CN106176610A - A kind of preparation method of Lepidinm meyenii Walp fine powder - Google Patents
A kind of preparation method of Lepidinm meyenii Walp fine powder Download PDFInfo
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- CN106176610A CN106176610A CN201610655384.XA CN201610655384A CN106176610A CN 106176610 A CN106176610 A CN 106176610A CN 201610655384 A CN201610655384 A CN 201610655384A CN 106176610 A CN106176610 A CN 106176610A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
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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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- 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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- 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
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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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
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
The present invention discloses the preparation method of a kind of Lepidinm meyenii Walp fine powder, comprises the following steps that: pulverize → extract → centrifugal → evaporation → be spray-dried.Gained Lepidinm meyenii Walp product of the present invention, rich in macamide and Lepidinm meyenii Walp alkene, it is possible to ensures that its content is identical, effect consistent, and prevents from quickly volatilizing such that it is able to reaches substantially efficiently to utilize the advantage of Lepidinm meyenii Walp.The activity substance content of gained Lepidinm meyenii Walp fine powder is high, saves the time again, conservation and the energy.The Lepidinm meyenii Walp fine powder obtained can reach following quality index: fine maca opaque figureofmerit table Lepidinm meyenii Walp alkene >=1.0%, macamide >=2.0%.
Description
Technical field
The present invention relates to the preparation method of a kind of Lepidinm meyenii Walp fine powder.
Background technology
Lepidinm meyenii Walp (Lepidium meyeniiWalp., Maca) it is derived from the Andean a kind of cruciate flower of South America
Section plant, suitably grows in High aititude, low latitudes, high day and night temperature, subacidity sandy loam, sun-drenched soil, is introduced into
There is the plantation of larger area in the area such as Yunnan Province of China, Xinjiang, 2015, only just exceedes at Lijiang, yunnan Lepidinm meyenii Walp industrial base area
140000 mu.Lepidinm meyenii Walp is a kind of pure natural medicine food dual-purpose raw material, and it is nutritious, has the reputation of " South America Radix Ginseng ".
The Lepidinm meyenii Walp of plantation, after collection, needs to be dried in time into dry product raw material, is prepared as product as early as possible, and seals preservation,
The volatilization of effective ingredient can be prevented.This respect, existing relevant criterion: DB53/T 655 Lepidinm meyenii Walp raw material authentication technique specification and DBS
53/001 Lepidinm meyenii Walp dry products.At present, Lepidinm meyenii Walp dry products is made generally in compression forms, such as Publication No. " CN104920762A ", name
It is referred to as the application for a patent for invention of " a kind of Rhizoma Polygonati Lepidinm meyenii Walp pressed candy and preparation method thereof ", Publication No. " CN104687048A ", name
It is referred to as the application for a patent for invention of " a kind of Lepidinm meyenii Walp tabletting and preparation method thereof ", and Publication No. " CN105394766A ", title
For the application for a patent for invention of " a kind of Ricipe for health care food containing Lepidinm meyenii Walp and preparation method ", all use Lepidinm meyenii Walp dry product raw material powder
The method of broken compounding tabletting.Above-mentioned tabletting prepares form, safety and sanitation, food as the one of health product and food
With convenient, nutrition and have the effective ingredient such as material of special efficacy to be not easy to be destroyed, long shelf-life.
And Maca reactive composition be macamide (macamides) and Lepidinm meyenii Walp alkene (macaenes), both materials are to flat
Weighing apparatus human body hormone secretion has remarkable effect, and the natural hormone electromotor so Lepidinm meyenii Walp is otherwise known as is eaten used people and had body
Power is abundant, spirit vigorous will not be tired sensation, there is the effect improving immunity, strengthen prostatic function.Due to by planting
Plant area, kind source, manage, the impact of the key element such as gather, the difference of Maca reactive composition is obvious.Usually, height above sea level 3000 meters
The active ingredient of above high mountain plantation Lepidinm meyenii Walp is significantly higher than Plain plantation.Color deeper higher than paler colour.Even if
Being same producer, take the material of areal, the difference of batch, its Maca reactive composition just has and reaches several times.Therefore, if
With the content of Maca reactive composition as standard, above-mentioned sheeted product is only capable of as raw material, and Maca reactive composition is low and changes
Amplitude is big, and the ratio accounting for dry product is 0.01～0.2%.Need 20 (0.25g) for each person every day, if edible same amount of agate
Coffee dry product, the content of the Maca reactive composition that some people ingests can exceed that the content that can bear, and some people is owing to ingesting
Content extremely low and there is no any effect.
