CN108685969A - A kind of extracting method of maca total alkaloid - Google Patents
A kind of extracting method of maca total alkaloid Download PDFInfo
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- CN108685969A CN108685969A CN201810595202.3A CN201810595202A CN108685969A CN 108685969 A CN108685969 A CN 108685969A CN 201810595202 A CN201810595202 A CN 201810595202A CN 108685969 A CN108685969 A CN 108685969A
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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
- A61K2236/10—Preparation or pretreatment of starting material
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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
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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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
- A61K2236/35—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
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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Abstract
The present invention relates to a kind of methods of extraction maca total alkaloid, and this approach includes the following steps:Broken wall treatment is carried out to maca particle, obtains broken wall product;Broken wall product is ultrasonically treated, is collected by filtration to obtain the first filtrate, the first filter residue is for use;By in step the first filter residue according to maca:Hydrochloric acid ratio is 1:10-1:15 are added hydrochloric acid, then according to maca:Distilled water ratio is 1:20-1:25 proportioning is poured into 80-90 DEG C of distilled water, water-bath 2-3h, is collected by filtration to obtain the second filtrate, the second filter residue is for use;Second filter residue is placed in cryogenic high pressure vessel and is cooled to negative 20-40 DEG C rapidly, and applies the pressure 15-25min of 400-500MPa, then restores to normal pressure in 1 second, and be rapidly heated to 80-90 DEG C, is collected by filtration to obtain third filtrate;First filtrate, the second filtrate and third filtrate are mixed, NaOH is added and adjusts pH to 7.6-8, isometric chloroform extracts 3 times, merging filtrate, and then by chloroform evaporated to doing, absolute ethyl alcohol dissolving is added.The recovery rate of maca total alkaloid of the present invention reaches 2.53%-2.74%.
Description
Invention field
The present invention relates to a kind of extracting methods of maca bioactive ingredients, and in particular to a kind of maca total alkaloid carries
Take method.
Technical background
Maca (Lepidium meyenii Walp) is a kind of and closes the crucifer of medicine-food two-purpose together, I
Lijiang County In Yunnan Province is mainly originated in state, and other countries' such as South America main product mainly has yellow, purple, blue, black in Andes
The colors such as color, its various composition content of different colours is also different, studies have shown that containing compared with multi-nutrient such as amino in maca
Acid, phytoprotein, trace element and fat etc., secondary metabolites principal component have:Alkaloid (macamides
(macamides), agate card dilute (macaenes) and glucosinolate etc..The safety of maca is also very high, and maca also contains very much
Pharmacological action enhances learning and remembering ability and can protect nerve;Make immunity of organisms enhancing and antifatigue efficiency;Change
Good reproductive development power and sexual function;Endocrine function and antidepression effect even can also be adjusted;Anti-aging, antioxidation;It is right
Resist certain cancers and prevent some hyperblastosises effect etc..This so that maca is rapid hot on the market, mainly as
Health products it is most widely used.Maca alkaloid is a kind of nitrogenous organic matter, possesses anti-oxidant, and cell viability is made to increase effect
Up to the present fruit and anti-fatigue active, maca total alkaloid mainly take ethyl alcohol, methanol to also have water etc. to be used as Extraction solvent.
Periodical literature " response surface optimization maca alkaloid extracting technique ", Zheng Yongqing etc., the 33-38 pages, food with fermentation
Science and technology, 2017, it was recently reported that using ethyl alcohol as Extraction solvent carry out maca alkaloid extraction method, and have studied extraction time,
Influence of the factors such as solid-liquid ratio to maca alkaloid recovery rate, however using ethyl alcohol as the extracting method of solvent in optimized parameter carry
Rate is taken to be also only 0.252%.Periodical literature " Yunnan plants maca total alkaloid extracting technique optimizing research ", Jiang Yuemeng etc., the
232-234 pages, food industry science and technology, 2013, it was recently reported that the technique that extract total alkaloids in maca are planted from Yunnan, and to extraction
The parameters such as solvent, extraction time, Extracting temperature, solid-liquid ratio have carried out unitary variant impact analysis, finally obtain solid-liquid ratio 1:20,
Under the conditions of 70 DEG C of Extracting temperature, extraction time 100min, the recovery rate of maca total alkaloid is 1.58%.
