CN103980383B - The preparation method of a kind of maca polysaccharide and glucosinolate - Google Patents
The preparation method of a kind of maca polysaccharide and glucosinolate Download PDFInfo
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- CN103980383B CN103980383B CN201410246829.XA CN201410246829A CN103980383B CN 103980383 B CN103980383 B CN 103980383B CN 201410246829 A CN201410246829 A CN 201410246829A CN 103980383 B CN103980383 B CN 103980383B
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Abstract
The invention discloses the preparation method of a kind of maca polysaccharide and glucosinolate, comprise the following steps: agate coffee raw material pulverizing, after ethanol wet, through microwave ethanol-extracted, freezing and crystallizing filters to obtain maca polysaccharide, and concentrating filter liquor acidification filters to obtain agate coffee glucosinolate.The present invention is safe and simple, maca polysaccharide and glucosinolate productive rate and purity high, and technique is simple, easy to operate, is easy to continuous large-scale production.
Description
Technical field
The present invention relates to the technique of a kind of microwave extraction maca polysaccharide and glucosinolate, specifically first by the pueraria root powder ethanol wet after pulverizing, then through microwave ethanol-extracted, freezing and crystallizing sedimentation obtains maca polysaccharide, after desugar alcoholic solution is concentrated, obtain the thick glucosinolate of agate coffee through acidification.The invention belongs to field of natural organic chemistry.
Background technology
Agate coffee (Maca), originates in Peru, 2003 in Yunnan successful introduction, wherein outstanding with the quality of Lijing Yulong Xueshan.Containing abundant active substance in fresh agate coffee, wherein carbohydrate containing more than 40%, glucosinolate 5% ~ 10%.
Agate coffee carbohydrate is in the majority with polysaccharide content.Domestic scholars is studied each kind of plant, animal, microbial polysaccharide, and prove that polysaccharide has antitumor, anti-oxidant, immunity moderation power, reducing blood-fat, hypoglycemic, antibacterial isoreactivity, there are some researches show, maca polysaccharide has very strong anti-oxidant activity.
Glucosinolate and degradation production benzyl isothiocyanide thereof are considered to one of effective constituent of agate coffee, and it as agent for increasing testosterone level, and can improve the sexuality of learning and memory and the male sex; Separately there are some researches show that glucosinolate and isosulfocyanate material have effect of anti-kinds cancer, 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, and allyl group isosulfocyanate and PITC have supression effect to lung tumors transfer.
Generally adopt water extraction, alcohol deposition method to the extraction of polysaccharide at present, the extremely sad filter of solution after this method water extraction, concentrated not only energy consumption is high, and easily bubbles, and thickening efficiency is extremely low; Need gradient alcohol precipitation, not only technique is loaded down with trivial details simultaneously, and consumes a large amount of ethanolic solns.The report of current glucosinolate mostly is its Study on Physiological Activity, and several sections that rarely have are extracted the crude extract that report is glucosinolate, and adopt noxious solvent to extract, product purity is low and added value is low, strongly limit its application.
Summary of the invention
The object of the invention is to the deficiency overcoming prior art, a kind of method of applicable green continuous seepage high-quality maca polysaccharide and glucosinolate is provided.
The object of the invention is to be achieved through the following technical solutions:
A preparation method for maca polysaccharide and glucosinolate, comprises the steps:
Step one: raw material pulverizing, wetting
(1) the agate coffee ethanol uniform wet for fourth or powder will be pulverized.
(2) described (1) pueraria root powder particle degree is 0.5mm ~ 30mm, and alcohol concn used is 90.0% ~ 95.0%, and ethanol consumption is 0.5 ~ 2.0 times of agate coffee weight.
Step 2: microwave ethanol-extracted
(1) above-mentioned wetting after agate coffee, adopt microwave high concentration ethanol to extract, filter after extraction and obtain maca polysaccharide and glucosinolate extracting solution.
(2) described (1) extracts alcohol concn used is 90.0% ~ 95.0%, and ethanol consumption is 2 ~ 6 times of agate coffee weight, and Extracting temperature is 60 ~ 85 DEG C, and extraction time is 30min ~ 120min, and extraction time is 1 ~ 4 time.
(3) described (1) microwave frequency is 2450MHz.
Step 3: freezing and crystallizing is separated maca polysaccharide
(1) above-mentioned filtrate carries out the sedimentation of stirring freezing and crystallizing, filters and obtains filter residue and filtrate, obtain maca polysaccharide after filter residue and drying.