Up to now, China does not also have to mark the product of Lepidinm meyenii Walp composition.
Summary of the invention
The technical problem to be solved is the Lepidinm meyenii Walp fine powder that can determine Lepidinm meyenii Walp content, i.e. provides to have and determines
Macamide and the Lepidinm meyenii Walp fine powder of Lepidinm meyenii Walp alkene content, it is possible to ensure that its content is identical, effect consistent, and prevent from quickly volatilizing, from
And can reach substantially efficiently to utilize the advantage of Lepidinm meyenii Walp.
The present invention solves the technical scheme that above-mentioned technical problem used: the preparation method of a kind of Lepidinm meyenii Walp fine powder, passes through
Following each step:
A, pulverizing: by moisture content be 5～9% Lepidinm meyenii Walp dry product be placed in multifunctional crusher and pulverize, make the granularity of pueraria root powder
It is 100～300 mesh；
B, extraction: the pueraria root powder of step a is put in multi-function extractor, then in extraction pot add concentration be 65～
The edible ethanol of 95v/v%, sealed extraction pot, with temperature 40～60 DEG C of reflux, extract, 30～120 minutes；
C, centrifugal: to be centrifuged separating by centrifuge by step b gained Lepidinm meyenii Walp extracting solution, take filtrate, filtering residue is repeated extraction
Once, twice gained filtrate is merged；
D., evaporation: merging gained filtrate is placed in cryoconcentration machine, enters for 0.003Mpa with temperature 25～30 DEG C, vacuum
Row low-temperature reduced-pressure evaporates, and recycling design obtains extractum, and the relative density of gained extractum is 1.10～1.15 (55 DEG C)；
E, spray drying: be spray-dried by spray dryer by the extractum of step d, i.e. obtained Lepidinm meyenii Walp fine powder, make Lepidinm meyenii Walp
Fine powder uniform drying, water content are below 3%.
The Lepidinm meyenii Walp dry product of described step a is to be cleaned by the tuber of fresh Lepidinm meyenii Walp, and natural air drying is cut into thickness after 2 days be 0.2
～the lamellar of 0.5 centimetre, then be placed at 50 DEG C be dried to moisture content be 5～9%.
Pueraria root powder and the edible ethanol of described step b are calculated as 1:(8～15 by solid-to-liquid ratio kg:L) mix.
The spray drying of described step e be control hot air drying temperature be 100～120 DEG C, outlet temperature be 75～80 DEG C.
Within products obtained therefrom, aluminium foil bag, outer fiber can are packed.
Compared with prior art, it is an advantage of the current invention that after dry Lepidinm meyenii Walp raw material pulverizing, by innoxious solvent ethanol
Extract, obtain the Lepidinm meyenii Walp product of high-load, rich in macamide and Lepidinm meyenii Walp alkene, it is possible to ensure that its content is identical, effect consistent, and
Prevent from quickly volatilizing such that it is able to reach substantially efficiently to utilize the advantage of Lepidinm meyenii Walp.The activity substance content of gained Lepidinm meyenii Walp fine powder
Height, saves the time again, conservation and the energy.Under the conditions of said extracted, it is thus achieved that Lepidinm meyenii Walp fine powder can reach following quality
Index: fine maca opaque figureofmerit table Lepidinm meyenii Walp alkene >=1.0%, macamide >=2.0%.
