CN102086237A - Method for preparing jujube polysaccharide from red dates and jujube polysaccharide - Google Patents
Method for preparing jujube polysaccharide from red dates and jujube polysaccharide Download PDFInfo
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- CN102086237A CN102086237A CN 201010606048 CN201010606048A CN102086237A CN 102086237 A CN102086237 A CN 102086237A CN 201010606048 CN201010606048 CN 201010606048 CN 201010606048 A CN201010606048 A CN 201010606048A CN 102086237 A CN102086237 A CN 102086237A
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Abstract
The invention provides a method for preparing jujube polysaccharide from red dates and the jujube polysaccharide. The method comprises the following steps: denucleating the red dates, and smashing the denucleated red dates to obtain smashed raw material particles, wherein the red dates are imperfect dried red dates; based on volume concentration, adding 60%-95% ethanol solution into the smashed raw material particles, carrying out microwave heating, wherein the mass ratio of the ethanol solution to the smashed raw material particles is (10-18): 1, microwave power is 70 watts-490 watts, and microwave heating time is 90 seconds-150 seconds; filtering the product subjected to microwave heating, so that precipitate A is obtained; and carrying out heating extraction and organic solvent impurity removal on the precipitate A so as to obtain the jujube polysaccharide. In the method, an extraction and pretreatment mode, namely microwave impurity removal, is adopted to simplify the process, so that the process flow is simple to operate, the cost is low, and the extraction ratio of the jujube polysaccharide is improved, and the functional property of the jujube polysaccharide is maintained; and the imperfect dried red dates are used as raw materials, thus the comprehensive utilization way of the imperfect dried red dates is broadened.
Description
Technical field
The present invention relates to foods processing technique, relate in particular to a kind of method and jujube polysaccharide that utilizes red date to produce the jujube polysaccharide.
Background technology
Jujube is the fruit of Rhamnaceae (Rhamnaceae) deciduous tree jujube tree.Red date is fragrant and sweet delicious, and is nutritious, is loved by the people.
The effect of red date " benefiting qi and nourishing blood " is mainly derived from the jujube polysaccharide, polysaccharide component in the red date has tangible anticomplementary activity, can reduce lipid peroxidation in mice plasma, the liver homogenate (LPO) level, promote normal and immunosuppressed mice peritoneal macrophage phagocytic function, promote lymphocyte transformation, large and small mouse model of blood dificiency, deficiency in both Qi and blood model are had better improvement effect.Various health care functions and biological activitys such as red jujube polysaccharide is anti-ageing in addition, raising antibody mediated immunity power, this has fully shown the possibility of red jujube polysaccharide widespread use in each field of food medical treatment.Along with to the deepening continuously of red jujube polysaccharide research, China's red date resource abundance in addition, the development and use of red jujube polysaccharide will have broad application prospects.
The existing method of utilizing the solvent leach extraction method to extract the jujube polysaccharide is generally: adopt high-quality date as raw material, add the solvent greater than 20 times of raw materials, extracting more than 5 hours under 90 ℃ the condition; Extract three times repeatedly and just can reach the good extraction effect.Thus, the existing method complex process of from red date, extracting the jujube polysaccharide, and contain impurity such as a large amount of monose, lipid, pigment in the extract, bring very big difficulty for follow-up purifying technique.
Summary of the invention
The object of the present invention is to provide a kind of method and jujube polysaccharide that utilizes red date to produce the jujube polysaccharide,, reduce extraction cost to simplify the extraction process of jujube polysaccharide.
The invention provides a kind of method of utilizing red date to produce the jujube polysaccharide, this method comprises:
With extracting red date stone, fragmentation obtains the raw material particle; Described red date is inferior extra dry red wine jujube;
Adding volumetric concentration in described raw material particle is the ethanolic soln of 60%-95%, carries out microwave heating then; The mass ratio of described ethanolic soln and described raw material particle is 10-18: 1, be preferably 12-16: and 1, more excellent is 14: 1; Microwave power is 70 watts-490 watts, is preferably 140 watts-420 watts, and more excellent is 210 watts; Microwave heating time is 90 seconds-150 seconds, is preferably 100 seconds-140 seconds, and more excellent is 120 seconds;
The microwave heating after product is filtered, obtain precipitate A;
Precipitate A after heating extraction and organic solvent removal of impurities, is obtained the jujube polysaccharide.