(2) described (1) freezing and crystallizing temperature is 0 ~ 25 DEG C, and the freezing and crystallizing time is 2h ~ 48h, and filter residue and drying temperature is 20 ~ 60 DEG C.
Step 4: acidification is separated agate coffee glucosinolate
(1) above-mentioned filtrate is through being evaporated to without after alcohol taste, and acid adding carries out acidification, and filter after leaving standstill 10 ~ 60min and obtain sour water insolubles, insolubles obtains agate coffee glucosinolate extract through washing drying.
(2) hydrochloric acid that described in, the acid used of (1) acidification is, sulfuric acid, phosphoric acid, Glacial acetic acid, citric acid, tartrate or matrimony vine acid etc., acid concentration is 0.5% ~ 10%, acid consumption is 2 ~ 10 times of concentrated solution weight, washing times is 1 ~ 5 time, washing water consumption is 2 ~ 10 times of insolubles weight, drying mode is lyophilize, vacuum-drying or heat pump drying, and drying temperature is-10 DEG C ~ 50 DEG C.
(3) described (1) concentrating under reduced pressure temperature is 40 ~ 65 DEG C, and vacuum tightness is-0.080 ~-0.095MPa.
The present invention compared with prior art tool has the following advantages:
1, the present invention adopts microwave extraction, and not only extraction time can shorten over half compared with traditional method, and can reduce by more than 20% energy consumption.
2, only use ethanol as solvent in the present invention, thus safe, nontoxic, pollution-free.
3, the present invention adopts ethanol as solvent, microwave extraction, can play sterilization simultaneously, go out enzyme, the effect of anti-glucosinolate degraded.
4, adopt high concentration ethanol to extract and can prevent the strong substance dissolves of starch, albumen and wetting ability, therefore extracting solution impurity is few, and the aftertreatments such as filtration, concentration and recovery solvent are easy.
5, the present invention can obtain maca polysaccharide and agate coffee glucosinolate simultaneously, and process is simple, maca polysaccharide and glucosinolate productive rate and purity high, energy consumption and loss of material low, easy to operate, easily realize serialization industrial production.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
By following embodiment and accompanying drawing thereof, the present invention is described in further detail, but embodiments of the present invention are not limited thereto, and for the processing parameter do not indicated especially, can refer to routine techniques and carry out.
Embodiment 1
A kind of microwave extraction maca polysaccharide and glucosinolate method, step and condition as follows:
Step one: raw material pulverizing, wetting
10.00kg agate coffee (containing maca polysaccharide 5.26%, glucosinolate 4.05%) is ground into powder (granularity is 1.0mm) and then uses 5.00kg ethanol (concentration is 90.0%) uniform wet.
Step 2: microwave height ethanol-extracted
Above-mentioned wetting after pueraria root powder, adopt microwave high concentration ethanol to extract, alcohol concn used is 90.0%, ethanol consumption 30.00kg, and Extracting temperature is 85.0 DEG C, and extraction time is 50min, and extraction time is 4 times.Microwave frequency is 2450MHz.
The alcohol extract obtained containing maca polysaccharide and glucosinolate is filtered after extraction.
Step 3: freezing and crystallizing is separated maca polysaccharide
Above-mentioned alcohol extract is through stirring freezing and crystallizing sedimentation, filtration obtains filter residue and filtrate, filter residue obtains 501.2g white maca polysaccharide (polysaccharide content 92.82% through 50.0 DEG C of vacuum-dryings (vacuum tightness-0.099MPa), percentage extraction is 88.44%), wherein freezing temp is 0.0 DEG C, and freezing time is 6.0h.
Step 4: acidification is separated agate coffee glucosinolate
Above-mentioned filtrate is through being evaporated to without after alcohol taste (solution weight is 2.65kg), and acid adding carries out acidification, and suction filtration after standing 20min, obtains sour water insolubles.Acidification acid used is the hydrochloric acid of 0.5%, and sour consumption is 20.00kg.Concentrating under reduced pressure temperature is 65 DEG C, and vacuum tightness is-0.080MPa.Gained insolubles 2.50kg distilled water wash 2 times, 25.0 DEG C of heat pump dryings obtain 502.3g glucosinolate (glucosinolate content 74.31%, percentage extraction is 92.15%).