By the above-mentioned prior art it is found that cannot still meet current need for the recovery rate of maca total alkaloid at present
It asks.
Invention content
In order to overcome the above-mentioned deficiencies of the prior art, present invention aims at provide a kind of extraction side of maca total alkaloid
Method, this method can improve the recovery rate of maca alkaloid.
Technical proposal that the invention solves the above-mentioned problems is as follows:
A kind of extracting method of maca total alkaloid, this approach includes the following steps:
Step 1, broken wall treatment is carried out to maca particle, obtains broken wall product;
Step 2, above-mentioned broken wall product is ultrasonically treated, is collected by filtration to obtain the first filtrate, the first filter residue is for use;
Step 3, into above-mentioned first filter residue according to maca:Hydrochloric acid ratio is 1:10-1:15 are added concentrated hydrochloric acid, then according to agate
Coffee:Distilled water ratio is 1:20-1:25 proportioning is poured into 80-90 DEG C of distilled water, water-bath 2h or more, is collected by filtration to obtain the second filter
Liquid, the second filter residue are for use;
Step 4, the second filter residue is placed in cryogenic high pressure vessel and is cooled to -20 DEG C rapidly hereinafter, and applying 400-
The pressure 15-25min of 500MPa, it is then rapid to restore to normal pressure, and be rapidly heated to 80-90 DEG C, it is collected by filtration to obtain third
Filtrate;
Step 5, NaOH is added after the first filtrate, the second filtrate and third filtrate being mixed and adjusts pH to 7.6-8, in equal volume
Chloroform extracts 3 times, merging filtrate, then by chloroform evaporated to dry, addition 20mL absolute ethyl alcohols dissolving.
Further, the grain size of the maca particle is 0.1-0.5mm;
Further, the content of the maca particle is 10-15g;
Further, the broken wall treatment refers to that the particle is placed in the container of sealing, and high to being inputted in container
Gauge pressure is 0.3~0.5MPa and maintains 60~90 seconds in pressure air to container, and the gauge pressure in container is reduced to 0Pa in 1 second;
Using ethyl alcohol eluant container, it is the broken wall product to collect washings;
Further, described be ultrasonically treated refers to mixing the broken wall product with ethyl alcohol, is adopted after being heated to 30~40 DEG C
With 30~50min of ultrasonic activation of 80-100KHz, supersound process in triplicate is carried out to filter residue after filtering;
Further, restore the time control to normal pressure in the step 3 in 1 second.
The present invention uses broken wall and supersound process first, and having carried out initial physical breaking apart to cell wall makes a part of total biology
Alkali is released, and then makes alkaloid forming salt by chemical method, and is dissolved in therewith in solvent distilled water, due to solvent
Temperature is higher, promotes the solvent that Particles Moving accelerates alkaloid forming salt, and the alkaloid thus further increased is received
Rate.Second filter residue is carried out cold pressing to be crushed, since maca intraor extracellular osmotic pressure increases in the filter residue after chemical treatment, extremely cold
Under being acted on high pressure, the percentage of damage of cell wall greatly increases, and a large amount of total alkaloid is made to be released, and then greatly improves total
The recovery rate of alkaloid.
Compared with the existing technology, the present invention is by using physical-chemical-physical union processing mode, in conjunction with various processing
The characteristics of mode, makes the recovery rate of total alkaloid reach maximization, and by using the extracting method of the present invention, final maca is always given birth to
The recovery rate of alkaloids reaches 2.53%-2.74%, has ideal recovery rate, and the flow used is simple, extraction effect
Rate is high.