Wherein, the concentration of ethanolic soln is for being preferably 85%-95%, and more excellent is 90%.
Further, described precipitate A is extracted and the process of organic solvent removal of impurities comprises through heating:
Add solvent and heat lixiviate in precipitate A, Heating temperature is 75-85 ℃, 2.5-3.5 hour heat-up time; Product after the described heating lixiviate is filtered, obtain supernatant liquor; Described solvent is a water, and the mass ratio of described solvent and precipitate A is 12-18: 1;
After described supernatant concentration, cooling, add dehydrated alcohol;
The flocks filtration that the adding dehydrated alcohol is obtained obtains deposit B;
With deposit B oven dry, add entry and redissolve, add the chloroform layering again after, obtain aqueous layer;
With described aqueous layer decolouring, concentrated, oven dry.
Wherein, heat in the process of lixiviate at adding solvent in precipitate A, adjusting the pH value is 8.0-9.2.In process, with the 1/3-1/5 of described supernatant concentration to original volume with described supernatant concentration; Described dehydrated alcohol in the supernatant liquor after add concentrating with concentrate after the volume ratio of supernatant liquor be 3-6: 1.
The jujube polysaccharide that the present invention also provides a kind of method of the present invention to make.Jujube polysaccharide described in the present invention extracts from inferior extra dry red wine jujube by method provided by the invention.
The present invention adopts the extraction pretreatment process of microwave removal of impurities, can simplify technology, makes technical process simple to operate, and is with low cost, and improved the extraction yield of jujube polysaccharide, kept the functional performance of jujube polysaccharide; And the present invention is that raw material is made with inferior extra dry red wine jujube, has widened the comprehensive Utilization Ways of inferior red date.Thus, the method for producing the jujube polysaccharide that the present invention adopts, raw material is easy to get, product yield height, the making processes simple and effective, cost is low, is fit to suitability for industrialized production.
Description of drawings
The polysaccharide canonical plotting of Fig. 1 during for quantitative assay of the present invention.
Embodiment
For the purpose, technical scheme and the advantage that make the embodiment of the invention is clearer, below the technical scheme in the embodiment of the invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, rather than whole embodiment.
Embodiment one
The method embodiment one that utilizes red date to produce the jujube polysaccharide provided by the invention can may further comprise the steps:
Step 101, inferior extra dry red wine jujube is cleaned, dry surface-moisture.Wherein, the inferior extra dry red wine jujube among the present invention is meant the inferior red date after air-dry, and moisture content wherein is generally less than 25%.
The weather that the geography of China, soil and most of area are influenced by the subtropics monsoon is well suited for the growth of jujube tree, and China's jujube producing region distributes very wide thus.But because jujube tree result's many sub-features and management, gather, unmanageable factors such as airing, weather, annual all can produce a large amount of little jujubes, the jujube that falls, split inferior jujube fruit such as jujube, these inferior jujube fruits can't be caused great loss thus directly as commodity selling.Through discovering that jujube polysaccharide content in the inferior red date and exterior quality best possible merchandise jujube do not have significant difference.Thus, the present invention adopts inferior red date as raw material.
Step 102, with the inferior extra dry red wine jujube stoning that step 101 obtains, obtain inferior jujube meat.
Step 103, the inferior jujube meat that step 102 is obtained are crushed to 0.5mm-1.0mm.
Wherein, obtain product in the step 103 and be raw material particle of the present invention.
Step 104, the product that step 103 is obtained are packed in the container, add volumetric concentration and be 90% ethanolic soln; Add 90% alcoholic acid quality and be 14 times of product quality that step 103 obtains.
