CN104127468A - Preparation extraction process of Maca extract - Google Patents
Preparation extraction process of Maca extract Download PDFInfo
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- CN104127468A CN104127468A CN201410369470.5A CN201410369470A CN104127468A CN 104127468 A CN104127468 A CN 104127468A CN 201410369470 A CN201410369470 A CN 201410369470A CN 104127468 A CN104127468 A CN 104127468A
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Abstract
The invention relates to a preparation extraction process of a Maca extract. The method comprises the following steps: 1) conducting enzyme protein inactivation on Maca root by using ultrahigh pressure treatment; 2) conducting superfine grinding wall breaking treatment on the inactivated raw material; 3) conducting ultrasonic extraction on the wall-broken ultramicro powder obtained from the previous step with an ethanol surface active agent mixed leaching solution; 4) conducting frame filter and ultrafiltration membrane filtration on the extract collected in the previous step, and collecting filtrate with molecular weight greater than 5000 Da; 5) conducting ultralow temperature freeze drying treatment on the filtrate with molecular weight more than 5000Da collect in the previous step, so as to obtain the Maca extract. The invention adopts the ultrahigh pressure enzyme inactivation, superfine wall breaking and crushing, surfactant ultrasonic synergistic extraction, ultrafiltration condensation and ultralow temperature drying technology, so as to greatly improve the extraction process in the past. The method of the invention can obtain a concentrated powder of the effective components of Maca root.
Description
Technical field
The present invention relates to effective ingredients in plant and prepare extraction process, relate in particular to a kind of preparation extraction process of Lepidinm meyenii Walp extract, belong to plant processing extraction field.
Background technology
Lepidinm meyenii Walp, extensive use on Peru plateau, there is very high nutritive value, and the functional component such as Lepidinm meyenii Walp alkaloid, glucosinolate, Lepidinm meyenii Walp amide and sterol has the fertility of raising, sexual desire promoting, adaptation originality, promotes the physiological functions such as hormone metabolism is synthetic, therefore, Lepidinm meyenii Walp is also described as " Peru's national treasure " or " Peru's Radix Ginseng ", closely during the last ten years, becomes gradually one of focus of global medicine food dual purpose plant exploitation.
Lepidinm meyenii Walp is shorter at the introducing a fine variety of China, implantation time, is mainly distributed in the ground such as Shangri-la, Yunnan Province, Lijing, Huize, has realized scale plantation, and its quality can compare favourably with Peru's Lepidinm meyenii Walp quality.But at present, the Lepidinm meyenii Walp product of selling on market is uneven, greatly mainly with the former powder of Lepidinm meyenii Walp root as product, without crossing senior processed, to sell, this series products active constituent content is low, DeGrain, in the low-end product of field of health care products, in the roughing stage, not symmetrical with the potential value that Lepidinm meyenii Walp itself contains.Therefore, carry out the preparation of Lepidinm meyenii Walp extract, the Lepidinm meyenii Walp extract that functional component is rich in acquisition is the task of top priority of current Lepidinm meyenii Walp health promoting product exploitation, relevant Study on extraction is also progressively being carried out: patent No. CN201410014832 mentions and carries out Lepidinm meyenii Walp extraction by microwave-ultrasonic method, it does not carry out enzyme deactivation, super-micro wall-broken processing to Maca powder, and solvent for use is chloroform constituents, be easy to cause the residual of organic solvent, cause the pollution of extract component, on future products, application has great impact.The employing countercurrent extraction Maca extract method that patent No. CN201310523259 mentions, it does not carry out enzyme deactivation to Maca powder, super-micro wall-broken processing, thus can damage glucosinolate constituents.Patent No. CN201310457767, owing to having adopted the organic solvent residuals such as ethyl acetate, can cause the pollution of extract, and on future products, application has great impact.It does not carry out the deactivation of enzyme patent No. CN201210371187 to Maca powder, thereby can damage glucosinolate constituents.CN03128262, CN201410014874 adopt HP-20 macroporous resin column, neutral alumina column, high speed adverse current chromatogram the method such as to prepare to prepare extract, more difficult application in commercial production.Therefore, searching out a kind of Lepidinm meyenii Walp extraction efficiency process for extracting high, that purity is high is very important.
