CN104593155A - Method for extracting maca essential oil - Google Patents
Method for extracting maca essential oil Download PDFInfo
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- CN104593155A CN104593155A CN201510017850.7A CN201510017850A CN104593155A CN 104593155 A CN104593155 A CN 104593155A CN 201510017850 A CN201510017850 A CN 201510017850A CN 104593155 A CN104593155 A CN 104593155A
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- CN
- China
- Prior art keywords
- maca
- filtrate
- essential oil
- extraction
- glucosinolate
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
Abstract
The invention discloses a method for extracting maca essential oil. The method comprises the following steps: cleaning maca roots and stems, air-drying to remove water on surfaces, then cutting root barks of spherical maca roots and/or fine roots besides the spherical maca roots, and cutting into pieces for later use; then mixing the pieces with an ethanol aqueous solution; performing sealed soaking at normal temperature; then performing low-temperature filtration to obtain a filtrate; adjusting the pH of the filtrate to be neutral; adding pure water into the filtrate; then cooling to ensure that the filtrate is completely frozen into a solid state, and crushing to obtain solid particles; performing supercritical CO2 extraction on the solid particles, and collecting the maca essential oil. According to the method disclosed by the invention, the yield of the maca essential oil reaches more than or equal to 0.25%, the content of glucosinolate accounts for more than or equal to 20.2% of the essential oil, and the mustard pungent taste in the essential oil can be kept for 36-72 hours at normal temperature. The essential oil can avoid decomposition and disassimilation of aromatic glucosinolate, so that the essential oil is good in quality, is rich in aroma and pure in mustard pungent taste, and does not have odors and other peculiar smells after decomposition of glucosinolate.
Description
Technical field
The invention belongs to natural product chemistry and field of plant extraction, relate to a kind of method extracting fine maca oil specifically.
Background technology
Agate coffee (Maca) for Cruciferae separate row Vegetable spp herbaceous plant (
lepidium meyeniiwalp.), originating in South America, is a kind of functional foodstuff having pharmaceutical use and economic implications.The research of its effect basic substance shows, agate coffee is rich in the secondary metabolite such as the nutritive substances such as mineral element, amino acid, VITAMIN and alkaloid, sterol, glucosinolate, has improvement function, anti-ageing, antitumor, anti-oxidant isoreactivity.
Wherein, glucosinolate is a kind of hydrophilic plant secondary metabolites of nitrogenous and sulphur, and be one of effect component main in agate coffee block root, being mainly distributed in agate coffee leaf and agate coffee root, is fine maca main body of oil.In fresh of agate coffee and leaf thereof, find that the glucosinolate that content is the highest is aromatic series glucosinolate; mainly comprise: p-hydroxybenzyl mustard oil glycosides, pentane-4-thiazolinyl glucosinolate, indoles-3-methyl-mustard oil glycosides, 5-methyl sulfinyl pentyl glucosinolate, 4-methoxy-Indole-3-methyl-mustard oil glycosides and to methoxy-benzyl glucosinolate etc. six kinds, experiment is compared and is found the content of the glucosinolate content in agate coffee leaf and agate coffee root skin far above agate coffee spherical-shaped piece root.Current research shows that glucosinolate has effect of antagonism kinds cancer, and benzyl mustard oil glycosides and the tumour of meta-methoxy benzyl mustard oil glycosides to a lot of tumour especially gastro-intestinal system have good prophylactic effect.In addition many investigators think that agate coffee improves fertility, sexual function improving is all relevant with glucosinolate and degradation production thereof.
But when agate coffee plant tissue is subject to damaging, glucosinolate can be hydrolyzed by endogenous myrosin, produce the compounds such as cyanogen class, zolidine thione, thiocyanic ester and lsothiocyanates.Cyanogen class material generally all has certain toxicity, and should avoid its generation in the uncertain situation of its function.Simultaneously, in the process that glucosinolate is hydrolyzed by myrosin, the smell of agate coffee itself can change with the exclusive fragrant and sweet smell of agate coffee the pungent odor being similar to rotten egg by the peppery pungent taste of mustard into, all completes until transform and changes the only surplus exclusive fragrant and sweet smell of agate coffee into.It is agate coffee ovendry power or lyophilized powder that current agate coffee extracts conventional extraction raw material, and minority is fresh of agate coffee.And in processing, be no matter the wherein contained Fe of cutter, slicing machine or pulverizer
2+all can generate complex compound with the glucosinolate generation chemical reaction in agate coffee, affect it and absorb, agate coffee extracting solution can be made simultaneously with dense metal ion taste, affect the mouthfeel of the finished product.