Step 105, the product that step 104 is obtained adopt microwave heating lixiviate removal of impurities; Wherein, microwave power is 210W; Microwave heating time is 120 seconds.
Step 106, the product that step 105 is obtained filter, and obtain solution and precipitation two portions; Wherein the precipitation that obtains of this step is precipitate A of the present invention.
Concrete filtering step can for: use earlier gauze coarse filtration, suction filtration again.Through this step, the jujube polysaccharide component is retained in the precipitation, and most of monose, lipid, impurity such as pigment are removed in solution.
Step 107, adding solvent heating lixiviate in the precipitation that step 106 obtains.Wherein, solvent is a water, and the quality that adds solvent is 12 times of precipitation quality, adjusts pH value to 9.2, and Heating temperature is 85 ℃, 2.5 hours heat-up times.
Step 108, the product that step 107 is obtained filter, and obtain supernatant liquor.
Step 109, the product that step 108 is obtained are concentrated into 1/4 of original volume, cooling.
Step 110, in the product that step 109 obtains, add 4 times of volume dehydrated alcohols, have flocks to produce, filter and obtain precipitation.
Step 111, the product oven dry that step 110 is obtained are with 10 times of quality water redissolution.
Step 112, in the product that step 111 obtains, add chloroform, behind the concuss, remove Deproteinization, recycle-water solution layer then behind the standing demix.
Concrete, the volume that adds chloroform be step 111 obtain the product volume 1/3; The time of concuss is 10 minutes.
Step 113, the aqueous layer that step 112 is obtained decolour.
Concrete, the step of decolouring can for: add the gac of 0.1% quality in this aqueous layer, place boiling water bath 10min, and constantly stir, cooled and filtered discards the gac filter residue, obtains settled solution.
Step 114, the product that step 113 is obtained concentrate, and oven dry obtains the jujube polysaccharide.
Embodiment two
Embodiment two is identical with the step of the foregoing description one, and its difference is, in embodiment two:
Alcoholic acid volumetric concentration in the step 104 is 85%, and quality is 12 times of the product quality that obtains of step 103;
In the step 105, microwave power is 280W; Microwave heating time is 100 seconds;
In the step 107, the quality that adds solvent is 18 times of precipitation quality, adjusts pH value to 8.0, and Heating temperature is 80 ℃, 3.5 hours heat-up times;
In the step 109, the product that step 108 is obtained is concentrated into 1/3 of original volume;
In the step 110, in the product that step 109 obtains, add 5 times of volume dehydrated alcohols;
In the step 111,, redissolve with 12 times of quality water with the product oven dry that step 110 obtains;
In the step 112, the volume that adds chloroform be step 111 obtain the product volume 1/2; The time of concuss is 15 minutes.
Embodiment three
Embodiment three is identical with the step of the foregoing description one, and its difference is, in embodiment three:
Alcoholic acid volumetric concentration in the step 104 is 80%, and quality is 16 times of the product quality that obtains of step 103;
In the step 105, microwave power is 420W; Microwave heating time is 140 seconds;
In the step 107, the quality that adds solvent is 15 times of precipitation quality, adjusts pH value to 8.8, and Heating temperature is 83 ℃, 3 hours heat-up times;
In the step 109, the product that step 108 is obtained is concentrated into 1/5 of original volume;
In the step 110, in the product that step 109 obtains, add 3 times of volume dehydrated alcohols;
In the step 111,, redissolve with 9 times of quality water with the product oven dry that step 110 obtains;
In the step 112, the volume that adds chloroform be step 111 obtain the product volume 1/4; The time of concuss is 12 minutes.
