CN103275241A - Method for preparing rose apple nucleolus polysaccharide - Google Patents
Method for preparing rose apple nucleolus polysaccharide Download PDFInfo
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- CN103275241A CN103275241A CN2013102502277A CN201310250227A CN103275241A CN 103275241 A CN103275241 A CN 103275241A CN 2013102502277 A CN2013102502277 A CN 2013102502277A CN 201310250227 A CN201310250227 A CN 201310250227A CN 103275241 A CN103275241 A CN 103275241A
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Abstract
The invention relates to a method for preparing rose apple nucleolus polysaccharide, which comprises the following steps: (1) after drying and crushing rose apple nucleoli, adding the dried and crushed rose apple nucleoli into petroleum ether solution, performing water-bath heating reflux, then adding ethanol to carry out reflux after extraction filtration, and drying after extraction filtration; (2) adding dried powder into water and processing solution by using ultrasonic waves; (3) after finishing ultrasonic processing, regulating the pH value, adding cellulase and then performing enzymolysis and enzyme killing; and (4) removing precipitates in the solution which is subjected to enzyme killing and is cooled, taking out supernatant to carry out concentration, then adding chloroform and n-butyl alcohol mixed solution, centrifuging, taking out supernatant to be added with absolute ethyl alcohol precipitate polysaccharide, performing extraction filtration after standing, taking out solid matter to be washed sequentially by acetone, diethyl ether and absolute ethyl alcohol, and after drying, obtaining rose apple nucleolus polysaccharide powder. According to the invention, an ultrasonic-assisted enzymic method is adopted to extract the rose apple nucleolus polysaccharide; and not only is the method good in extracting effect, but also extraction time can be effectively shortened and production efficiency is improved.
Description
Technical field
The present invention relates to a kind of preparation method of water Portugal kernel polysaccharide.
Background technology
The water Portugal has another name called fragrant fruit, wind drum, mirabilitum crystallina pomegranate, belongs to Myrtaceae, and Syzygium is tropical perennial aiphyllium.Originate in India, the Malay Peninsula and Andaman.The 17th century is introduced China Taiwan, and successively introduce a fine variety in Hainan, Guangdong, Guangxi, Fujian and Yunnan after the thirties in 20th century.
The leaf of water Portugal, flower, fruit and seed can be as medicinal materials, and leaf and flower are mashed and can be controlled hemorrhoid, and the shell infusing drugs in wine has antiabortive and controls the effect of vomitting, and seed can be controled the inferior and be rushed down and dysentery characterized by blood in the stool.
Because Portugal belongs to the tropical and subtropical zone fruit tree, with respect to the cash crop that are grown in tropical and subtropical zone equally and other wide plants in growth region, for the relative much less of its research, really be to be phoenix feathers and unicorn horns at water Portugal kernel STUDY ON POLYSACHAROSE.
In the present disclosed document, record the test method of water Portugal kernel Crude polysaccharides in " response surface is optimized the Study on extraction of water Portugal kernel polysaccharide ", it mainly is to adopt water extraction to extract water Portugal kernel polysaccharide, extraction time reaches nearly 3 hours, extraction time is long, production efficiency is low, is unfavorable for suitability for industrialized production.
Summary of the invention
The technical problem to be solved in the present invention is: a kind of preparation method who adopts the ultrasound wave auxiliary enzyme method to extract the water Portugal kernel polysaccharide of water Portugal kernel polysaccharide is provided, this method not only extraction effect is good, and can shorten extraction time effectively, enhance productivity, solved above-mentioned problems of the prior art.
The technical scheme that solves the problems of the technologies described above is: a kind of preparation method of water Portugal kernel polysaccharide may further comprise the steps:
With water Portugal kernel be dried to moisture below 10% after, fragmentation obtains water Portugal kernel powder, adding volumetric concentration by solid-liquid ratio M:V=1:4-6 is in the 75-85% petroleum ether solution, in 45-50 ℃ of heating in water bath backflow 1-2h, press solid-liquid ratio M:V=1:4-6 behind the suction filtration and add volumetric concentration 75-85% ethanol in 55-65 ℃ of backflow 1-2h, dry behind the suction filtration to moisture content and obtain powder below 10%;
⑵ the powder after will dry is added to the water by solid-liquid ratio M:V=1:10-20, use power as the ultrasonic wave of 70-100W to solution-treated 10-20min, temperature maintenance is at 65-75 ℃ in the ultrasonication process;
⑶ after treat that ultrasonication finishes, regulating the pH value is 5-6, add cellulase, the cellulase consumption is the 1-2% of water Portugal kernel powder quality, put into constant temperature oscillator then, the adjusting rotating speed is 140-150r/min, and 50-60 ℃ of enzymolysis 50-60min places the 95-105 ℃ of water-bath enzyme 10-15min that goes out with the reactant behind the enzymolysis;
⑷ the enzyme that will go out is cooled to solution after 25-30 ℃, with the centrifugal 15-20min of the rotating speed of 3000-4000r/min, remove precipitation, get supernatant concentration, be concentrated into 1/4 of centrifugal preceding liquor capacity, obtain concentrated solution, chloroform-propyl carbinol the mixed solution that adds concentrated solution volume 1/4 then, centrifugal behind the maintenance 150-200 r/min vibration 10-20min, get the dehydrated alcohol precipitation polysaccharide that supernatant liquor adds 4 times of supernatant liquor volumes, put into then and leave standstill suction filtration behind the 10-14h in 0-4 ℃ the refrigerator, get solid substance successively with acetone, ether, absolute ethanol washing, washing is placed on 55-65 ℃ and is dried to moisture content and can obtains water Portugal kernel polysaccharide powder below 6%;
Material in the described solid-liquid ratio all is raw water Portugal kernel powder.
