CN103330157A - Red date extract extraction method and red date extracts - Google Patents
Red date extract extraction method and red date extracts Download PDFInfo
- Publication number
- CN103330157A CN103330157A CN2013101436403A CN201310143640A CN103330157A CN 103330157 A CN103330157 A CN 103330157A CN 2013101436403 A CN2013101436403 A CN 2013101436403A CN 201310143640 A CN201310143640 A CN 201310143640A CN 103330157 A CN103330157 A CN 103330157A
- Authority
- CN
- China
- Prior art keywords
- solution
- precipitate
- jujube
- extract
- red date
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention provides a red date extract extraction method and red date extracts. The method comprises: adding a 60-95% ethanol solution to raw material crushed particles prepared from inferior dried red date, and carrying out microwave extraction; filtering the microwave extracted product to obtain a solution A1 and a precipitate B1; concentrating the solution A1, adding a flocculant, filtering to obtain a solution A2 and a precipitate B2, and concentrating the solution A2 to obtain a date flavonoid extract; dissolving the precipitate B2 with dehydrated alcohol, filtering to remove insoluble substances to obtain a solution A3, and concentrating the solution A3 to obtain a date triterpene extract; adding a solvent to the precipitate B1, carrying out hot extraction, and filtering the hot extracted product to obtain a solution A4 and a precipitate B4; drying the precipitate B4 to obtain a date dietary fiber extract; and carrying out organic solvent impurity removing on the solution A4 to obtain a date polysaccharide extract. According to the present invention, a plurality of red date extracts are respectively subjected to diversion extraction utilization through a process so as to simplify the process and broaden a comprehensive utilization approach of inferior red date.
Description
Technical field
The present invention relates to foods processing technique, relate in particular to a kind of extracting method and extract of red date extract.
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 amino acid that contains needed by human in the jujube fruit.Comprising becoming alanine, threonine, tryptophan, methionine, lysine and the valine that can not synthesize in the human body, and the histidine that must can not synthesize again in children's body, arginine etc.And jujube really is rich in multivitamin, and Vc content is especially high, and Vc content exceeds 1-2 doubly up to 500-800mg than Kiwi berry in the bright jujube of 100g, than the high 7-10 of oranges and tangerines doubly, is 100 times of apple.After fresh date was made dried jujube, vitamin also had higher storage rate, contained Vc15-67mg in the dried jujube of every 100g, carrotene 0.4mg, Cobastab
10.05mg, Cobastab
220.15mg, niacin (nicotinic acid) 1.1mg,, the Vp content in the jujube also is the hat of all kinds of fruits.Also contain abundant mineral element in the jujube fruit, mainly contain nitrogen, phosphorus, potassium, calcium, iron, copper, zinc etc., indispensable mineral element in these human bodies, particularly important with raising intelligence to health treatment for adults and promotion child development.The jujube fruit also has multiple functional component, for example flavonoids, triterpenes, cyclic nucleotide, jujube polysaccharide etc. except having very high nutritive value.
At present from jujube the method for abstraction function composition only at a certain composition wherein, and extraction process complexity.
Summary of the invention
The object of the present invention is to provide a kind of extracting method and extract of red date extract, with the extraction process of simplification red date extract, and realize from red date, extracting multiple extract.
The invention provides a kind of extracting method of red date extract, this method comprises:
With extracting red date stone, fragmentation obtains the raw material particle;
Adding volumetric concentration in described raw material particle is the ethanolic solution of 60%-95%, carries out the microwave lixiviate then; The volumetric concentration of described ethanolic solution is preferably 85%-95%, and more excellent is 90%; The mass ratio of described ethanolic solution and described raw material particle is 10-18:1, is preferably 12-16:1, and 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;
Product after the microwave lixiviate is filtered, obtain solution A 1 and precipitate B 1;
With solution A 1 concentrated, desolventizing, add flocculant again, obtain solution A 2 and precipitate B 2 after the filtration, concentrated solution A2 obtains the jujube flavone extract; Wherein, described flocculant is 1% chitosan solution, and the addition of described flocculant is 0.006g/L;
Precipitate B 2 is used anhydrous alcohol solution, remove by filter insoluble matter and obtain solution A 3, concentrated solution A3 obtains the jujube triterpene extracts;
Add solvent in the precipitate B 1 and heat lixiviate, adjusting the pH value is 8.0-9.2, is preferably 8.6, and heating-up temperature is 75-85 ℃, is preferably 80 ℃, and be 2.5-3.5 hour heat time heating time, is preferably 3 hours; Product after the described heating lixiviate is filtered, obtain solution A 4 and precipitate B 4; Described solvent is water, and the mass ratio of described solvent and precipitate B 1 is 12-18:1, is preferably 15:1;
To obtain insoluble jujube dietary fiber extract after precipitate B 4 oven dry;
After solution A 4 carried out the organic solvent removal of impurities, obtain the jujube polyoses extract.