Agate coffee is introduced a fine variety in China, and implantation time is shorter, the agate coffee healthcare products therefore sold in the market, is raw material greatly mainly with agate coffee root dry powder.Because active constituent content is low, taking dose is large, and health-care effect is not obvious.And absorb easily at present, convenient and swift, the coffee essential oil being rich in active substance not yet has the correlative study of extracting method.
Summary of the invention
In order to overcome, agate coffee healthcare products active constituent content is low, health-care effect is not obvious, the not easily problem such as absorption, the invention provides a kind of method extracting fine maca oil, to avoid decomposition and the alienation of aromatic series glucosinolate in fine maca oil.
The present invention is realized by following technical proposal: a kind of method extracting fine maca oil, through following each step:
(1) MAJIA Rhizome is cleaned, dry the radicula beyond the root skin of lower spherical of the agate coffee of cutting after surface-moisture and/or spherical, shred for subsequent use afterwards;
(2) by solid-liquid ratio kg/L 1:(2 ~ 10), by step (1) shred after root skin and/or radicula with pH=2 ~ 5 and the aqueous ethanolic solution that concentration is 30 ~ 80v/v% mix, seal immersion 3 ~ 12 hours at normal temperatures again, then at 0 ~ 10 DEG C, carry out filtration obtain filtrate, regulate filtrate pH to neutral, then in filtrate, add pure water make its alcohol concn be 10 ~ 15v/v%;
(3) filtrate after step (2) being processed is cooled to less than-20 DEG C, pulverizes, obtain solid particulate after making it form solid completely;
(4) step (3) gained solid particulate is carried out supercritical CO
2extraction 30 ~ 90min, collects and obtains fine maca oil.
The cutting of described step (1) uses sintex.Avoid the activeconstituents in agate coffee and the Fe in metal knife
2+there is chemical reaction and generate complex compound.
Filtrate pH is regulated to use the hydrochloric acid soln of 2wt% or the NaOH solution of 1wt% to regulate in described step (1).
In described step (3), rate of temperature fall is 6 ~ 10 DEG C/min.
The supercritical CO of described step (4)
2extraction conditions is extraction temperature is 15 ~ 25 DEG C, extracting pressure is 10 ~ 17MPa, CO
2flow is 5 ~ 15mL/min, starts dynamic extraction after arriving set(ting)value.
Compared with prior art, the invention has the beneficial effects as follows: the present invention uses root beyond spherical of fresh agate coffee or agate coffee root skin, avoid the loss of aromatic series glucosinolate in heating, drying process on the one hand, ensure aromatic series glucosinolate content in the feed on the other hand.Use pH value be 2 ethanolic soln can accelerate the hydrolysis of agate coffee cell walls, make the endogenous myrosin inactivation in agate coffee simultaneously, the filtration velocity of agate coffee extracting solution can also be improved.The present invention has started the extracting method of fine maca oil, and present invention process flow process is simple, and with short production cycle, extraction yield is high, the coffee essential oil quality better of production.Fine maca of the present invention oil yield reaches >=2.5 ‰, glucosinolate content account for essential oil >=20.2%, under normal temperature, in essential oil, the peppery pungent taste of mustard can keep 36 ~ 72 hours.Essential oil can avoid decomposition and the alienation of aromatic series glucosinolate, essential oil quality better, and its essential oil shows as and gives off a strong fragrance, and has the peppery pungent taste of pure mustard, stink and other peculiar smell after decomposing without glucosinolate.
Embodiment
Further illustrate the present invention below in conjunction with embodiment, but the present invention is not limited to these embodiments.