Summary of the invention
Object of the present invention provides a kind of extraction ratio high, and active component destroys few, avoids aborning using explosives, and device therefor is also common equipment, and the processing that is applicable to enterprise is extracted.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation extraction process of Lepidinm meyenii Walp extract, comprises the following steps:
1) deactivation of enzyme: adopt ultra high pressure treatment to carry out pheron deactivation Lepidinm meyenii Walp root, obtain the raw material after supertension inactivation treatment;
2) pulverize: the raw material after the inactivation treatment that previous step is obtained carries out micronizing broken wall treatment, obtain breaking cellular wall superfine powder;
3) lixiviate: the breaking cellular wall superfine powder that adopts ethanol-surfactant mixing lixiviating solution to obtain previous step carries out ultrasonic-leaching, stirring after lixiviate, centrifugal, collection lixiviating solution;
4) filter: the lixiviating solution that previous step is collected passes through plate-and-frame filtration, ultrafiltration membrance filter successively, collect the filtrate that molecular weight is greater than 5000Da;
5) lyophilization: the molecular weight that previous step is collected is greater than the filtrate of 5000Da and carries out cryogenic temperature freezing drying processing, obtains Lepidinm meyenii Walp extract.
On the basis of technique scheme, the present invention can also do following improvement.
Further, step 1) described Lepidinm meyenii Walp root be Lepidinm meyenii Walp fresh with or the dry root of Lepidinm meyenii Walp, and described Lepidinm meyenii Walp is selected from any one or a few the mixing in purple Lepidinm meyenii Walp, black Lepidinm meyenii Walp, white Lepidinm meyenii Walp.
Further, step 1) condition of described ultra high pressure treatment is 100～600Mpa, processing time 5～15min.
Described supertension technique enzyme denaturing technology, food is put into sealing, the high-intensity physico-chemical property that can change food after applying high static pressure (general pressure) more than 100Mpa and maintaining certain hour, thereby reach a kind of processing method that changes enzymatic activity, compare and heat treatment method, can better reduce the loss of heat sensitivity composition of food, its process is a pure physical process, completely different from traditional heating of food treatment process mechanism, after food material volume in liquid medium is compressed, form the hydrogen bond of polymer substance stereochemical structure, the non-covalent bond such as ionic bond and hydrophobic bond changes, cause the inactivation of enzyme composition, but to the polymer substances such as protein and vitamin, the covalent bond of the materials such as mineral has no effect.
Further, step 2) particle diameter of described breaking cellular wall superfine powder is 300～1000 orders.
The Lepidinm meyenii Walp breaking cellular wall superfine powder that the present invention adopts superfine communication technique to obtain, its granule footpath is at 1-75 μ m, have quality controllable, save medical material, effectively stripping of functional component, the functional component extraction ratio advantage such as be greatly improved.
Further, step 3) described in surfactant be selected from any one or the multiple mixing in Tween-20, polyoxyethylene sorbitol acid anhydride monopalmitate, polyoxyethylene sorbitan monostearate and polyoxyethylenesorbitan sorbitan monooleate.
Further, step 3) described in the preparation method of ethanol-surfactant mixing lixiviating solution be: the surfactant that adds ethanol water gross mass 0.2～2wt% in the ethanol water that is 50～80v/v% to concentration of alcohol.
Further, step 3) in breaking cellular wall superfine powder be 1:5～1:30 with the mass ratio of ethanol-surfactant mixing lixiviating solution.
Further, step 3) in, described hyperacoustic frequency is 50-80Hz, and extracting temperature is 10～40 DEG C, and extraction time is 30～60min.