The volume ratio of chloroform and propyl carbinol is 4:1 in described chloroform-propyl carbinol mixed solution.
It is the 50-80 order that described water Portugal kernel is crushed to the order number.
Among the step ⑶, the material that is used for adjusting pH value is NaOH or HCl.
The Enzymatic Extraction polysaccharide has advantages such as reaction conditions gentleness, efficient height, impurity easily remove, technology is easy and save time, and ultrasonic technology has characteristics such as easy and simple to handle, that extraction rate is fast, efficient is high, power consumption is few.The preparation method of a kind of water Portugal kernel polysaccharide of the present invention, wherein adopted ultrasonic technology to assist Enzymatic Extraction water Portugal kernel polysaccharide, extraction time, only about 1 hour, this technology extraction effect was good, easy to use, cost is low, less investment has shortened the time of extracting greatly, shortens preparation time effectively, enhance productivity, be beneficial to suitability for industrialized production.Adopt the present invention to prepare water Portugal kernel polysaccharide, the yield of water Portugal kernel polysaccharide can reach 5.95%, and purity can reach 71.4%.
Below, the technical characterictic to the preparation method of a kind of water Portugal kernel polysaccharide of the present invention is further described in conjunction with the embodiments.
Embodiment
Embodiment 1: a kind of preparation method of water Portugal kernel polysaccharide may further comprise the steps:
With water Portugal kernel be dried to moisture below 10% after, be crushed to the order number and obtain water Portugal kernel powder for the 50-80 order, be that to add volumetric concentration be in 80% the petroleum ether solution to 1:5 (solid-liquid ratio M:V is the ratio of the volume mL of the quality g of water Portugal kernel powder and petroleum ether solution herein) by solid-liquid ratio, in 45-50 ℃ of heating in water bath backflow 1.5h, add volumetric concentration 80% ethanol in 60 ℃ backflow 1.5hs by solid-liquid ratio 1:5 (solid-liquid ratio M:V is the ratio of the volume mL of the quality g of water Portugal kernel powder and ethanol) herein behind the suction filtration, dry behind the suction filtration to moisture content and obtain powder below 10%.
⑵ the powder after will dry is added to the water by solid-liquid ratio 1:15 (solid-liquid ratio M:V is the ratio of the volume mL of the quality g of water Portugal kernel powder and water) herein, use power as the ultrasonic wave of 80W to solution-treated 15min, temperature maintenance is at 70 ℃ in the ultrasonication process.
⑶ after treat that ultrasonication finishes, utilizing NaOH or HCl to regulate the pH value is 5.5, add cellulase, the cellulase consumption is 1.6% of water Portugal kernel powder quality, put into constant temperature oscillator then, the adjusting rotating speed is 140-150r/min, and 55 ℃ of enzymolysis 50min place the 95-105 ℃ of water-bath enzyme 10-15min that goes out with the reactant behind the enzymolysis.
⑷ the enzyme that will go out is cooled to solution after 25-30 ℃ with the centrifugal 15-20min of the rotating speed of 3000r/min, remove precipitation, get supernatant concentration, be concentrated into 1/4 of centrifugal preceding liquor capacity, obtain concentrated solution, the back adds the chloroform-propyl carbinol mixed solution of concentrated solution volume 1/4, the volume ratio of chloroform and propyl carbinol is 4:1 in described chloroform-propyl carbinol mixed solution, keep centrifugal behind the 180 r/min vibration 10min, get the dehydrated alcohol precipitation polysaccharide that supernatant liquor adds 4 times of supernatant liquor volumes, put into then and leave standstill suction filtration behind the 10-14h in 4 ℃ the refrigerator, get solid substance successively with acetone, ether, absolute ethanol washing, washing is placed on 60 ℃ and is dried to moisture content and can obtains water Portugal kernel polysaccharide powder below 6%.
The yield of water Portugal kernel polysaccharide can reach 5.95% in the present embodiment, and purity can reach 71.4%.Utilize the ultrasound wave auxiliary enzyme method to extract water Portugal kernel polysaccharide, not only extraction effect is good, and can shorten extraction time effectively, enhances productivity.