Described polysaccharide content detects sees NYT1676-2008: the mensuration of Crude polysaccharides content in edible mushrooms, glucosinolate content detects NY/T1103.3-2006: the mensuration of glucosinolate.
Embodiment 2
A kind of microwave extraction maca polysaccharide of the present embodiment and glucosinolate method, except for the following differences, other steps and processing condition thereof are with embodiment 1:
(1) raw material is agate coffee fourth, and granularity is 30mm.
(2) wetting ethanol weight used is 10.00kg, and alcohol concn is 92.0%.
(3) microwave extraction ethanol weight used is 40.00kg, and alcohol concn is 92.0%, and Extracting temperature is 75.0 DEG C, and extraction time is 80min, extraction time 3 times.
(4) freezing and crystallizing temperature is 10.0 DEG C, and the freezing and crystallizing time is 24.0h.
(5) polysaccharide crystallization sediment drying mode is heat pump drying, and drying temperature is 35.0 DEG C.
(6) filtrate is concentrated into 2.73kg, and concentrating under reduced pressure temperature is 55 DEG C, and vacuum tightness is-0.090MPa.
(7) acidifying acid used is the citric acid of 5.0%, and sour consumption is 15.00kg, leaves standstill 40min.
(8) water washing consumption is 3.50kg, and washing times is 3 times.
(9) acid non-soluble substance drying mode is vacuum-drying, and drying temperature is 40.0 DEG C.
(10) gained maca polysaccharide 489.4g (polysaccharide content 93.43%, percentage extraction is 86.95%), agate coffee glucosinolate 520.1g (glucosinolate content is 73.47%, and percentage extraction is 94.35%).
Embodiment 3
A kind of microwave extraction maca polysaccharide of the present embodiment and glucosinolate method, except for the following differences, other steps and processing condition thereof are with embodiment 1:
(1) raw material is pueraria root powder, and granularity is 5.0mm.
(2) wetting ethanol weight used is 15.00kg, and alcohol concn is 95.0%.
(3) microwave extraction ethanol weight 50.00kg used is concentration, and ethanol is 95.0%, Extracting temperature 65.0 DEG C, and extraction time is 120min, extraction time 2 times.
(4) freezing and crystallizing temperature is 20.0 DEG C, and the freezing and crystallizing time is 48.0h.
(5) polysaccharide crystallization sediment drying mode is vacuum-drying, and drying temperature is 50.0 DEG C.
(6) filtrate is concentrated into 2.64kg, and concentrating under reduced pressure temperature is 45 DEG C, and vacuum tightness is-0.095MPa.
(7) acidifying acid used is the matrimony vine acid of 8.0%, and sour consumption is 10.00kg, leaves standstill 60min.
(8) water washing consumption is 5.00kg, and washing times is 4 times.
(9) acid non-soluble substance drying mode is lyophilize, and drying temperature is 10 DEG C.
(10) gained maca polysaccharide 463.7g (polysaccharide content 94.43%, percentage extraction is 83.25%), agate coffee glucosinolate 511.7g (glucosinolate content is 75.47%, and percentage extraction is 95.35%).
Claims (10)
1. a preparation method for maca polysaccharide, is characterized in that, comprises the steps:
Step one: raw material pulverizing, wetting
By the agate coffee fourth after pulverizing or pueraria root powder high concentration ethanol uniform wet;
Step 2: microwave ethanol-extracted
Above-mentioned wetting after agate coffee, adopt microwave high concentration ethanol to extract, filter the extracting solution obtained containing maca polysaccharide and glucosinolate after extraction, described Extracting temperature is 60 ~ 85 DEG C, and extraction time is 30min ~ 120min, and extraction time is 1 ~ 4 time;
Step 3: freezing and crystallizing is separated maca polysaccharide
Said extracted liquid carries out the sedimentation of stirring freezing and crystallizing, filters to obtain filter residue and filtrate, obtains maca polysaccharide after filter residue and drying.
2. method according to claim 1, is characterized in that, step one, two alcohol concn used are volume fraction 90.0% ~ 95.0%, and described grinding particle size is 0.5mm ~ 30mm.
3. method according to claim 2, is characterized in that, in step one, ethanol consumption is 0.5 ~ 2.0 times of agate coffee weight; In step 2, ethanol consumption is 2 ~ 6 times of agate coffee weight.