Further, step 3) in, the speed of described stirring is 15～45rpm, mixing time is 10～40 minutes.
Further, step 3) in, described centrifugal rotational speed is 2000～12000rpm.
Further, step 4) in, plate-and-frame filtration filter paper filtering order used number is 100-300 order; The molecular weight of described ultrafilter membrane membrance separation is 5000～10000Da, 25～40 DEG C of operative temperatures.
Plate-and-frame filtration is by stainless steel multilayer plate and frame type filter-press, be applicable to the following viscosity of concentration 50% lower, the less liquid of dregginess is done airtight filtration to reach purification, the requirement of the fine straining such as sterilizing, clarification, half fine straining, there is extensive use in industries such as pharmacy, chemical industry, food, be applied in the filtration of pharmaceutical factory's injection liquor, effect is excellent.
Ultrafilter membrane is that a kind of aperture specification is consistent, and specified pore diameter range is the micropore filtering film of 0.001～0.02 micron.A side at film imposes suitable pressure, just can sift out the solute molecule that is less than aperture, is greater than with isolated molecule amount the granule that 500 dalton, particle diameter are greater than 2～20 nanometers.Adopting the membrane filtering method of ultrafilter membrane taking pressure differential as motive force is ultrafiltration membrance filter.Ultrafilter membrane makes by acetate fiber or with the similar macromolecular material of its performance mostly, is suitable for separation and the enrichment of solute in Treatment Solution most, is also usually used in the separation of the colloidal suspensions that other isolation technics have been difficult to.
Further: step 5) temperature of described cryogenic temperature freezing drying is-20～-40 DEG C, the processing time is 6-12h.
The advantage of described cryogenic temperature freezing drying is, dry run is to carry out at very low temperature, and has substantially completely cut off air, has therefore effectively suppressed biology, chemistry or the physical change of extract, and preserved preferably active substance, keep the color and luster of raw material.
Second aspect present invention discloses a kind of Lepidinm meyenii Walp extract, adopts aforementioned extraction process to prepare.
In the Lepidinm meyenii Walp extract that extraction process of the present invention obtains, contain 2200～4500mg/100g benzyl mustard oil methods of glycosides, 140～240mg/100g total flavonoid composition, and 250～460mg/100g total saponins composition.
Third aspect present invention discloses the application of aforementioned extraction process at Lepidinm meyenii Walp manufacture field.
The present invention adopts the technology such as supertension enzyme denaturing, super-micro wall-broken pulverizing, the extraction of surfactant supersonic synergic, ultrafiltration and concentration, ultralow temperature are dried, greatly improve extraction process in the past, adopt method of the present invention, the concentrated powder of the effective ingredient in the Lepidinm meyenii Walp root finally obtaining.
Brief description of the drawings
Fig. 1 is the preparation extraction process flow chart of Lepidinm meyenii Walp extract.
Detailed description of the invention
Below in conjunction with accompanying drawing, principle of the present invention and feature are described, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
Lepidinm meyenii Walp root is cleaned and put into extra-high tension unit, and setting pressure is 100Mpa, processing time 15min clock.The Lepidinm meyenii Walp root obtaining is joined to superfine powder high speed Universalpulverizer and carry out broken wall treatment, obtain 600 object Lepidinm meyenii Walp breaking cellular wall superfine powder.According to solid-to-liquid ratio 1:10, add the alcoholic solution of 50v/v%, and add the Tween-20 surfactant of total solution weight 0.2%, and to put in ultrasonic device, setting supersonic frequency is 50Hz, extracting temperature is 20 DEG C, after extracting 60min, stir, mixing speed is 30rpm, and mixing time is 10min, adopting rotating speed is that 2000rpm is centrifugal, collects filtrate.Gained filtrate is processed through the plate-and-frame filtration equipment of 1 μ m and 0.2 μ m successively, extract altogether twice, merging filtrate, gained clear filtrate is through ultrafiltration membrance filter device processes, and isolated molecule amount is 5000Da, and operative temperature is 25 DEG C, collect the liquid of molecular weight > 5000Da, gained liquid is dry through-40 DEG C of ultra low temperature vacuums, and be 6h drying time, obtains Lepidinm meyenii Walp extract powder.