For at utmost ensureing macamide and the yield of Lepidinm meyenii Walp alkene in Lepidinm meyenii Walp, the present invention uses following scheme: (1)
Cold drying: macamide and Lepidinm meyenii Walp alkene are heat-sensitive materials, easily thermal decomposition of being heated for a long time.To Lepidinm meyenii Walp fresh goods in the present invention
After section, low temperature (≤50 DEG C) vacuum drying obtains the Lepidinm meyenii Walp dry product that water content is 3～5%, to avoid agate during normal temperature drying
Macamide and the loss of Lepidinm meyenii Walp alkene in coffee raw material.(2) green, Continuous Countercurrent Extraction: traditional extraction uses extraction pot to extract
To extracting solution, intermittently operated, the poor stability of product quality between time-consuming, laborious, batch.The present invention uses Continuous Countercurrent Extraction to fill
Putting and extract, Extraction solvent is harmless edible ethanol, and pueraria root powder is 1:8～1:15 with the weight ratio of solvent, Extracting temperature
Being maintained at 40～60 DEG C, extraction time is 30～120 minutes.The present invention by Continuous Countercurrent Extraction can improve macamide and
The dissolution rate of Lepidinm meyenii Walp alkene, shortens extraction time, reduces solvent load, and serialization, automatization extract and reduce labor intensity, raising batch
The stability of secondary product quality.(3) cryogenic vacuum evaporation: conventional triple effect concentrates, thin film evaporation, and evaporating temperature is above 50 DEG C,
Evaporation time is long, and the easy heat of heat-sensitive materials is decomposed.The present invention uses cryogenic vacuum vaporising device, and controlling evaporating temperature is 25～30
DEG C, the vacuum of vaporization chamber is 0.003 MPa, is evaporated by cryogenic vacuum, it is ensured that heat-sensitive ingredients macamide and Lepidinm meyenii Walp
Alkene, in evaporation process, farthest retains.(4) it is spray-dried: be spray-dried and have that heat time heating time is short, continuous and automatic behaviour
The advantages such as work, gained xeraphium are fine and smooth, uniform, soluble.Therefore, the present invention obtains Lepidinm meyenii Walp fine powder by being spray-dried.In a word,
The present invention is by above several critical processes, to retain active component macamide and Lepidinm meyenii Walp alkene in Lepidinm meyenii Walp, integrated modern first
Enter to extract, evaporate, the technique such as be dried, to ensure macamide and the content of Lepidinm meyenii Walp alkene in Lepidinm meyenii Walp fine powder.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
A, pulverizing: cleaned by the tuber of fresh Lepidinm meyenii Walp, natural air drying is cut into the lamellar that thickness is 0.3 centimetre, then is placed in 50 after 2 days
Being dried at DEG C to the Lepidinm meyenii Walp dry product that moisture content is 6%, then be placed in multifunctional crusher and pulverize, the granularity making pueraria root powder is
200 mesh；
B, extraction: put in multi-function extractor by the pueraria root powder of step a, be then calculated as 1:10 to extraction by solid-to-liquid ratio kg:L
Adding concentration in tank is the edible ethanol of 95v/v%, seals extraction pot, with 55 DEG C of reflux, extract, of temperature 90 minutes；
C, centrifugal: to be centrifuged separating by centrifuge by step b gained Lepidinm meyenii Walp extracting solution, take filtrate, filtering residue is repeated extraction
Once, twice gained filtrate is merged；
D., evaporation: merging gained filtrate is placed in cryoconcentration machine, carries out low with temperature 28 DEG C, vacuum for 0.003Mpa
Temperature is evaporated under reduced pressure, and recycling design obtains extractum, and the relative density of gained extractum is 1.10～1.15 (55 DEG C)；
E, spray drying: be spray-dried by spray dryer by the extractum of step d, controlling hot air drying temperature is 110
DEG C, outlet temperature be 78 DEG C, i.e. obtain Lepidinm meyenii Walp fine powder, make fine maca powder uniform drying, water content below 3%.