Embodiment four
Embodiment four is identical with the step of the foregoing description one, and its difference is, in embodiment four:
Alcoholic acid volumetric concentration in the step 104 is 95%, and quality is 15 times of the product quality that obtains of step 103;
In the step 105, microwave power is 140W; Microwave heating time is 110 seconds;
In the step 107, the quality that adds solvent is 16 times of precipitation quality, adjusts pH value to 9.2, and Heating temperature is 78 ℃, 2.8 hours heat-up times;
In the step 109, the product that step 108 is obtained is concentrated into 1/3 of original volume;
In the step 110, in the product that step 109 obtains, add 4.5 times of volume dehydrated alcohols;
In the step 111,, redissolve with 11 times of quality water with the product oven dry that step 110 obtains;
In the step 112, the volume that adds chloroform be step 111 obtain the product volume 1/4; The time of concuss is 8 minutes.
Embodiment five
Embodiment five is identical with the step of the foregoing description one, and its difference is, in embodiment five:
Alcoholic acid volumetric concentration in the step 104 is 85%, and quality is 13 times of the product quality that obtains of step 103;
In the step 105, microwave power is 300W; Microwave heating time is 130 seconds;
In the step 107, the quality that adds solvent is 14 times of precipitation quality, adjusts pH value to 8.5, and Heating temperature is 82 ℃, 3.2 hours heat-up times;
In the step 109, the product that step 108 is obtained is concentrated into 1/5 of original volume;
In the step 110, in the product that step 109 obtains, add 3.5 times of volume dehydrated alcohols;
In the step 111,, redissolve with 12 times of quality water with the product oven dry that step 110 obtains;
In the step 112, the volume that adds chloroform be step 111 obtain the product volume 1/2; The time of concuss is 9 minutes.
The jujube polysaccharide that obtains among the embodiment one to embodiment five is detected respectively, and the extraction yield that records jujube polysaccharide among the embodiment one to embodiment five is respectively 128.8mg/g, 130.1mg/g, 129.6mg/g, 129.2mg/g and 127.9mg/g.Wherein, this extraction yield is the extraction yield that extracts the jujube polysaccharide from inferior extra dry red wine jujube.
Detection method to the jujube polysaccharide is as follows:
A, to the qualitative detection of the jujube polysaccharide that extracts
The detection of A1, sample starch
(1) preparation of rare iodine liquid: balance takes by weighing 0.50g I, and 1.00g KI adds 10.0mL distilled water in a beaker, standby with the glass stick mixing.
(2) get two clean white plaques, add an amount of testing sample and an amount of amylose starch respectively, add 2-3 more respectively and drip iodine liquid, observe colour-change.This testing sample be above-mentioned system the jujube polysaccharide.
Experimental result: the starch solution group becomes blueness, and sample sets keeps iodine liquid former orange-yellow.So it is not starch-containing in the proof sample.
The detection of A2, total reducing sugar
(1) preparation of Morse reagent: get the 0.5g naphthyl alcohol with balance and use 95% dissolve with ethanol that configures, face with preceding preparation standby to 10mL.
(2) in a clean tube, add 2.5mL sample distilled water immersion liquid, add 3 of Morse reagent, shake up immediately, test tube is tilted, slowly add vitriol oil 2.75mL along tube wall with liquid-transfering gun, can not jolting.Sulfuric acid layer is sunken to test tube bottom and sugar soln and is divided into two-layerly, observes the liquid level intersection and has or not the purple ring to occur.
Experimental result: have the purple ring to occur in the example reaction solution, detecting of carbohydrate arranged in the sample as can be known.
The detection of A3, monose
(1) preparation of expense beautiful jade reagent: balance takes by weighing 0.5g NaOH and be dissolved in 5mL distilled water in beaker, makes expense beautiful jade reagent a liquid, and is standby; Take by weighing the 0.25g anhydrous cupric sulfate in addition and be dissolved in 5mL distilled water, make expense beautiful jade reagent b liquid, standby.
(2) get two test tubes, wherein a test tube A adds with liquid-transfering gun and takes beautiful jade reagent a liquid 1mL, adds and takes beautiful jade reagent b liquid 1mL, adds 1mL behind the mixing immediately and prepares standby glucose solution; Another test tube B adds equally respectively and takes beautiful jade reagent a liquid and b liquid mixing adding later on sample distilled water solution 1mL.Test tube A, B all put into the hot water bath water-bath 5 minutes.Observe colour-change.