Embodiment 2
Lepidinm meyenii Walp root is cleaned and put into extra-high tension unit, and setting pressure is 300Mpa, processing time 10min clock.The Lepidinm meyenii Walp root obtaining is joined to superfine powder high speed Universalpulverizer and carry out broken wall treatment, obtain 300 object Lepidinm meyenii Walp breaking cellular wall superfine powder.According to solid-to-liquid ratio 1:20, add the alcoholic solution of 70v/v%, and add 1% polyoxyethylene sorbitol acid anhydride monopalmitate of total solution weight, and to put in ultrasonic device, setting supersonic frequency is 60Hz, extracting temperature is 30 DEG C, after extracting 30min, stir, mixing speed is 15rpm, and mixing time is 20min, adopting rotating speed is that 5000rpm is centrifugal, collects filtrate.Gained filtrate is processed through the plate-and-frame filtration equipment of 1 μ m and 0.2 μ m successively, extract altogether twice, merging filtrate, gained clear filtrate is through ultrafiltration membrance filter device processes, and isolated molecule amount is 6000Da, and operative temperature is 25 DEG C, collect the liquid of molecular weight > 6000Da, gained liquid is dry through-30 DEG C of ultra low temperature vacuums, and be 7h drying time, obtains Lepidinm meyenii Walp extract powder.
Embodiment 3
Lepidinm meyenii Walp root is cleaned and put into extra-high tension unit, and setting pressure is 500Mpa, processing time 5min clock.The Lepidinm meyenii Walp root obtaining is joined to superfine powder high speed Universalpulverizer and carry out broken wall treatment, obtain 800 object Lepidinm meyenii Walp breaking cellular wall superfine powder.According to solid-to-liquid ratio 1:5, add the alcoholic solution of 70v/v%, and add 0.6% polyoxyethylene sorbitan monostearate of total solution weight, and to put in ultrasonic device, setting supersonic frequency is 55Hz, extracting temperature is 25 DEG C, after extracting 40min, stir, mixing speed is 25rpm, and mixing time is 16min, adopting rotating speed is that 3000rpm is centrifugal, collects filtrate.Gained filtrate is processed through the plate-and-frame filtration equipment of 1 μ m and 0.2 μ m successively, extract altogether twice, merging filtrate, gained clear filtrate is through ultrafiltration membrance filter device processes, and isolated molecule amount is 7000Da, and operative temperature is 25 DEG C, collect the liquid of molecular weight > 7000Da, gained liquid is dry through-35 DEG C of ultra low temperature vacuums, and be 7h drying time, obtains Lepidinm meyenii Walp extract powder.
Embodiment 4
Lepidinm meyenii Walp root is cleaned and put into extra-high tension unit, and setting pressure is 600Mpa, processing time 5min clock.The Lepidinm meyenii Walp root obtaining is joined to superfine powder high speed Universalpulverizer and carry out broken wall treatment, obtain 1000 object Lepidinm meyenii Walp breaking cellular wall superfine powder.According to solid-to-liquid ratio 1:30, add the alcoholic solution of 80v/v%, and add 2% polyoxyethylenesorbitan sorbitan monooleate of total solution weight, and to put in ultrasonic device, setting supersonic frequency is 80Hz, extracting temperature is 10 DEG C, after extracting 50min, stir, mixing speed is 45rpm, and mixing time is 40min, adopting rotating speed is that 12000rpm is centrifugal, collects filtrate.Gained filtrate is processed through the plate-and-frame filtration equipment of 1 μ m and 0.2 μ m successively, extract altogether twice, merging filtrate, gained clear filtrate is through ultrafiltration membrance filter device processes, and isolated molecule amount is 10000Da, and operative temperature is 40 DEG C, collect the liquid of molecular weight > 10000Da, gained liquid is dry through-20 DEG C of ultra low temperature vacuums, and be 12h drying time, obtains Lepidinm meyenii Walp extract powder.