Embodiment 1
(1) fresh MAJIA Rhizome is cleaned, after drying surface-moisture, cut the radicula beyond lower spherical of agate coffee, for subsequent use after using sintex to be shredded;
(2) by solid-liquid ratio kg/L 1:3, by step (1) shred after radicula with pH=2 and the aqueous ethanolic solution that concentration is 70v/v% mix, seal immersion 6 hours at normal temperatures again, then at 10 DEG C, carry out filtration obtain filtrate, use the NaOH solution of the hydrochloric acid soln of 2wt% or 1wt% to regulate filtrate pH to neutral, then in filtrate, add pure water make its alcohol concn be 15v/v%;
(3) filtrate after step (2) being processed is that 8 DEG C/min is cooled to less than-20 DEG C by rate of temperature fall, pulverizes, obtain solid particulate after making it form solid completely;
(4) step (3) gained solid particulate is placed in extraction kettle and carries out supercritical CO by following condition
2extraction 40min: extraction temperature is 15 DEG C, extracting pressure is 10MPa, CO
2flow is 10mL/min, starts dynamic extraction after arriving set(ting)value, collects and obtains fine maca oil.
Fine maca oil is faint yellow, and have the fragrant and sweet and peppery pungent taste of mustard of agate coffee, essential oil yield 2.5 ‰, glucosinolate content is 20.7% of essential oil, and under normal temperature, in essential oil, the peppery pungent taste of mustard can keep 72 hours simultaneously.
Embodiment 2
(1) fresh MAJIA Rhizome is cleaned, after drying surface-moisture, cut the root skin of lower spherical of agate coffee, for subsequent use after using sintex to be shredded;
(2) by solid-liquid ratio kg/L 1:10, by step (1) shred after root skin with pH=4 and the aqueous ethanolic solution that concentration is 30v/v% mix, seal immersion 12 hours at normal temperatures again, then at 0 DEG C, carry out filtration obtain filtrate, use the NaOH solution of the hydrochloric acid soln of 2wt% or 1wt% to regulate filtrate pH to neutral, then in filtrate, add pure water make its alcohol concn be 12v/v%;
(3) filtrate after step (2) being processed is that 10 DEG C/min is cooled to less than-20 DEG C by rate of temperature fall, pulverizes, obtain solid particulate after making it form solid completely;
(4) step (3) gained solid particulate is placed in extraction kettle and carries out supercritical CO by following condition
2extraction 90min: extraction temperature is 20 DEG C, extracting pressure is 15MPa, CO
2flow is 15mL/min, starts dynamic extraction after arriving set(ting)value, collects and obtains fine maca oil.
Fine maca oil is faint yellow, and have the fragrant and sweet and peppery pungent taste of mustard of agate coffee, essential oil yield 2.7 ‰, glucosinolate content is 23.9% of essential oil, and under normal temperature, in essential oil, the peppery pungent taste of mustard can keep 60 hours simultaneously.
Embodiment 3
(1) fresh MAJIA Rhizome is cleaned, dry the radicula beyond the root skin of lower spherical of the agate coffee of cutting after surface-moisture and spherical, use sintex shred rear for subsequent use;
(2) by solid-liquid ratio kg/L 1:2, by step (1) shred after root skin and radicula with pH=5 and the aqueous ethanolic solution that concentration is 80v/v% mix, seal immersion 3 hours at normal temperatures again, then at 5 DEG C, carry out filtration obtain filtrate, use the NaOH solution of the hydrochloric acid soln of 2wt% or 1wt% to regulate filtrate pH to neutral, then in filtrate, add pure water make its alcohol concn be 10v/v%;
(3) filtrate after step (2) being processed is that 6 DEG C/min is cooled to less than-20 DEG C by rate of temperature fall, pulverizes, obtain solid particulate after making it form solid completely;
(4) step (3) gained solid particulate is placed in extraction kettle and carries out supercritical CO by following condition
2extraction 30min: extraction temperature is 25 DEG C, extracting pressure is 17MPa, CO
2flow is 5mL/min, starts dynamic extraction after arriving set(ting)value, collects and obtains fine maca oil.