Embodiment 2
A, pulverizing: cleaned by the tuber of fresh Lepidinm meyenii Walp, natural air drying is cut into the lamellar that thickness is 0.2 centimetre, then is placed in 50 after 2 days
Being dried at DEG C to the Lepidinm meyenii Walp dry product that moisture content is 5%, then be placed in multifunctional crusher and pulverize, the granularity making pueraria root powder is
100 mesh；
B, extraction: put in multi-function extractor by the pueraria root powder of step a, be then calculated as 1:8 to extraction by solid-to-liquid ratio kg:L
Adding concentration in tank is the edible ethanol of 65v/v%, seals extraction pot, with 40 DEG C of reflux, extract, of temperature 120 minutes；
C, centrifugal: to be centrifuged separating by centrifuge by step b gained Lepidinm meyenii Walp extracting solution, take filtrate, filtering residue is repeated extraction
Once, twice gained filtrate is merged；
D., evaporation: merging gained filtrate is placed in cryoconcentration machine, carries out low with temperature 25 DEG C, vacuum for 0.003Mpa
Temperature is evaporated under reduced pressure, and recycling design obtains extractum, and the relative density of gained extractum is 1.10～1.15 (55 DEG C)；
E, spray drying: be spray-dried by spray dryer by the extractum of step d, controlling hot air drying temperature is 100
DEG C, outlet temperature be 75 DEG C, i.e. obtain Lepidinm meyenii Walp fine powder, make fine maca powder uniform drying, water content below 3%.
Embodiment 3
A, pulverizing: cleaned by the tuber of fresh Lepidinm meyenii Walp, natural air drying is cut into the lamellar that thickness is 0.5 centimetre, then is placed in 50 after 2 days
Being dried at DEG C to the Lepidinm meyenii Walp dry product that moisture content is 9%, then be placed in multifunctional crusher and pulverize, the granularity making pueraria root powder is
300 mesh；
B, extraction: put in multi-function extractor by the pueraria root powder of step a, be then calculated as 1:15 to extraction by solid-to-liquid ratio kg:L
Adding concentration in tank is the edible ethanol of 85v/v%, seals extraction pot, with temperature 60 C reflux, extract, 30 minutes；
C, centrifugal: to be centrifuged separating by centrifuge by step b gained Lepidinm meyenii Walp extracting solution, take filtrate, filtering residue is repeated extraction
Once, twice gained filtrate is merged；
D., evaporation: merging gained filtrate is placed in cryoconcentration machine, carries out low with temperature 30 DEG C, vacuum for 0.003Mpa
Temperature is evaporated under reduced pressure, and recycling design obtains extractum, and the relative density of gained extractum is 1.10～1.15 (55 DEG C)；
E, spray drying: be spray-dried by spray dryer by the extractum of step d, controlling hot air drying temperature is 120
DEG C, outlet temperature be 80 DEG C, i.e. obtain Lepidinm meyenii Walp fine powder, make fine maca powder uniform drying, water content below 3%.
Respectively with variable concentrations edible ethanol as Extraction solvent, 50 DEG C are extracted 2 hours, survey active substance in gained Lepidinm meyenii Walp fine powder and contain
Amount.When concentration of alcohol is 65% ethanol to 95% ethanol, along with the rising of concentration of alcohol, the activity substance content of gained Lepidinm meyenii Walp fine powder
It is stepped up；The activity substance content that 95% ethanol extraction three times obtains Lepidinm meyenii Walp fine powder is the highest, reaches 2.96%；65% ethanol extraction
Time, the activity substance content of Lepidinm meyenii Walp fine powder is minimum, and only 1.02%, it is shown in Table 1.
Table 1 different concentration ethanol is on the impact of activity substance content in Lepidinm meyenii Walp fine powder
Extract with different time respectively, survey activity substance content in gained Lepidinm meyenii Walp fine powder.Along with the prolongation of extraction time, fine maca
In powder, the content of active substance steps up, upon extracting between when being 1.5h, in Lepidinm meyenii Walp fine powder, activity substance content is up to
2.82%；Extraction time is 2h, and activity substance content is slightly increased, and reaches 2.87%.Illustrate, proper extension extraction time, help
In Lepidinm meyenii Walp, the effectively dissolving of active component, extraction are shown in Table 2.