Specific implementation mode
Embodiment 1
A kind of extracting method of maca total alkaloid, specific extraction step are as follows:
Step 1, the maca grains that 10g grain sizes are 0.1mm are placed in the container of sealing, and high to being inputted in container
Gauge pressure is 0.5MPa and maintains 60 seconds in pressure air to container, and the gauge pressure in container is reduced to 0Pa in 1 second;Using ethyl alcohol
Eluant container, it is the broken wall product to collect washings;
Step 2, above-mentioned broken wall product is ultrasonically treated, is collected by filtration to obtain the first filtrate, the first filter residue is for use;
Step 3, into above-mentioned first filter residue according to maca:Hydrochloric acid ratio is 1:10 are added concentrated hydrochloric acid, then according to maca:It steams
Distilled water ratio is 1:20 proportioning is poured into 80 DEG C of distilled water, water-bath 2h, is collected by filtration to obtain the second filtrate, the second filter residue is for use;
Step 4, the second filter residue is placed in cryogenic high pressure vessel and is cooled to -20 DEG C rapidly, and apply the pressure of 400MPa,
15min is maintained, it is then rapid to restore to normal pressure, and be rapidly heated to 80 DEG C, it is collected by filtration to obtain third filtrate;
Step 5, NaOH is added after the first filtrate, the second filtrate and third filtrate being mixed and adjusts pH to 7.6, isometric chlorine
Imitative extraction 3 times, merging filtrate, then by chloroform evaporated to dry, addition 20mL absolute ethyl alcohols dissolving.
Embodiment 2
A kind of extracting method of maca total alkaloid, specific extraction step are as follows:
Step 1, the maca grains that 12g grain sizes are 0.3mm are placed in the container of sealing, and high to being inputted in container
Gauge pressure is 0.3MPa and maintains 75 seconds in pressure air to container, and the gauge pressure in container is reduced to 0Pa in 1 second;Using ethyl alcohol
Eluant container, it is the broken wall product to collect washings;
Step 2, above-mentioned broken wall product is ultrasonically treated, is collected by filtration to obtain the first filtrate, the first filter residue is for use;
Step 3, into above-mentioned first filter residue according to maca:Hydrochloric acid ratio is 1:13 are added concentrated hydrochloric acid, then according to maca:It steams
Distilled water ratio is 1:25 proportioning is poured into 80 DEG C of distilled water, water-bath 3h, is collected by filtration to obtain the second filtrate, the second filter residue is for use;
Step 4, the second filter residue is placed in cryogenic high pressure vessel and is cooled to -30 DEG C rapidly, and apply the pressure of 500MPa,
25min is maintained, it is then rapid to restore to normal pressure, and be rapidly heated to 80 DEG C, it is collected by filtration to obtain third filtrate;
Step 5, NaOH is added after the first filtrate, the second filtrate and third filtrate being mixed and adjusts pH to 7.6, isometric chlorine
Imitative extraction 3 times, merging filtrate, then by chloroform evaporated to dry, addition 20mL absolute ethyl alcohols dissolving.
Embodiment 3
A kind of extracting method of maca total alkaloid, specific extraction step are as follows:
Step 1, the maca grains that 15g grain sizes are 0.5mm are placed in the container of sealing, and high to being inputted in container
Gauge pressure is 0.5MPa and maintains 90 seconds in pressure air to container, and the gauge pressure in container is reduced to 0Pa in 1 second;Using ethyl alcohol
Eluant container, it is the broken wall product to collect washings;
Step 2, above-mentioned broken wall product is ultrasonically treated, is collected by filtration to obtain the first filtrate, the first filter residue is for use;
Step 3, into above-mentioned first filter residue according to maca:Hydrochloric acid ratio is 1:15 are added concentrated hydrochloric acid, then according to maca:It steams
Distilled water ratio is 1:25 proportioning is poured into 90 DEG C of distilled water, water-bath 3h, is collected by filtration to obtain the second filtrate, the second filter residue is for use;
Step 4, the second filter residue is placed in cryogenic high pressure vessel and is cooled to -40 DEG C rapidly, and apply the pressure of 500MPa,
25min is maintained, it is then rapid to restore to normal pressure, and be rapidly heated to 90 DEG C, it is collected by filtration to obtain third filtrate;
Step 5, NaOH is added after the first filtrate, the second filtrate and third filtrate being mixed and adjusts pH to 8, isometric chloroform
Extraction 3 times, merging filtrate, then by chloroform evaporated to dry, addition 20mL absolute ethyl alcohols dissolving.