In the solution of the present invention, described red date is inferior extra dry red wine jujube.
Further, the described process that solution A 4 is carried out the organic solvent removal of impurities comprises: after solution A 4 is concentrated, cools off, add absolute ethyl alcohol; The flocculent deposit filtration that the adding absolute ethyl alcohol is obtained obtains precipitate B 5; With precipitate B 5 oven dry, add water redissolution, add the chloroform layering again after, obtain aqueous layer; With described aqueous layer decolouring, concentrated, oven dry.
Wherein, in the process that solution A 4 is concentrated, described solution A 4 is concentrated into the 1/3-1/5 of original volume; Described absolute ethyl alcohol in the solution A 4 after add concentrating with concentrate after the volume ratio of solution be 3-6:1.
The present invention also provides a kind of extract that is made by the extracting method of red date extract provided by the invention, described extract comprise in the following component any one or multiple: jujube polyoses extract, jujube dietary fiber extract, jujube triterpene extracts and jujube flavone extract.
The extracting method of a kind of red date extract provided by the invention and extract, this method adopts the technology of Microwave Extraction and flocculation separation, by a flow process, multiple compositions such as flavonoids, triterpene compound, jujube polysaccharide and dietary fiber are shunted extraction and application respectively, technological process is simple to operate, with low cost, kept various functional components and the characteristic thereof in the jujube comprehensively.
Moreover because the weather that geography, soil and most of area of China are influenced by the subtropics monsoon is well suited for the growth of jujube tree, China jujube producing region distributes very wide.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.The inventive method can inferior extra dry red wine jujube be that raw material is implemented, and has widened the comprehensive Utilization Ways of inferior jujube.By discovering of the inventor, the jujube polyoses content in the inferior red date and exterior quality best possible merchandise jujube do not have significant difference.
Extracting method of the present invention can make the jujube resource be fully used, and can obtain the various extracts of jujube with higher yield, and simple and convenient extraction is efficient, and cost is low, is particularly suitable for suitability for industrialized production.
Description of drawings
The jujube flavones canonical plotting of Fig. 1 during for quantitative assay of the present invention;
Oleanolic acid canonical plotting when Fig. 2 is quantitative assay of the present invention;
The polysaccharide canonical plotting of Fig. 3 during for quantitative assay of the present invention.
The specific 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 extracting method embodiment one of red date extract provided by the invention can may further comprise the steps:
Step 101, inferior extra dry red wine jujube is cleaned, dry surface moisture, stoning obtains jujube meat, and with the pulp crushing that obtains after the stoning to 0.5mm-1.0mm.
Wherein, the inferior extra dry red wine jujube among the present invention refers to the inferior red date after air-dry, and moisture wherein is generally less than 25%.
The present invention adopts inferior red date as raw material.
Wherein, obtain product (pulp after the fragmentation) in this step and be raw material particle of the present invention.
Step 102, the product that step 101 is obtained are packed in the container, add volumetric concentration and be 90% ethanolic solution; The quality that adds 90% ethanol is 14 times of the product quality that obtains of step 101.
Step 103, the product that step 102 is obtained adopt heating using microwave lixiviate removal of impurities; Wherein, microwave power is 210W; Microwave heating time is 120 seconds.
Step 104, the product that step 103 is obtained filter, and obtain supernatant and precipitation two parts; Wherein the supernatant that obtains of this step is solution A 1 of the present invention, and the precipitation that this step obtains is precipitate B 1 of the present invention.
