CN103980383A - Preparation method of maca polysaccharide and mustard oil glycoside - Google Patents
Preparation method of maca polysaccharide and mustard oil glycoside Download PDFInfo
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- CN103980383A CN103980383A CN201410246829.XA CN201410246829A CN103980383A CN 103980383 A CN103980383 A CN 103980383A CN 201410246829 A CN201410246829 A CN 201410246829A CN 103980383 A CN103980383 A CN 103980383A
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Abstract
The invention discloses a preparation method of maca polysaccharide and mustard oil glycoside. The preparation method of the maca polysaccharide and mustard oil glycoside comprises the following steps: smashing a maca raw material, moistening with ethyl alcohol, and carrying out microwave ethanol extraction, freezing crystallization and filtering, so that the maca polysaccharide is obtained, and concentrating and acidizing filtrate, so that the mustard oil glycoside is obtained. The preparation method of the maca polysaccharide and mustard oil glycoside is safe and easy, yield and purity of the maca polysaccharide and mustard oil glycoside are high, a technology is simple, operation is easy, and continuous large scale production can be easily realized.
Description
Technical field
The present invention relates to the technique of a kind of microwave extraction maca polysaccharide and glucosinolate, be first that the pueraria root powder after pulverizing is wetting with ethanol specifically, then through microwave ethanol-extracted, freezing and crystallizing sedimentation obtains maca polysaccharide, after desugar alcoholic solution is concentrated, through acidification, obtain the thick glucosinolate of agate coffee.The invention belongs to natural organic chemistry field.
Background technology
Agate coffee (Maca), originates in Peru, and 2003 in Yunnan successful introduction, wherein outstanding with the quality of Lijing Yulong Xueshan.In fresh agate coffee, contain abundant active substance, carbohydrate containing more than 40% wherein, glucosinolate 5%～10%.
Agate coffee carbohydrate is in the majority with polysaccharide content.Domestic scholars is studied each kind of plant, animal, microbial polysaccharide, prove polysaccharide have antitumor, anti-oxidant, regulate immunizing 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 can be as agent for increasing testosterone level, and can improve learning and memory and the male sex's sexuality; Separately there are some researches show that glucosinolate and isosulfocyanate material have the effect of anti-kinds cancer, benzyl mustard oil glycosides and meta-methoxy benzyl mustard oil glycosides have good prophylactic effect to the tumour of a lot of tumours especially gastro-intestinal system, and allyl group isosulfocyanate and PITC shift and have supression effect lung tumors.
At present the extraction of polysaccharide is generally adopted to water extraction, alcohol deposition method, 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 pieces that rarely have are extracted the crude extract that report is glucosinolate, adopt noxious solvent to extract, and product purity is low and added value is low, has greatly limited its application.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art, provide a kind of applicable green to produce continuously the method for high-quality maca polysaccharide and glucosinolate.
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 1: raw material pulverizing, wetting
(1) the agate coffee of pulverizing as fourth or powder is evenly wetting with ethanol.
(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) the agate coffee after above-mentioned soaking, adopts microwave high concentration ethanol to extract, and after extraction, filters and obtains maca polysaccharide and glucosinolate extracting solution.
(2) described (1) to extract alcohol concn used be 90.0%～95.0%, and ethanol consumption is 2～6 times of agate coffee weight, and extracting temperature is 60～85 ℃, and extraction time is 30min～120min, and extraction time is 1～4 time.
(3) described (1) microwave frequency is 2450MHz.
Step 3: the separated maca polysaccharide of freezing and crystallizing
(1) above-mentioned filtrate is stirred freezing and crystallizing sedimentation, filters and obtains filter residue and filtrate, obtains maca polysaccharide after filter residue and drying.
(2) described (1) freezing and crystallizing temperature is 0～25 ℃, and the freezing and crystallizing time is 2h～48h, and filter residue and drying temperature is 20～60 ℃.
Step 4: the separated agate coffee of acidification glucosinolate
(1) above-mentioned filtrate is after being evaporated to without alcohol taste, and acid adding is carried out acidification, after standing 10～60min, filters and obtains sour water insolubles, and insolubles is through washing the dry agate coffee glucosinolate extract that obtains.
(2) described (1) acidification acid used is hydrochloric acid, 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 ℃～50 ℃.
(3) described (1) concentrating under reduced pressure temperature is 40～65 ℃, 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 halfly compared with traditional method, and can reduce by 20% above energy consumption.
2, in the present invention, only use ethanol as solvent, thus safe, nontoxic, pollution-free.
3, the present invention adopts ethanol to make solvent, and microwave extraction can play sterilization, the enzyme that goes out simultaneously, 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, so extracting solution impurity is few, 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, and maca polysaccharide and glucosinolate productive rate and purity are high, and energy consumption and loss of material are 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 to this, for not dated especially processing parameter, can carry out with reference to routine techniques.
Embodiment 1
Microwave extraction maca polysaccharide and a glucosinolate method, step and condition thereof are as follows:
Step 1: raw material pulverizing, wetting
10.00kg agate coffee (containing maca polysaccharide 5.26%, glucosinolate 4.05%) is ground into powder (granularity is 1.0mm) then uses 5.00kg ethanol (concentration is 90.0%) evenly wetting.