Solid-liquid ratio of the present invention refers to the ratio of the volume of the quality of expecting and liquid; The mass unit of material is g, and the volume unit of liquid is mL.
Claims (4)
1. the preparation method of a water Portugal kernel polysaccharide is characterized in that: may further comprise the steps:
With water Portugal kernel be dried to moisture below 10% after, fragmentation obtains water Portugal kernel powder, adding volumetric concentration by solid-liquid ratio M:V=1:4-6 is in the 75-85% petroleum ether solution, in 45-50 ℃ of heating in water bath backflow 1-2h, press solid-liquid ratio M:V=1:4-6 behind the suction filtration and add volumetric concentration 75-85% ethanol in 55-65 ℃ of backflow 1-2h, dry behind the suction filtration to moisture content and obtain powder below 10%;
⑵ the powder after will dry is added to the water by solid-liquid ratio M:V=1:10-20, use power as the ultrasonic wave of 70-100W to solution-treated 10-20min, temperature maintenance is at 65-75 ℃ in the ultrasonication process;
⑶ after treat that ultrasonication finishes, regulating the pH value is 5-6, add cellulase, the cellulase consumption is the 1-2% of water Portugal kernel powder quality, put into constant temperature oscillator then, the adjusting rotating speed is 140-150r/min, and 50-60 ℃ of enzymolysis 50-60min places the 95-105 ℃ of water-bath enzyme 10-15min that goes out with the reactant behind the enzymolysis;
⑷ the enzyme that will go out is cooled to solution after 25-30 ℃, with the centrifugal 15-20min of the rotating speed of 3000-4000r/min, remove precipitation, get supernatant concentration, be concentrated into 1/4 of centrifugal preceding liquor capacity, obtain concentrated solution, chloroform-propyl carbinol the mixed solution that adds concentrated solution volume 1/4 then, centrifugal behind the maintenance 150-200 r/min vibration 10-20min, get the dehydrated alcohol precipitation polysaccharide that supernatant liquor adds 4 times of supernatant liquor volumes, put into then and leave standstill suction filtration behind the 10-14h in 0-4 ℃ the refrigerator, get solid substance successively with acetone, ether, absolute ethanol washing, washing is placed on 55-65 ℃ and is dried to moisture content and can obtains water Portugal kernel polysaccharide powder below 6%;
Material in the described solid-liquid ratio all is raw water Portugal kernel powder.
2. the preparation method of a kind of water Portugal kernel polysaccharide according to claim 1, it is characterized in that: the volume ratio of chloroform and propyl carbinol is 4:1 in described chloroform-propyl carbinol mixed solution.
3. the preparation method of a kind of water Portugal kernel polysaccharide according to claim 1, it is characterized in that: it is the 50-80 order that described water Portugal kernel is crushed to the order number.
4. the preparation method of a kind of water Portugal kernel polysaccharide according to claim 1 is characterized in that: among the step ⑶, be NaOH or HCl for the material of regulating the pH value.
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| CN201310250227.7A CN103275241B (en) | 2013-06-24 | 2013-06-24 | A kind of preparation method of water Portugal kernel polysaccharide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106108011A (en) * | 2016-06-25 | 2016-11-16 | 孙凤平 | A kind of water Jambul plant buccal tablet and preparation method thereof |
| CN110050933A (en) * | 2019-04-16 | 2019-07-26 | 嘉应学院 | A kind of hypoglycemic solid beverage and preparation method thereof of the active component of fruit containing Portugal |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102061322A (en) * | 2010-11-12 | 2011-05-18 | 盐城工学院 | Method for preparing polysaccharide, flavone and dietary fiber of peanut hulls in united manner |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102061322A (en) * | 2010-11-12 | 2011-05-18 | 盐城工学院 | Method for preparing polysaccharide, flavone and dietary fiber of peanut hulls in united manner |
Non-Patent Citations (3)
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| 易阳等: "龙眼多糖超声波-酶解辅助提取工艺优化", 《农业机械学报》, vol. 41, no. 5, 31 May 2010 (2010-05-31), pages 131 - 135 * |
| 曾凡梅等: "超声波协同纤维素酶提取山药多糖的工艺及组分测定研究", 《食品科技》, no. 2, 30 June 2010 (2010-06-30), pages 32 - 34 * |
| 程谦伟等: "响应面优化水蒲桃核仁多糖的提取工艺研究", 《食品工业》, no. 3, 31 December 2012 (2012-12-31), pages 20 - 23 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106108011A (en) * | 2016-06-25 | 2016-11-16 | 孙凤平 | A kind of water Jambul plant buccal tablet and preparation method thereof |
| CN110050933A (en) * | 2019-04-16 | 2019-07-26 | 嘉应学院 | A kind of hypoglycemic solid beverage and preparation method thereof of the active component of fruit containing Portugal |
| CN110050933B (en) * | 2019-04-16 | 2022-08-12 | 嘉应学院 | Hypoglycemic solid beverage containing effective parts of rose apple fruits and preparation method thereof |
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