, improves yield；
Alumina powder is used for the removal of impurity, improves the purity of product；
Using extraction separation method cost of the present invention relatively low, and solvent consumption is few with low cost, product purity and yield are high, and extraction time shortens, and operating procedure is simple, and industrial applications has a extensive future.
Detailed description of the invention
For the technical scheme making those skilled in the art be more fully understood that in the application, below in conjunction with the application specific embodiment, the present invention is more clearly and completely described, it is clear that, described embodiment is only some embodiments of the present application rather than whole embodiments.Based on the embodiment in the application, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, all should belong to the scope of protection of the invention.
Embodiment 1
A kind of Maca alkene, the extraction separation method of macamides, it comprises the steps:
Step 1): fresh of the Maca (moisture content 57%) taking Lijing Maca growing area is raw material 1000g, clean, be immersed in 6%(w/w) sodium chloride solution in 6 hours, then take out, dry, be ground into the powder of 8 mesh, irradiating 15 minutes with ultraviolet, uitraviolet intensity is 2000uW/cm again2；
Step 2): the powder of step 1) is obtained mixture according to the quality of 1:1 than mixing homogeneously with kieselguhr；Described diatomaceous particle diameter is 50 mesh；
Step 3): use critical CO2Extraction mode, the ethanol with 95% is 27.5MPa as entrainer, control extracting pressure, and extraction time is 3 hours, and extraction temperature is 40 DEG C；Repeating identical extraction conditions to extract once again, merge twice extract, be placed in vacuum evaporator, be 0.82MPa in vacuum, temperature is evaporated being concentrated to give concentrated solution under conditions of being 43 DEG C；
Step 4): add the petroleum ether of double weight in concentrated solution, at 60 DEG C of extractions, then stratification, collects the aqueous phase extraction for polysaccharose substance of lower floor；
Step 5): upper strata petroleum ether is evaporated under reduced pressure mutually, reclaims petroleum ether, and debris compares mixing and stirring with alumina powder according to the quality of 1:1, dry, be then added to aluminium oxide eluting post, to be preferred away from opening part 40cm, carry out eluting with petroleum ether, collect eluent；
Step 6): in eluent add 3%(w/w) activated carbon, at reflux keep decolouring 40min, filter, concentrated filtrate, then 40 DEG C be dried 2 hours, obtain containing Maca alkene, the extract of macamides.
Obtaining Maca extract 69.2g altogether, detect through HPLC, Maca alkene content is 1.71%, and macamides content is 0.023%.
Embodiment 2
A kind of Maca alkene, the extraction separation method of macamides, it comprises the steps:
Step 1): fresh of the Maca (moisture content 58%) taking Lijing Maca growing area is raw material 1000g, clean, be immersed in 6%(w/w) sodium chloride solution in 6 hours, then take out, dry, be ground into the powder of 10 mesh, irradiating 15 minutes with ultraviolet, uitraviolet intensity is 2000uW/cm again2；
Step 2): the powder of step 1) is obtained mixture according to the quality of 1:1 than mixing homogeneously with kieselguhr；Described diatomaceous particle diameter is 100 mesh；
Step 3): use critical CO2Extraction mode, the ethanol with 95% is 29.5MPa as entrainer, control extracting pressure, and extraction time is 4 hours, and extraction temperature is 40 DEG C；Repeating identical extraction conditions to extract once again, merge twice extract, be placed in vacuum evaporator, be 0.82MPa in vacuum, temperature is evaporated being concentrated to give concentrated solution under conditions of being 43 DEG C；
Step 4): add the petroleum ether of double weight in concentrated solution, at 80 DEG C of extractions, then stratification, collects the aqueous phase extraction for polysaccharose substance of lower floor；
Step 5): upper strata petroleum ether is evaporated under reduced pressure mutually, reclaims petroleum ether, and debris compares mixing and stirring with alumina powder according to the quality of 1:1, dry, be then added to aluminium oxide eluting post, to be preferred away from opening part 40cm, carry out eluting with petroleum ether, collect eluent；
Step 6): in eluent add 3%(w/w) activated carbon, at reflux keep decolouring 40min, filter, concentrated filtrate, then 60 DEG C be dried 2 hours, obtain containing Maca alkene, the extract of macamides.
Obtaining Maca extract 67.8g altogether, detect through HPLC, Maca alkene content is 1.76%, and macamides content is 0.021%.
Comparative example 1
Operating procedure is with embodiment 1, and difference is that lacking step 1) is dipped into the step of sodium chloride solution and ultra-vioket radiation；Obtaining Maca extract 68.2g altogether, in HPLC Detection and Extraction thing, Maca alkene content is 1.08%, and macamides content is 0.013%.
Comparative example 2
Operating procedure is with embodiment 1, and difference is to lack step 2)；Obtaining Maca extract 68.6g altogether, in HPLC Detection and Extraction thing, Maca alkene content is 1.54%, and macamides content is 0.018%.
Finally, in addition it is also necessary to be only several specific embodiments of the present invention it is noted that listed above.It is clear that the invention is not restricted to above example, it is also possible to there are many deformation.All deformation that those of ordinary skill in the art can directly derive from present disclosure or associate, are all considered as protection scope of the present invention.
Claims (4)
1. an extraction separation method for Maca alkene, macamides, it comprises the steps: that step 1) is soaked and ultra-vioket radiation, step 2) mixing, the critical CO of step 3)2Extraction and concentration, step 4) petroleum ether extraction, step 5) eluting, step 6) is decoloured, is concentrated and be dried.
Extraction separation method the most according to claim 1, it is characterised in that described extraction separation method comprises the steps:
Step 1) is soaked and ultra-vioket radiation: taking fresh of Maca be raw material, cleans, is immersed in 6%(w/w) sodium chloride solution in 6 hours, then take out, dry, be ground into the powder of 8-10 mesh, then with ultraviolet irradiation 15 minutes；
Step 2) mixing: the powder of step 1) is obtained mixture according to the quality of 1:1 than mixing homogeneously with kieselguhr；
The critical CO of step 3)2Extraction and concentration: use critical CO2Extraction mode, the ethanol with 95% is 27.5-29.5MPa as entrainer, control extracting pressure, and extraction time is 3-4 hour, and extraction temperature is 40 DEG C；Repeating to extract once, merge twice extract, be placed in vacuum evaporator, be 0.82MPa in vacuum, temperature is evaporated being concentrated to give concentrated solution under conditions of being 43 DEG C；
Step 4) petroleum ether extraction: add the petroleum ether of double weight in concentrated solution, at 60-90 DEG C of extraction, then stratification, collects the aqueous phase extraction for polysaccharose substance of lower floor；
Step 5) eluting: be evaporated under reduced pressure mutually by step 4) gained upper strata petroleum ether, reclaims petroleum ether, and debris and alumina powder than mixing and stirring according to the quality of 1:1, dry, are then added to eluting post, carry out eluting with petroleum ether, collect eluent；
Step 6) decolouring, concentrate and be dried: toward eluent in, add 3%(w/w) activated carbon, keep decolouring 40min at reflux, filtration, concentrated filtrate, then dry 2 hours at 40-60 DEG C, obtain containing Maca alkene, the extract of macamides.
Extraction separation method the most according to claim 2, it is characterised in that the intensity of described ultraviolet is 2000uW/cm2。
Extraction separation method the most according to claim 2, it is characterised in that described diatomaceous particle diameter is 50-100 mesh.
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Cited By (1)
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| CN114671755A (en) * | 2022-04-24 | 2022-06-28 | 陕西嘉禾生物科技股份有限公司 | Preparation method of high-content macaene |
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