Step 2: the high ethanol-extracted of microwave
Pueraria root powder after above-mentioned soaking, adopts microwave high concentration ethanol to extract, and alcohol concn used is 90.0%, ethanol consumption 30.00kg, and extracting temperature is 85.0 ℃, and extraction time is 50min, and extraction time is 4 times.Microwave frequency is 2450MHz.
After extraction, filtration obtains the alcohol extract that contains maca polysaccharide and glucosinolate.
Step 3: the separated maca polysaccharide of freezing and crystallizing
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 ℃ of vacuum-dryings (vacuum tightness-0.099MPa), percentage extraction is 88.44%), wherein freezing temp is 0.0 ℃, and freezing time is 6.0h.
Step 4: the separated agate coffee of acidification glucosinolate
Above-mentioned filtrate is after being evaporated to without alcohol taste (solution weight is 2.65kg), and acid adding is carried out acidification, and suction filtration after standing 20min obtains sour water insolubles.The hydrochloric acid that acidification acid used is 0.5%, sour consumption is 20.00kg.Concentrating under reduced pressure temperature is 65 ℃, and vacuum tightness is-0.080MPa.2.50kg distilled water wash 2 times of gained insolubles, 25.0 ℃ 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 detection 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 ℃, and extraction time is 80min, extraction time 3 times.
(4) freezing and crystallizing temperature is 10.0 ℃, 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 ℃.
(6) filtrate is concentrated into 2.73kg, and concentrating under reduced pressure temperature is 55 ℃, and vacuum tightness is-0.090MPa.
(7) citric acid that acidifying acid used is 5.0%, sour consumption is 15.00kg, standing 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 ℃.
(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 used 50.00kg is concentration, and ethanol is 95.0%, extracts 65.0 ℃ of temperature, and extraction time is 120min, extraction time 2 times.
(4) freezing and crystallizing temperature is 20.0 ℃, and the freezing and crystallizing time is 48.0h.
(5) polysaccharide crystallization sediment drying mode is vacuum-drying, and drying temperature is 50.0 ℃.
(6) filtrate is concentrated into 2.64kg, and concentrating under reduced pressure temperature is 45 ℃, and vacuum tightness is-0.095MPa.
(7) the matrimony vine acid that acidifying acid used is 8.0%, sour consumption is 10.00kg, standing 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 ℃.
(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 1: raw material pulverizing, wetting
Agate coffee fourth after pulverizing or pueraria root powder is evenly wetting with high concentration ethanol;
Step 2: microwave ethanol-extracted
Agate coffee after above-mentioned soaking, adopts microwave high concentration ethanol to extract, and filters the extracting solution obtaining containing maca polysaccharide and glucosinolate after extraction, and described extraction temperature is 60～85 ℃, and extraction time is 30min～120min, and extraction time is 1～4 time;
Step 3: the separated maca polysaccharide of freezing and crystallizing
Said extracted liquid stirs freezing and crystallizing sedimentation, 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 1, 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 1, 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. according to the method described in claim 1 or 2 or 3, it is characterized in that, described freezing and crystallizing temperature is 0～25 ℃, and the freezing and crystallizing time is 2h～48h, and filter residue and drying temperature is 20～60 ℃.
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:
The filtrate that method described in claim 1～5 any one is made is after being evaporated to without alcohol taste, and acid adding is carried out acidification, after standing 10～60min, filters and obtains sour water insolubles, and insolubles is through washing the dry glucosinolate that obtains.
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. according to the method described in claim 6 or 7, it is characterized in that, described concentrating under reduced pressure temperature is 40～65 ℃, and vacuum tightness is-0.08～-0.095MPa.
9. according to the method described in claim 6 or 7, it is characterized in that, described washing times is 1～5 time, and washing water consumption is 2～10 times of insolubles weight.
10. according to the method described in claim 6 or 7, it is characterized in that, described dry mode is lyophilize, vacuum-drying or heat pump drying, and drying temperature is-10 ℃～50 ℃.
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| CN104207134A (en) * | 2014-10-11 | 2014-12-17 | 王衍彬 | Production method of maca extracts |
| 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 |
| CN104621436A (en) * | 2014-10-10 | 2015-05-20 | 浙江玛卡人生生物工程研究所 | Maca extract sugar-removing technology |
| 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 |
| 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 |
| CN105832801A (en) * | 2016-05-22 | 2016-08-10 | 深圳市先康达生物科技有限公司 | Extraction and separation method for macaenes and maca amides |
| 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 |
| CN109453300A (en) * | 2018-12-29 | 2019-03-12 | 雨润慕德生物科技（连云港）有限公司 | A kind of extracting method and its application of macamide and glucosinolate |
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| CN105832801A (en) * | 2016-05-22 | 2016-08-10 | 深圳市先康达生物科技有限公司 | Extraction and separation method for macaenes and maca amides |
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| 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 |
| CN109453300A (en) * | 2018-12-29 | 2019-03-12 | 雨润慕德生物科技（连云港）有限公司 | A kind of extracting method and its application of macamide and glucosinolate |
| 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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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. |