Table 2 different extraction time is on the impact of activity substance content in Lepidinm meyenii Walp fine powder
The different Extracting temperature of table 3 is on the impact of activity substance content in Lepidinm meyenii Walp fine powder
Extract with different temperatures respectively, survey activity substance content in gained Lepidinm meyenii Walp fine powder.As known from Table 3, temperature 30 DEG C, 40
DEG C, 50 DEG C, 60 DEG C time, along with the rising of Extracting temperature, in gained Lepidinm meyenii Walp fine powder, the content of active substance is also stepped up, when carrying
Taking temperature when reaching 50 DEG C, the content of active substance reaches maximum, then raises along with the continuation of temperature, the content of active substance
It is declined slightly.Along with the rising of temperature, the dissolving of the extraction efficiency raising of Extraction solvent, beneficially active substance and extraction.But
Temperature is too high, in Lepidinm meyenii Walp, active structure is unstable, it may occur however that decompose.Therefore, when extracting Maca reactive material, temperature is with 50
DEG C it is advisable.
Claims (4)
1. the preparation method of a Lepidinm meyenii Walp fine powder, it is characterised in that through following each step:
A, pulverizing: by moisture content be 5～9% Lepidinm meyenii Walp dry product pulverize, the granularity making pueraria root powder is 100～300 mesh；
B, extraction: the pueraria root powder of step a is added the edible ethanol that concentration is 65～95v/v%, carries with temperature 40～60 DEG C of backflows
Take 30～120 minutes；
C, centrifugal: to be centrifuged step b gained Lepidinm meyenii Walp extracting solution separating, take filtrate, repeat to extract once by filtering residue, merge two
Secondary gained filtrate；
D., evaporation: gained filtrate will be merged, carry out low-temperature reduced-pressure evaporation with temperature 25～30 DEG C, vacuum for 0.003Mpa, and return
Receiving solvent, obtain extractum, the relative density of gained extractum is 1.10～1.15；
E, spray drying: be spray-dried by the extractum of step d, i.e. obtain Lepidinm meyenii Walp fine powder.
The preparation method of Lepidinm meyenii Walp fine powder the most according to claim 1, it is characterised in that: the Lepidinm meyenii Walp dry product of described step a is
Being cleaned by the tuber of fresh Lepidinm meyenii Walp, natural air drying is cut into the lamellar that thickness is 0.2～0.5 centimetre after 2 days, then is placed at 50 DEG C dry
Dry to moisture content be 5～9%.
The preparation method of Lepidinm meyenii Walp fine powder the most according to claim 1, it is characterised in that: the pueraria root powder of described step b and food
It is calculated as 1:(8～15 by solid-to-liquid ratio kg:L with ethanol) mix.
The preparation method of Lepidinm meyenii Walp fine powder the most according to claim 1, it is characterised in that: the spray drying of described step e is
Control hot air drying temperature be 100～120 DEG C, outlet temperature be 75～80 DEG C.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20070073663A (en) * | 2007-04-26 | 2007-07-10 | (주)에이지아이 | Preparation method for the extract from maca and the composition containing the same |
| CN105687284A (en) * | 2016-01-21 | 2016-06-22 | 长春中医药大学 | Extraction analysis and application method of mair-cona active constituents |
-
2016
- 2016-08-11 CN CN201610655384.XA patent/CN106176610A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20070073663A (en) * | 2007-04-26 | 2007-07-10 | (주)에이지아이 | Preparation method for the extract from maca and the composition containing the same |
| CN105687284A (en) * | 2016-01-21 | 2016-06-22 | 长春中医药大学 | Extraction analysis and application method of mair-cona active constituents |
Non-Patent Citations (2)
| Title |
|---|
| 唐燕文等: "玛咖有效成分多种提取方法的比较研究", 《食品工业科技》 * |
| 张雯雯等: "正交试验优化喷雾干燥法制备玛咖精粉工艺", 《食品科学》 * |
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Application publication date: 20161207 |
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| RJ01 | Rejection of invention patent application after publication |