The step of concrete filtration can for: use earlier gauze coarse filtration, suction filtration again.Through this step, jujube polysaccharide, dietary fiber component are retained in the precipitation, and jujube flavonoids, triterpenes components are present in the supernatant.
Step 105, with supernatant concentration, desolventizing that step 104 obtains, add flocculant again, obtain supernatant and precipitation after the filtration; The supernatant that this step obtains is solution A 2 of the present invention, and the precipitation that this step obtains is precipitate B 2 of the present invention.
Concrete, the supernatant vacuum that step 104 is obtained is concentrated into original volume 1/10, removes ethanol, adds 3 times of volume distilled water then; Add flocculant again, addition is 0.006g/L, and this flocculant for example can 1% chitosan solution, can also be existing other flocculants; Can produce a large amount of precipitations after adding flocculant, this moment, triterpenes components was precipitated, and the jujube flavonoids is present in the supernatant.
Step 106, the supernatant that obtains in the step 105 is concentrated, obtain the jujube flavone extract.
Step 107, the precipitate B 2 that step 105 is obtained are used anhydrous alcohol solution, remove by filter insoluble matter and obtain solution A 3, and concentrated solution A3 obtains the jujube triterpene extracts.
For example: 3 times of volume anhydrous alcohol solutions of precipitate B 2 usefulness that step 105 is obtained, filter, remove insoluble matter, keep solution, and be concentrated into solvent and remove fully, namely make described jujube triterpene extracts.
Add solvent in step 108, the precipitate B 1 that obtains to step 104 and heat lixiviate.
Concrete, the solvent in this step can be water, and the adding quality of solvent is 12 times of precipitate B 1, and adjusting the pH value is 9.2, and heating-up temperature is 85 ℃, be 2.5 hours heat time heating time.
Step 109, the product after the heating lixiviate that obtains in the step 108 is filtered, obtain supernatant and precipitation, obtain insoluble jujube dietary fiber extract after will precipitating oven dry.
The supernatant that this step obtains is solution A 4 of the present invention, and the precipitation that this step obtains is precipitate B 4 of the present invention.At this moment, the jujube polysaccharide is present in the supernatant (ie in solution A4).
Step 110, the supernatant concentration with obtaining in the step 109, cooling; For example with this supernatant concentration to 1/3 of original volume.
Add absolute ethyl alcohol in step 111, the product that obtains to step 110, for example the volume ratio of the product of the absolute ethyl alcohol of Jia Ruing and step 110 can be 6:1; There is flocculent deposit to produce then, filters and obtain precipitate B 5.
Step 112, precipitate B 5 oven dry that step 111 is obtained, add water redissolution; The quality that for example adds water is 10 times of oven dry postprecipitation B5 quality.
Add chloroform in step 113, the product that obtains to step 112, behind the concuss, behind the standing demix except deproteinized, recycle-water solution layer then.
Concrete, the volume that adds chloroform be step 112 obtain the product volume 1/3; The time of concuss is 10 minutes.
Step 114, the aqueous layer that obtains in the step 113 is decoloured, concentrates, dries, obtain the jujube polyoses extract.
Concrete, the step of decolouring for example can for: add the active carbon of 0.1% quality in this aqueous layer, place boiling water bath 10min, and constantly stir, cooled and filtered discards the active carbon filter residue, obtains settled solution.
Embodiment two
Embodiment two is identical with the step of above-described embodiment one, and its difference is, in embodiment two:
The volumetric concentration of the ethanol in the step 102 is 85%, and quality is 12 times of the product quality that obtains of step 101;
In the step 103, microwave power is 280W; Microwave heating time is 100 seconds;
In the step 108, the quality that adds solvent is 18 times of precipitate B 1 quality, adjusts pH value to 8.0, and heating-up temperature is 80 ℃, 3.5 hours heat time heating times;
In the step 110, the product that step 109 is obtained is concentrated into 1/4 of original volume;
In the step 111, add 5 times of volume absolute ethyl alcohols in the product that obtains to step 110;
In the step 112, with the product oven dry that step 111 obtains, redissolve with 12 times of quality water;
In the step 113, the volume that adds chloroform be step 112 obtain the product volume 1/2; The time of concuss is 15 minutes.