Experimental result: glucose solution produces brick-red precipitation with expense beautiful jade reagent react, and sample sets does not have brick-red precipitation, and produces Gu (OH)
2Blue precipitation is not so detect monose in the sample.
A4, proteinic detection
(1) preparation of ninhydrin reagent: balance takes by weighing the 0.10g triketohydrindene hydrate, is dissolved in the 100mL distilled water, and mixing is standby.
(2) getting 3 test tubes is respectively: A adds 2mL distilled water, and B adds 2mL sample distilled water solution, and C adds 2mL peptone powder liquid, adds 3,4 ninhydrin reagents that prepare then respectively, hot water bath 5 minutes, and colour-change is observed in the cooling back.
Experimental result: the C pipe becomes purple, and A pipe and B pipe color are constant, so do not detect protein in the sample.
By the qualitative detection result as can be known, the extract that obtains of the present invention is not starch-containing, monose and proteinic polysaccharose substance.
B, employing phenol sulfuric acid process are carried out detection by quantitative to the jujube polysaccharide that extracts
B1, polysaccharide typical curve are drawn:
The glucose standardized solution: get 0.2038g glucose and use the distilled water constant volume in the 100mL volumetric flask, get 0,1.0,2.0,3.0,4.0 respectively again, 5.0mL is constant volume in the 100mL volumetric flask, is made into standardized solution.
The 50mL vitriol oil is slowly added in the 10mL water, be cooled to room temperature after, add the 0.6g phenol crystal, stir and make dissolution of crystals, be made into colour developing liquid.
Get the 1mL standardized solution respectively in test tube, add 5mL colour developing liquid, concussion is evenly put and is incubated 30min in the boiling water bath, takes out, and is cooled to after the room temperature at 490nm place survey light absorption value.
The typical curve of gained polysaccharide as shown in Figure 1, the polysaccharide canonical plotting of Fig. 1 during for quantitative assay of the present invention.
B2, sample determination:
The jujube polysaccharide that embodiment one to embodiment five is made, getting 1g is dissolved in the 10ml distilled water, dilute 250 times then, according to the method mensuration polysaccharide content wherein in the above-mentioned typical curve drafting, the extraction yield that records jujube polysaccharide among the embodiment one to embodiment five is respectively 128.8mg/g, 130.1mg/g, 129.6mg/g, 129.2mg/g and 127.9mg/g.
Method provided by the invention, the extraction pretreatment process of employing microwave removal of impurities can be simplified technology, reduce the consumption of extraction solvent, reduce to extract the required time, make technical process simple to operate, with low cost, and improved the extraction yield of jujube polysaccharide, kept the functional performance of jujube polysaccharide; And the present invention is that raw material is made with inferior extra dry red wine jujube, has widened the comprehensive Utilization Ways of inferior red date.Thus, the method for producing the jujube polysaccharide that the present invention adopts, raw material is easy to get, product yield height, the making processes simple and effective, cost is low, and the jujube polyoses extract quality better, the purity height that obtain, is easy to preserve, and is fit to suitability for industrialized production.
It should be noted that at last: above embodiment only in order to technical scheme of the present invention to be described, is not intended to limit; Although with reference to previous embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that: it still can be made amendment to the technical scheme that aforementioned each embodiment put down in writing, and perhaps part technical characterictic wherein is equal to replacement; And these modifications or replacement do not make the essence of appropriate technical solution break away from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (10)
1. a method of utilizing red date to produce the jujube polysaccharide is characterized in that, comprising:
With extracting red date stone, fragmentation obtains the raw material particle; Described red date is inferior extra dry red wine jujube;
Adding volumetric concentration in described raw material particle is the ethanolic soln of 60%-95%, carries out microwave heating then; The mass ratio of described ethanolic soln and described raw material particle is 10-18: 1, and microwave power is 70 watts-490 watts, microwave heating time is 90 seconds-150 seconds;
The microwave heating after product is filtered, obtain precipitate A;
Precipitate A after heating extraction and organic solvent removal of impurities, is obtained the jujube polysaccharide.