Fine maca oil is faint yellow, and have the fragrant and sweet and peppery pungent taste of mustard of agate coffee, essential oil yield 2.8 ‰, glucosinolate content is 20.2% of essential oil, and under normal temperature, in essential oil, the peppery pungent taste of mustard can keep 48 hours simultaneously.
Comparative example 1: identical with embodiment 1, only replacing raw material is fresh MAJIA Rhizome.
Comparative example 2: identical with embodiment 1, only replaces supercritical CO
2extraction is conventional negative pressure-cavitation homogenous solid-liquid phase liquid-solid extraction.
Claims (5)
1. extract a method for fine maca oil, it is characterized in that through following each step:
(1) MAJIA Rhizome is cleaned, dry the radicula beyond the root skin of lower spherical of the agate coffee of cutting after surface-moisture and/or spherical, shred for subsequent use afterwards;
(2) by solid-liquid ratio kg/L 1:(2 ~ 10), by step (1) shred after root skin and/or radicula with pH=2 ~ 5 and the aqueous ethanolic solution that concentration is 30 ~ 80v/v% mix, seal immersion 3 ~ 12 hours at normal temperatures again, then at 0 ~ 10 DEG C, carry out filtration obtain filtrate, regulate filtrate pH to neutral, then in filtrate, add pure water make its alcohol concn be 10 ~ 15v/v%;
(3) filtrate after step (2) being processed is cooled to less than-20 DEG C, pulverizes, obtain solid particulate after making it form solid completely;
(4) step (3) gained solid particulate is carried out supercritical CO
2extraction 30 ~ 90min, collects and obtains fine maca oil.
2. the method for extraction fine maca oil according to claim 1, is characterized in that: the cutting of described step (1) uses sintex.
3. the method for extraction fine maca oil according to claim 1, is characterized in that: regulate filtrate pH to use the hydrochloric acid soln of 2wt% or the NaOH solution of 1wt% to regulate in described step (1).
4. the method for extraction fine maca oil according to claim 1, is characterized in that: in described step (3), rate of temperature fall is 6 ~ 10 DEG C/min.
5. the method for extraction fine maca oil according to claim 1, is characterized in that: the supercritical CO of described step (4)
2extraction conditions is extraction temperature is 15 ~ 25 DEG C, extracting pressure is 10 ~ 17MPa, CO
2flow is 5 ~ 15mL/min, starts dynamic extraction after arriving set(ting)value.
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| CN201510017850.7A CN104593155B (en) | 2015-01-14 | 2015-01-14 | A kind of method for extracting maca essential oil |
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| CN201510017850.7A CN104593155B (en) | 2015-01-14 | 2015-01-14 | A kind of method for extracting maca essential oil |
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| CN104593155B CN104593155B (en) | 2017-11-28 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106318629A (en) * | 2015-07-07 | 2017-01-11 | 广东玛海娑生物科技有限责任公司 | Supercritical extraction method of maca essential oil |
| CN107041973A (en) * | 2016-07-11 | 2017-08-15 | 合肥九研医药科技开发有限公司 | A kind of condom for being coated with maca essential oil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1473594A (en) * | 2003-07-01 | 2004-02-11 | 华中科技大学 | Extract of Maka root |
| CN104120037A (en) * | 2014-08-08 | 2014-10-29 | 广西壮族自治区林业科学研究院 | Extracting method for jasmine flower essential oil |
-
2015
- 2015-01-14 CN CN201510017850.7A patent/CN104593155B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1473594A (en) * | 2003-07-01 | 2004-02-11 | 华中科技大学 | Extract of Maka root |
| CN104120037A (en) * | 2014-08-08 | 2014-10-29 | 广西壮族自治区林业科学研究院 | Extracting method for jasmine flower essential oil |
Non-Patent Citations (1)
| Title |
|---|
| 艾中等: "国产玛咖芥子油苷的组分分析和含量测定", 《食品科技》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106318629A (en) * | 2015-07-07 | 2017-01-11 | 广东玛海娑生物科技有限责任公司 | Supercritical extraction method of maca essential oil |
| CN107041973A (en) * | 2016-07-11 | 2017-08-15 | 合肥九研医药科技开发有限公司 | A kind of condom for being coated with maca essential oil |
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| CN104593155B (en) | 2017-11-28 |
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