The detection of embodiment 5 Lepidinm meyenii Walp extracts
Implement in obtained Lepidinm meyenii Walp extract by the inventive method, effective substance result is as shown in table 1 below.
Table 1 Lepidinm meyenii Walp extract effective substance result
Implement by method of the present invention, can enrichment obtain the extract that content range is 2200～4500mg/100g benzyl mustard oil methods of glycosides, 140～240mg/100g total flavonoid composition, 250～460mg/100g total saponins composition.
The present invention is taking the benzyl mustard oil glycosides in Lepidinm meyenii Walp extract, total flavones, total Saponin as main examination criteria, set up Lepidinm meyenii Walp amide, Lepidinm meyenii Walp alkene different from other patents of declaring, main cause is, Lepidinm meyenii Walp amide and Lepidinm meyenii Walp alkene content in Lepidinm meyenii Walp is very low is approximately ten thousand/, kind has 8,9 kind more than, and its do not exist at present corresponding in mark, external standard standard substance, there is very large defect in existing detection method, error is very large, can not objectively reflect the quality of extract own.Therefore, this patent is in order better to weigh Lepidinm meyenii Walp extract quality, benzyl mustard oil glycosides, total flavones, total these three kinds of materials of Saponin are adopted first, three has the detection method of content of comparison scientific and precise, and its biological effect also has reported literature support widely, be suitable as the standard of weighing Lepidinm meyenii Walp extract quality.
The detection method of benzyl mustard oil glycosides is internal standard method, list of references, and Piace nte S was published in the method adopting in " Journal of Agricultural and Food Chemistry " in 2002.Name of document is the method that Investigation of the tuber constituents of maca (Lepidium meyenii Walp.) flavone, Saponin detection method are regulation in " health food inspection and assessment technique specification 2003 ".
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a preparation extraction process for Lepidinm meyenii Walp extract, comprises the following steps:
1) deactivation of enzyme: adopt ultra high pressure treatment to carry out pheron deactivation Lepidinm meyenii Walp root, obtain the raw material after supertension inactivation treatment;
2) pulverize: the raw material after the inactivation treatment that previous step is obtained carries out micronizing broken wall treatment, obtain breaking cellular wall superfine powder;
3) lixiviate: the breaking cellular wall superfine powder that adopts ethanol-surfactant mixing lixiviating solution to obtain previous step carries out ultrasonic-leaching, stirring after lixiviate, centrifugal, collection lixiviating solution;
4) filter: the lixiviating solution that previous step is collected passes through plate-and-frame filtration, ultrafiltration membrance filter successively, collect the filtrate that molecular weight is greater than 5000Da;
5) lyophilization: the molecular weight that previous step is collected is greater than the filtrate of 5000Da and carries out cryogenic temperature freezing drying processing, obtains Lepidinm meyenii Walp extract.
2. extraction process as claimed in claim 1, is characterized in that step 1) condition of described ultra high pressure treatment is 100～600Mpa, processing time 5～15min.
3. extraction process as claimed in claim 1, is characterized in that step 2) particle diameter of described breaking cellular wall superfine powder is 300～1000 orders.
4. extraction process as claimed in claim 1, it is characterized in that step 3) described in surfactant be selected from any one or the multiple combination in Tween-20, polyoxyethylene sorbitol acid anhydride monopalmitate, polyoxyethylene sorbitan monostearate and polyoxyethylenesorbitan sorbitan monooleate.