2. the method for utilizing red date to produce the jujube polysaccharide according to claim 1 is characterized in that, the mass ratio of described ethanolic soln and described raw material particle is 12-16: 1.
3. the method for utilizing red date to produce the jujube polysaccharide according to claim 2 is characterized in that, the mass ratio of described ethanolic soln and described raw material particle is 14: 1.
4. the method for utilizing red date to produce the jujube polysaccharide according to claim 1 is characterized in that, described microwave power is 140 watts-420 watts.
5. the method for utilizing red date to produce the jujube polysaccharide according to claim 4 is characterized in that, described microwave power is 210 watts.
6. the method for utilizing red date to produce the jujube polysaccharide according to claim 1 is characterized in that, described microwave heating time is 100 seconds-140 seconds.
7. the method for utilizing red date to produce the jujube polysaccharide according to claim 6 is characterized in that, described microwave heating time is 120 seconds.
8. according to the arbitrary described method of utilizing red date to produce the jujube polysaccharide of claim 1-7, it is characterized in that, described precipitate A extracted and the process of organic solvent removal of impurities comprises through heating:
Add solvent and heat lixiviate in precipitate A, adjusting the pH value is 8.0-9.2, and Heating temperature is 75-85 ℃, 2.5-3.5 hour heat-up time; Product after the described heating lixiviate is filtered, obtain supernatant liquor; Described solvent is a water, and the mass ratio of described solvent and precipitate A is 12-18: 1;
After described supernatant concentration, cooling, add dehydrated alcohol;
The flocks filtration that the adding dehydrated alcohol is obtained obtains deposit B;
With deposit B oven dry, add entry and redissolve, add the chloroform layering again after, obtain aqueous layer;
With described aqueous layer decolouring, concentrated, oven dry.
9. the method for utilizing red date to produce the jujube polysaccharide according to claim 8 is characterized in that:
In the process with described supernatant concentration, with the 1/3-1/5 of described supernatant concentration to original volume;
Described dehydrated alcohol in the supernatant liquor after add concentrating with concentrate after the volume ratio of supernatant liquor be 3-6: 1.
10. jujube polysaccharide that the arbitrary described method of claim 1-9 makes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103284320A (en) * | 2013-06-09 | 2013-09-11 | 红云红河烟草(集团)有限责任公司 | Date palm extract and application thereof in cigarettes |
| CN103330157A (en) * | 2013-04-23 | 2013-10-02 | 申琳 | Red date extract extraction method and red date extracts |
| CN106109620A (en) * | 2016-07-14 | 2016-11-16 | 塔里木大学 | A kind of deep working method of Fructus Jujubae processing waste |
-
2010
- 2010-12-24 CN CN 201010606048 patent/CN102086237A/en active Pending
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| 《应用科技》 20081231 石奇等 微波法提取大枣多糖的工艺研究 55-57 1-10 第35卷, 第7期 * |
| 《延安大学学报（自然科学版）》 20061231 吕磊等 微波强化提取大枣多糖的研究 61-63,66 1-10 第25卷, 第2期 * |
| 《食品科学》 20051231 林勤保等 不同方法提取大枣多糖工艺的优化研究 368-371 1-10 第26卷, 第9期 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103330157A (en) * | 2013-04-23 | 2013-10-02 | 申琳 | Red date extract extraction method and red date extracts |
| CN103284320A (en) * | 2013-06-09 | 2013-09-11 | 红云红河烟草(集团)有限责任公司 | Date palm extract and application thereof in cigarettes |
| CN106109620A (en) * | 2016-07-14 | 2016-11-16 | 塔里木大学 | A kind of deep working method of Fructus Jujubae processing waste |
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Application publication date: 20110608 |