Embodiment three
Embodiment three is identical with the step of above-described embodiment one, and its difference is, in embodiment three:
The volumetric concentration of the ethanol in the step 102 is 80%, and quality is 16 times of the product quality that obtains of step 101;
In the step 103, microwave power is 420W; Microwave heating time is 140 seconds;
In the step 108, the quality that adds solvent is 15 times of precipitate B 1 quality, adjusts pH value to 8.8, and heating-up temperature is 83 ℃, 3 hours heat time heating times;
In the step 110, the product that step 109 is obtained is concentrated into 1/5 of original volume;
In the step 111, add 4 times of volume absolute ethyl alcohols in the product that obtains to step 110;
In the step 112, with the product oven dry that step 111 obtains, redissolve with 9 times of quality water;
In the step 113, the volume that adds chloroform be step 112 obtain the product volume 1/4; The time of concuss is 12 minutes.
Embodiment four
Embodiment four is identical with the step of above-described embodiment one, and its difference is, in embodiment four:
The volumetric concentration of the ethanol in the step 102 is 95%, and quality is 15 times of the product quality that obtains of step 101;
In the step 103, microwave power is 140W; Microwave heating time is 110 seconds;
In the step 108, the quality that adds solvent is 16 times of precipitate B 1 quality, adjusts pH value to 8.6, and heating-up temperature is 78 ℃, 2.8 hours heat time heating times;
In the step 110, the product that step 109 is obtained is concentrated into 1/3 of original volume;
In the step 111, add 4.5 times of volume absolute ethyl alcohols in the product that obtains to step 110;
In the step 112, with the product oven dry that step 111 obtains, redissolve with 11 times of quality water;
In the step 113, the volume that adds chloroform be step 112 obtain the product volume 1/4; The time of concuss is 8 minutes.
Embodiment five
Embodiment five is identical with the step of above-described embodiment one, and its difference is, in embodiment five:
The volumetric concentration of the ethanol in the step 102 is 65%, and quality is 13 times of the product quality that obtains of step 101;
In the step 103, microwave power is 300W; Microwave heating time is 130 seconds;
In the step 108, the quality that adds solvent is 14 times of precipitate B 1 quality, adjusts pH value to 8.5, and heating-up temperature is 82 ℃, 3.2 hours heat time heating times;
In the step 110, the product that step 109 is obtained is concentrated into 1/5 of original volume;
In the step 111, add 3.5 times of volume absolute ethyl alcohols in the product that obtains to step 110;
In the step 112, with the product oven dry that step 111 obtains, redissolve with 12 times of quality water;
In the step 113, the volume that adds chloroform be step 112 obtain the product volume 1/2; The time of concuss is 9 minutes.
To the jujube flavone extract that obtains among the embodiment one to embodiment five, the jujube triterpene extracts, jujube dietary fiber extract and jujube polyoses extract detect respectively, the content that records the jujube flavone extract that obtains among the embodiment one to embodiment five is respectively: 2.89mg/g, 2.92mg/g, 3.55mg/g, 2.37mg/g, 3.47mg/g, the content of jujube triterpene extracts is respectively 15.23mg/g, 14.26mg/g, 12.17mg/g, 13.95mg/g and 9.46mg/g, the content of jujube dietary fiber extract is respectively 40.23mg/g, 47.60mg/g, 42.14mg/g, 43.26mg/g, 44.57mg/g the content of jujube polyoses extract is respectively 128.8mg/g, 130.1mg/g, 129.6mg/g, 129.2mg/g and 127.9mg/g.Wherein, above-mentioned content is all based on the gross weight of inferior extra dry red wine jujube.
The various extracts that the present invention is extracted detect below.