Comparative example 1
A kind of extracting method of maca total alkaloid, specific extraction step are as follows:
Step 1, the maca grains that 10g grain sizes are 0.1mm are placed in the container of sealing, and high to being inputted in container
Gauge pressure is 0.5MPa and maintains 60 seconds in pressure air to container, and the gauge pressure in container is reduced to 0Pa in 1 second;Using ethyl alcohol
Eluant container, it is the broken wall product to collect washings;
Step 2, above-mentioned broken wall product is ultrasonically treated, is collected by filtration to obtain the first filtrate, the first filter residue is for use;
Step 3, into above-mentioned first filter residue according to maca:Hydrochloric acid ratio is 1:10 are added concentrated hydrochloric acid, then according to maca:It steams
Distilled water ratio is 1:20 proportioning is poured into 80 DEG C of distilled water, water-bath 2h, is collected by filtration to obtain the second filtrate;
Step 4, NaOH is added after the first filtrate, the second filtrate being mixed and adjusts pH to 7.6, isometric chloroform extracts 3 times,
Merging filtrate, then by chloroform evaporated to dry, addition 20mL absolute ethyl alcohols dissolving.
Comparative example 2
A kind of extracting method of maca total alkaloid, specific extraction step are as follows:
Step 1, the maca grains that 10g grain sizes are 0.1mm are placed in the container of sealing, and high to being inputted in container
Gauge pressure is 0.5MPa and maintains 60 seconds in pressure air to container, and the gauge pressure in container is reduced to 0Pa in 1 second;Using ethyl alcohol
Eluant container, it is the broken wall product to collect washings;
Step 2, above-mentioned broken wall product is ultrasonically treated, is collected by filtration to obtain the first filtrate, the first filter residue is for use;
Step 3, the first filter residue is placed in cryogenic high pressure vessel and is cooled to -20 DEG C rapidly, and apply the pressure of 400MPa,
15min is maintained, it is then rapid to restore to normal pressure, and be rapidly heated to 80 DEG C, it is collected by filtration to obtain the second filtrate, the second filter residue waits for
With;
Step 4, into above-mentioned second filter residue according to maca:Hydrochloric acid ratio is 1:10 are added concentrated hydrochloric acid, then according to maca:It steams
Distilled water ratio is 1:20 proportioning is poured into 80 DEG C of distilled water, water-bath 2h, is collected by filtration to obtain third filtrate;
Step 5, NaOH is added after the first filtrate, the second filtrate and third filtrate being mixed and adjusts pH to 7.6, isometric chlorine
Imitative extraction 3 times, merging filtrate, then by chloroform evaporated to dry, addition 20mL absolute ethyl alcohols dissolving.
The assay of total alkaloid
Above-mentioned maca extract is added to the 0.01mol/L dilution heat of sulfuric acid 20ml of configuration, is slightly heated, is fully reacted,
1-2 drop methyl red indicators are added, then with the sodium hydroxide solution titration of the 0.02mol/L of configuration, observe titration end-point
(red becomes faint yellow), record consumption sodium hydroxide volume, the 12.9mg rhizome of Chinese monkshoods are equivalent to per 1mL sulfuric acid solutions 0.01mol/L
Alkali.Maca total alkaloid recovery rate calculation formula:(20ml- sodium hydroxides volume (V)) * 12.9mg/ maca dry powder quality (g) *
100%.