4. the method according to claim 1 or 2 or 3, it is characterized in that, described freezing and crystallizing temperature is 0 ~ 25 DEG C, the freezing and crystallizing time is 2h ~ 48h, and filter residue and drying temperature is 20 ~ 60 DEG C.
5. method according to claim 4, is characterized in that, step 2 microwave frequency is 2450MHz.
6. a preparation method for glucosinolate, is characterized in that, comprises the steps:
By filtrate obtained for method described in Claims 1 to 5 any one through being evaporated to without after alcohol taste, acid adding carries out acidification, and filter after leaving standstill 10 ~ 60min and obtain sour water insolubles, insolubles obtains glucosinolate through washing drying.
7. method according to claim 6, it is characterized in that, the acid used of described acidification is hydrochloric acid, sulfuric acid, phosphoric acid, Glacial acetic acid, citric acid, tartrate or matrimony vine acid, and the concentration of described acid is 0.5% ~ 10%, and sour consumption is 2 ~ 10 times of concentrated solution weight.
8. the method according to claim 6 or 7, is characterized in that, described concentrating under reduced pressure temperature is 40 ~ 65 DEG C, and vacuum tightness is-0.08 ~-0.095MPa.
9. the method according to claim 6 or 7, is characterized in that, described washing times is 1 ~ 5 time, and washing water consumption is 2 ~ 10 times of insolubles weight.
10. the method according to claim 6 or 7, is characterized in that, the mode of described drying is lyophilize, vacuum-drying or heat pump drying, and drying temperature is-10 DEG C ~ 50 DEG C.
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| CN104621436B (en) * | 2014-10-10 | 2017-12-15 | 浙江玛卡人生生物工程研究所 | A kind of Maca extract removes sugared technique |
| CN104207134B (en) * | 2014-10-11 | 2016-05-11 | 王衍彬 | A kind of preparation method of agate coffee extract |
| CN104257717A (en) * | 2014-10-13 | 2015-01-07 | 昆明固康保健品有限公司 | Preparation of high-activity Maca extract as well as compound preparation formula and application of Maca extract |
| CN105767345B (en) * | 2014-12-22 | 2021-02-19 | 康美（北京）药物研究院有限公司 | Maca instant tea, preparation method thereof and maca product |
| CN105581333A (en) * | 2015-12-30 | 2016-05-18 | 重庆骄王天然产物股份有限公司 | Fully-nutritional Maca powder and preparation method thereof |
| CN105832801B (en) * | 2016-05-22 | 2020-02-04 | 尹梦珍 | Extraction and separation method of macaene and macamide |
| CN106632534A (en) * | 2016-09-29 | 2017-05-10 | 广州市汇吉科技企业孵化器有限公司 | Process for extracting Glucosinolates from Moringa oleifera and application of Glucosinolates |
| CN107312046A (en) * | 2017-06-12 | 2017-11-03 | 安徽阳光药业有限公司 | The preparation method and Maca buccal tablets of glucosinolate in maca |
| CN109453300B (en) * | 2018-12-29 | 2021-05-14 | 雨润慕德生物科技（连云港）有限公司 | Extraction method and application of macamide and glucosinolate |
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| CN103463123A (en) * | 2013-09-30 | 2013-12-25 | 云南省农业科学院药用植物研究所 | Method for extracting effective constituents from maca |
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| JP2006206509A (en) * | 2005-01-28 | 2006-08-10 | Ｔｏｗａ Ｃｏｒｐｏｒａｔｉｏｎ 株式会社 | Method for producing maca extract |
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|---|---|---|---|---|
| CN1473594A (en) * | 2003-07-01 | 2004-02-11 | 华中科技大学 | Extract of Maka root |
| CN102526161A (en) * | 2012-02-10 | 2012-07-04 | 中国科学院过程工程研究所 | Preparation method for high-activity lepidium meyenii extract |
| CN103463123A (en) * | 2013-09-30 | 2013-12-25 | 云南省农业科学院药用植物研究所 | Method for extracting effective constituents from maca |
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Effective date of registration: 20190125 Address after: 650051 Ciman Five Society, Huangshan Residential Committee, Shuhe Street, Gucheng District, Lijiang City, Yunnan Province Patentee after: Lijiang Yinghuangji Bioengineering Co., Ltd. Address before: 674100 Huangshan Neighborhood Committee of Shuhe Street, Ancient District of Lijiang City, Yunnan Province Patentee before: Lijing mill at the age of one hundred years old biotechnology development corporation, Ltd. |
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