(1) the present invention adopts colorimetric method to identify the jujube flavone extract, and this method is as follows:
A. the drafting of jujube flavones calibration curve:
Take by weighing flavones (rutin standard items) 0.0114g, add a small amount of 60% ethanol, low-grade fever makes the standard items dissolving, is settled to 250mL with ethanol then, shakes up, and leaves standstill 5min, obtains the rutin titer.The rutin titer for preparing is got 0,1.0,2.0,3.0,4.0,5.0,6.0mL respectively in the 25mL volumetric flask, number 0-6, and mend to 6mL with distilled water, respectively add 5%NaNO then
21mL shakes up, and leaves standstill 6min, adds 10%Al (NO again
3)
3Solution 1mL shakes up, and leaves standstill 6min, adds 10%NaOH10mL again, and behind the 15min, constant volume shakes up, and leaves standstill.Make reference with No. 0, measure absorbance in the 500nm place, the drawing standard curve is seen Fig. 1.The jujube flavones canonical plotting of Fig. 1 during for quantitative assay of the present invention.
B. jujube flavone extract sample determination:
Press the assay method that jujube flavones calibration curve is drawn, testing sample (the jujube flavone extract that the embodiment of the invention one to embodiment five is extracted) is dissolved in a small amount of 60% ethanol respectively, be settled to 250mL with 60% ethanol then, shake up and make sample solution, get each sample solution 3mL respectively in the 25mL volumetric flask, mend to 6mL respectively and with distilled water, respectively add 5%NaNO then
21mL shakes up, and leaves standstill 6min, adds 10%Al (NO again
3)
3Solution 1mL shakes up, and leaves standstill 6min, adds 10%NaOH10mL again, behind the 15min, constant volume shakes up, leave standstill, No. 0 during with drafting jujube flavones calibration curve usefulness 1cm cuvette is measured embodiment one to embodiment five each sample solution absorbency values under 500nm as reference.The regression equation of gained absorbance substitution calibration curve, the content of calculating jujube flavone extract.According to said method, the content that records the jujube flavone extract that obtains among the embodiment one to embodiment five is respectively 2.89mg/g, 2.92mg/g, 3.55mg/g, 2.37mg/g, 3.47mg/g.
(2) the present invention adopts colorimetric method to identify the jujube triterpene extracts, and this method is as follows:
The drafting of A, triterpene substance calibration curve
Because the triterpene substance in the red date is mainly oleanolic acid, so generally, those skilled in the art represent the content of triterpene substance in the red date by the content of determining oleanolic acid in the red date.
Accurately take by weighing oleanolic acid standard items 0.0116g, add a small amount of absolute ethyl alcohol and make the standard items dissolving, be settled to 100mL with absolute ethyl alcohol then, shake up, leave standstill 5min, make the oleanolic acid titer.Get 0,0.1,0.2 respectively, 0.3,0.4,0.5,0.6mL the oleanolic acid titer is in the 10mL test tube, numbering 0-6 behind the dried solvent of heated volatile, adds 5mL distilled water concussion mixing respectively in above-mentioned 0-6 test tube, centrifugal 5 minutes at 10000 rev/mins then, after the abandoning supernatant, in above-mentioned 0-6 test tube, add 5% vanillic aldehyde-glacial acetic acid solution 0.3mL, perchloric acid 0.7mL respectively, 65 ℃ of water-bath 15min, take out flowing water immediately and be cooled to room temperature, in above-mentioned 0-6 test tube, add 4mL ethyl acetate respectively again, shake up, make reference with No. 0, measure absorbance at the 550nm place, the drawing standard curve is seen Fig. 2.The oleanolic acid canonical plotting of Fig. 2 during for quantitative assay of the present invention.
B, sample determination:
Assay method by the calibration curve drafting: testing sample (the jujube triterpene extracts that the embodiment of the invention one to embodiment five is extracted) is dissolved in a small amount of absolute ethyl alcohol respectively, be settled to 100mL with absolute ethyl alcohol then, shake up and make sample solution, get each sample solution 0.1mL of embodiment one to embodiment five respectively in the 10mL test tube, behind the dried solvent of heated volatile, add 5% vanillic aldehyde-glacial acetic acid solution 0.3mL respectively, perchloric acid 0.7mL, 65 ℃ of water-bath 15min, take out flowing water immediately and be cooled to room temperature, add 4mL ethyl acetate more respectively, shake up, measure embodiment one to embodiment five each sample solution absorbency values as reference at the 550nm place No. 0 during with drafting triterpene substance calibration curve.The regression equation of gained absorbance substitution calibration curve, the content of calculating jujube triterpene extracts.The content that records the jujube triterpene extracts that obtains among the embodiment one to embodiment five is respectively 15.23mg/g, 14.26mg/g, 12.17mg/g, 13.95mg/g and 9.46mg/g.