The recovery rate of total alkaloid in embodiment 1-3 is measured using said determination method as follows:
It the results are shown in Table 1.
1 embodiment 1-3 maca total alkaloid recovery rates of table
| Group | Recovery rate (%) |
| Embodiment 1 | 2.53 |
| Embodiment 2 | 2.65 |
| Embodiment 3 | 2.74 |
| Comparative example 1 | 1.56 |
| Comparative example 2 | 1.92 |
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (6)
1. a kind of extracting method of maca total alkaloid, it is as follows that this approach includes the following steps:
Step 1 carries out broken wall treatment to maca particle, obtains broken wall product;
Step 2 is ultrasonically treated above-mentioned broken wall product, is collected by filtration to obtain the first filtrate, the first filter residue is for use;
Step 3, into above-mentioned first filter residue according to maca:Hydrochloric acid ratio is 1:10-1:15 are added concentrated hydrochloric acid, then according to maca:
Distilled water ratio is 1:20-1:25 proportioning is poured into 80-90 DEG C of distilled water, water-bath 2h or more, is collected by filtration to obtain the second filtrate,
Second filter residue is for use;
Second filter residue is placed in cryogenic high pressure vessel and is cooled to -20 DEG C rapidly hereinafter, and applying 400-500MPa's by step 4
Pressure maintains 15-25min, then rapid to restore to normal pressure, and is rapidly heated to 80-90 DEG C, is collected by filtration to obtain third filter
Liquid;
NaOH adjusting pH to 7.6-8, isometric chloroform is added in step 5 after mixing the first filtrate, the second filtrate and third filtrate
Extraction 3 times, merging filtrate, then by chloroform evaporated to dry, addition 20mL absolute ethyl alcohols dissolving.
2. extracting method as described in claim 1, it is characterised in that:The grain size of the maca particle is 0.1-0.5mm.
3. extracting method as described in claim 1, it is characterised in that:The content of the maca particle is 10-15g.
4. extracting method as described in any one of claims 1-3, it is characterised in that:The broken wall treatment refers to by the particle
It is placed in the container of sealing, and be 0.3~0.5MPa and maintain 60~90 to inputting gauge pressure in pressure-air to container in container
Second, the gauge pressure in container is reduced to 0Pa in 1 second;Using ethyl alcohol eluant container, it is the broken wall production to collect washings
Object.
5. extracting method as described in any one of claims 1-3, it is characterised in that:The supersound process refers to by the broken wall
Product is mixed with ethyl alcohol, is heated to using 30~50min of ultrasonic activation of 80-100KHz after 30~40 DEG C, to filter after filtering
Slag carries out supersound process in triplicate.
Restore the time control to normal pressure 6. extracting method as described in any one of claims 1-3, in the step 3 at 1 second
It is interior.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104666384A (en) * | 2015-02-04 | 2015-06-03 | 广东长兴生物科技股份有限公司 | Separating and purifying method for bioactive constituents of maca |
| CN104688796A (en) * | 2015-02-04 | 2015-06-10 | 广东长兴生物科技股份有限公司 | Method for extracting maca bioactive components based on ultrasonic wave |
| CN105732506A (en) * | 2014-12-11 | 2016-07-06 | 黑龙江众生生物工程有限公司 | Preparation method for Lepidium meyenii alkaloid |
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- 2018-06-11 CN CN201810595202.3A patent/CN108685969A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105732506A (en) * | 2014-12-11 | 2016-07-06 | 黑龙江众生生物工程有限公司 | Preparation method for Lepidium meyenii alkaloid |
| CN104666384A (en) * | 2015-02-04 | 2015-06-03 | 广东长兴生物科技股份有限公司 | Separating and purifying method for bioactive constituents of maca |
| CN104688796A (en) * | 2015-02-04 | 2015-06-10 | 广东长兴生物科技股份有限公司 | Method for extracting maca bioactive components based on ultrasonic wave |
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Application publication date: 20181023 |