5. the extraction process as described in claim as arbitrary in claim 1 or 4, it is characterized in that step 3) described in the preparation method of ethanol-surfactant mixing lixiviating solution be: the surfactant that adds ethanol water gross mass 0.2～2wt% in the ethanol water that is 50～80v/v% to concentration of alcohol.
6. extraction process as claimed in claim 1, is characterized in that step 3) in, described hyperacoustic frequency is 50-80Hz, and extracting temperature is 10～40 DEG C, and extraction time is 30～60min.
7. extraction process as claimed in claim 1, is characterized in that step 4) in, plate-and-frame filtration filter paper filtering order used number is 100-300 order; The molecular weight of described ultrafilter membrane membrance separation is 5000～10000Da, 25～40 DEG C of operative temperatures.
8. extraction process as claimed in claim 1, is characterized in that step 5) temperature of described cryogenic temperature freezing drying is-20～-40 DEG C, the processing time is 6-12h.
9. a Lepidinm meyenii Walp extract, adopts extraction process described in claim 1-8 arbitrary claim to prepare.
Described in the arbitrary claim of claim 1-8 extraction process in the application of Lepidinm meyenii Walp manufacture field.
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| 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 |
| CN104904969A (en) * | 2015-05-12 | 2015-09-16 | 甘肃省轻工研究院 | Maca coffee |
| CN105663177A (en) * | 2016-04-13 | 2016-06-15 | 滁州学院 | Fresh medicine processing method |
| CN105767345A (en) * | 2014-12-22 | 2016-07-20 | 康美（北京）药物研究院有限公司 | Instant Maca tea, preparation method of instant Maca tea and Maca product |
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| CN108272848A (en) * | 2018-04-18 | 2018-07-13 | 佛山市飞程信息技术有限公司 | A kind of extraction process of Maca extract |
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| CN109082911A (en) * | 2018-07-05 | 2018-12-25 | 佛山市衣香蒂丝服装设计有限公司 | A kind of colouring method of dye yam extracting solution to silk fabric |
| CN109401358A (en) * | 2017-08-16 | 2019-03-01 | 冯顺珍 | A method of haematochrome is extracted from Jasmine flower residue |
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| CN105767345A (en) * | 2014-12-22 | 2016-07-20 | 康美（北京）药物研究院有限公司 | Instant Maca tea, preparation method of instant Maca tea and Maca product |
| CN105981876A (en) * | 2015-02-04 | 2016-10-05 | 玛卡龙酒业有限公司 | Maca coffee and preparation method thereof |
| 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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| CN104904969A (en) * | 2015-05-12 | 2015-09-16 | 甘肃省轻工研究院 | Maca coffee |
| CN105663177A (en) * | 2016-04-13 | 2016-06-15 | 滁州学院 | Fresh medicine processing method |
| CN106108008A (en) * | 2016-06-24 | 2016-11-16 | 丽江师范高等专科学校 | A kind of extracting method of effective component in Maka |
| CN106668115A (en) * | 2017-02-10 | 2017-05-17 | 烟台新时代健康产业有限公司 | Method for extracting active ingredients from maca |
| CN109401358A (en) * | 2017-08-16 | 2019-03-01 | 冯顺珍 | A method of haematochrome is extracted from Jasmine flower residue |
| CN108272848A (en) * | 2018-04-18 | 2018-07-13 | 佛山市飞程信息技术有限公司 | A kind of extraction process of Maca extract |
| CN108451996A (en) * | 2018-04-18 | 2018-08-28 | 佛山市飞程信息技术有限公司 | A method of preparing maca extract |
| CN109082911A (en) * | 2018-07-05 | 2018-12-25 | 佛山市衣香蒂丝服装设计有限公司 | A kind of colouring method of dye yam extracting solution to silk fabric |
| CN112294857A (en) * | 2020-11-02 | 2021-02-02 | 广东青云山药业有限公司 | Maca powder rich in glucosinolates and preparation method thereof |
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