(3) method of the content of evaluation jujube dietary fiber extract:
Because red date is mainly by water, carbohydrate, protein, fat four big materials are formed, by the extraction step to red date before, the aqueous solution and ethanolic solution and chloroform have been removed soluble saccharide, protein, fat, and baking step has been removed moisture, so surplus materials is jujube dietary fiber extract, be mainly non-water-soluble jujube dietary fiber.Can obtain so directly obtain insoluble material after 4 oven dry of weighing precipitate B, the content that records insoluble jujube dietary fiber extract in the red date that embodiment one to embodiment five obtains is respectively 40.23mg/g, 47.60mg/g, 42.14mg/g, 43.26mg/g, 44.57mg/g
(4) detection method to the jujube polyoses extract 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 bar mixing.
(2) get two clean white plaques, add an amount of testing sample and an amount of amylose respectively, add 2-3 more respectively and drip iodine liquid, observe change color.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 alpha-Naphthol with balance and be dissolved to 10mL with 95% ethanol that configures, face with preceding preparation standby.
(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 concentrated sulfuric acid 2.75mL with liquid-transfering gun along tube wall, can not jolting.Sulfuric acid layer is sunken to test tube bottom and sugar juice 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 bath water-bath 5 minutes.Observe change color.
Experimental result: glucose solution produces brick-red precipitation with expense beautiful jade reagent reacting, and sample sets does not have brick-red precipitation, and produces Gu (OH)
2Blue precipitation is not so detect monose in the sample.
The detection of A4, protein
(1) preparation of ninhydrin reagent: balance takes by weighing the 0.10g ninhydrin, 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 bath 5 minutes, and change color 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 the polysaccharose substance of not starch-containing, monosaccharide and protein.
B, employing phenol sulfuric acid process quantitatively detect the jujube polysaccharide that extracts
B1, polysaccharide calibration curve are drawn:
Glucose standard liquid: get 0.2038g glucose and in the 100mL volumetric flask, use the distilled water constant volume, get 0,1.0,2.0,3.0,4.0,5.0mL constant volume in the 100mL volumetric flask more respectively, be made into standard liquid.
The 50mL concentrated sulfuric acid 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 standard liquid 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 absorbance.
The calibration curve of gained polysaccharide as shown in Figure 3, the polysaccharide canonical plotting of Fig. 3 during for quantitative assay of the present invention.
B2, sample determination:
The jujube polyoses extract that embodiment one to embodiment five is made, getting 1g respectively is dissolved in the 10ml distilled water, dilute 250 times then and make sample solution, method in drawing according to above-mentioned calibration curve is measured the content of jujube polyoses extract in each sample solution, and the content of the jujube polyoses extract that obtains among the embodiment one to embodiment five that records is respectively 128.8mg/g, 130.1mg/g, 129.6mg/g, 129.2mg/g and 127.9mg/g.
Extracting method provided by the invention, adopt the technology of Microwave Extraction and flocculation separation, by a flow process, multiple compositions such as flavonoids, triterpene compound, jujube polysaccharide and dietary fiber are shunted extraction and application respectively, technological process is simple to operate, with low cost, kept the functional characteristic of various functional components; 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 jujube.Thus, the extracting method that the present invention adopts, raw material is easy to get, product yield height, the manufacturing process simple and effective, cost is low, is fit to suitability for industrialized production.
The red date extract that the present invention also provides extracting method according to the present invention to make, this red date extract comprise following any one or multiple: jujube flavone extract, jujube triterpene extracts, jujube dietary fiber extract and jujube polyoses extract.
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 puts 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. the extracting method of a red date extract is characterized in that, comprising:
With extracting red date stone, fragmentation obtains the raw material particle;
Adding volumetric concentration in described raw material particle is the ethanolic solution of 60%-95%, carries out the microwave lixiviate then; The mass ratio of described ethanolic solution and described raw material particle is 10-18:1, and microwave power is 70 watts-490 watts, and microwave heating time is 90 seconds-150 seconds;
Product after the microwave lixiviate is filtered, obtain solution A 1 and precipitate B 1;
With solution A 1 concentrated, desolventizing, add flocculant again, obtain solution A 2 and precipitate B 2 after the filtration, concentrated solution A2 obtains the jujube flavone extract;
Precipitate B 2 is used anhydrous alcohol solution, remove by filter insoluble matter and obtain solution A 3, concentrated solution A3 obtains the jujube triterpene extracts;
Add solvent in the precipitate B 1 and heat lixiviate, adjusting the pH value is 8.0-9.2, and heating-up temperature is 75-85 ℃, and be 2.5-3.5 hour heat time heating time; Product after the described heating lixiviate is filtered, obtain solution A 4 and precipitate B 4; Described solvent is water, and the mass ratio of described solvent and precipitate B 1 is 12-18:1;
To obtain insoluble jujube dietary fiber extract after precipitate B 4 oven dry;
After solution A 4 carried out the organic solvent removal of impurities, obtain the jujube polyoses extract.
2. method according to claim 1 is characterized in that, the mass ratio of described ethanolic solution and described raw material particle is 12-16:1.
3. method according to claim 1 is characterized in that, described microwave power is 140 watts-420 watts.
4. method according to claim 1 is characterized in that, described microwave heating time is 100 seconds-140 seconds.
5. method according to claim 1, it is characterized in that: described flocculant is 1% chitosan solution, the addition of described flocculant is 0.006g/L.
6. method according to claim 1 is characterized in that: add solvent in the precipitate B 1 and heat in the process of lixiviate described, adjusting the pH value is 8.6.
7. method according to claim 1 is characterized in that: add solvent in the precipitate B 1 and heat in the process of lixiviate described, the mass ratio of described solvent and precipitate B 1 is 15:1.
8. method according to claim 1 is characterized in that: add solvent in the precipitate B 1 and heat in the process of lixiviate described, heating-up temperature is 80 ℃, and be 3 hours heat time heating time.
9. according to the arbitrary described method of claim 1-8, it is characterized in that the described process that solution A 4 is carried out the organic solvent removal of impurities comprises:
Solution A 4 is concentrated, after the cooling, adds absolute ethyl alcohol;
The flocculent deposit filtration that the adding absolute ethyl alcohol is obtained obtains precipitate B 5;
With precipitate B 5 oven dry, add water redissolution, add the chloroform layering again after, obtain aqueous layer;
With described aqueous layer decolouring, concentrated, oven dry.
10. a red date extract makes according to the arbitrary described method of claim 1-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101436403A CN103330157A (en) | 2013-04-23 | 2013-04-23 | Red date extract extraction method and red date extracts |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101436403A CN103330157A (en) | 2013-04-23 | 2013-04-23 | Red date extract extraction method and red date extracts |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103330157A true CN103330157A (en) | 2013-10-02 |
Family
ID=49238417
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013101436403A Pending CN103330157A (en) | 2013-04-23 | 2013-04-23 | Red date extract extraction method and red date extracts |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103330157A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106109620A (en) * | 2016-07-14 | 2016-11-16 | 塔里木大学 | A kind of deep working method of Fructus Jujubae processing waste |
| CN106376912A (en) * | 2016-08-31 | 2017-02-08 | 恒枫食品科技有限公司 | Preparation method for red date extract |
| CN110760011A (en) * | 2019-08-05 | 2020-02-07 | 浙江李子园食品股份有限公司 | Method for separating and purifying red date polysaccharide from plants |
| CN112915126A (en) * | 2021-03-04 | 2021-06-08 | 长治医学院 | Method for extracting red date flavonoid compound |
| CN114521651A (en) * | 2022-02-21 | 2022-05-24 | 沧州恩际生物制品有限公司 | New red date extracting solution extracted by red date extraction process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101288468A (en) * | 2008-05-23 | 2008-10-22 | 山西省农业科学院农产品综合利用研究所 | Method of sequential extraction of biological activity component from jujube |
| CN102079773A (en) * | 2010-12-24 | 2011-06-01 | 申琳 | Oleanolic acid and method for preparing oleanolic acid by utilizing red dates |
| CN102086237A (en) * | 2010-12-24 | 2011-06-08 | 申琳 | Method for preparing jujube polysaccharide from red dates and jujube polysaccharide |
| CN102090635A (en) * | 2010-12-24 | 2011-06-15 | 申琳 | Method for preparing data flavone from red dates and data flavone |
-
2013
- 2013-04-23 CN CN2013101436403A patent/CN103330157A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101288468A (en) * | 2008-05-23 | 2008-10-22 | 山西省农业科学院农产品综合利用研究所 | Method of sequential extraction of biological activity component from jujube |
| CN102079773A (en) * | 2010-12-24 | 2011-06-01 | 申琳 | Oleanolic acid and method for preparing oleanolic acid by utilizing red dates |
| CN102086237A (en) * | 2010-12-24 | 2011-06-08 | 申琳 | Method for preparing jujube polysaccharide from red dates and jujube polysaccharide |
| CN102090635A (en) * | 2010-12-24 | 2011-06-15 | 申琳 | Method for preparing data flavone from red dates and data flavone |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106109620A (en) * | 2016-07-14 | 2016-11-16 | 塔里木大学 | A kind of deep working method of Fructus Jujubae processing waste |
| CN106376912A (en) * | 2016-08-31 | 2017-02-08 | 恒枫食品科技有限公司 | Preparation method for red date extract |
| CN110760011A (en) * | 2019-08-05 | 2020-02-07 | 浙江李子园食品股份有限公司 | Method for separating and purifying red date polysaccharide from plants |
| CN112915126A (en) * | 2021-03-04 | 2021-06-08 | 长治医学院 | Method for extracting red date flavonoid compound |
| CN114521651A (en) * | 2022-02-21 | 2022-05-24 | 沧州恩际生物制品有限公司 | New red date extracting solution extracted by red date extraction process |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103330157A (en) | Red date extract extraction method and red date extracts | |
| CN107969532B (en) | Fructus momordicae flavored instant drink and preparation method thereof | |
| CN103549562B (en) | Instant ginger decoction powder and instant ginger decoction | |
| CN104152521A (en) | Paeonia suffruticosa pollen protein polypeptide and preparation method and application thereof | |
| CN102295709B (en) | Ganoderma lucidum polysaccharide with light color and high molecular weight, and preparation method thereof | |
| CN101715993B (en) | Method for preparing lotus root juice drink from whole lotus root starch | |
| CN104095176B (en) | A kind of defecation method of honey | |
| CN112010989B (en) | Preparation method of dictyophora phalloidea mycelium polysaccharide with antioxidant activity | |
| CN108813615B (en) | Preparation method of mung bean extract with antioxidant activity | |
| CN108794651A (en) | The method that pectin is extracted in passion fruit pericarp | |
| CN111423524B (en) | Method for extracting lotus leaf polysaccharide | |
| CN113875981B (en) | Instant powder of herba Eupatorii and its preparation method | |
| CN104522604A (en) | Dried orange peel soup for Guiling jelly or beverage and preparation technology thereof | |
| CN104387490A (en) | Method for preparing non-araboxylan polysaccharides from plantain seed | |
| CN102352119A (en) | Method for preparing natural edible coloring agent | |
| CN112694541B (en) | Mild decoloring method for abelmoschus manihot polysaccharide | |
| CN106699908A (en) | Method for extracting amylose from high amylose corn starch | |
| CN107712170A (en) | A kind of preparation method and applications of soluble dietary fiber | |
| CN105859916B (en) | A kind of preparation method of south No. 9 jerusalem artichoke inulins of jerusalem artichoke | |
| CN102090635A (en) | Method for preparing data flavone from red dates and data flavone | |
| CN103549084A (en) | Houttuynia extract and method for preparing herbal tea and effervescent tablets from houttuynia extract | |
| CN112442136A (en) | Method for extracting functional components from tremella | |
| CN105566512A (en) | Extracting method of persimmon fruit pectin | |
| CN105294873A (en) | Extraction method for laminarin | |
| CN102086237A (en) | Method for preparing jujube polysaccharide from red dates and jujube polysaccharide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20131002 |