CN109608562A - A method of pectin being extracted from sunflower blueness disk using salt - Google Patents
A method of pectin being extracted from sunflower blueness disk using salt Download PDFInfo
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- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
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Abstract
The invention belongs to pectous extracting method technical fields, provide a kind of method for extracting pectin from sunflower blueness disk using salt.Using sunflower blueness disk as raw material, enzyme deactivation in thermostat water bath, filtering discards enzyme deactivation liquid；Distilled water is added in precipitating, ammonium oxalate is added or sodium citrate extracts, filters, filtrate decompression rotary distillation, concentration, the sunflower plate extracting solution being concentrated；Concentrate is precipitated with ethyl alcohol, is obtained by filtration pectin after standing, and gained pectin washs 1-2 dehydration with dehydrated alcohol, crosses 60 meshes, and naturally dry or 40 DEG C or less are dried, and crushes to obtain pectin powder.The method of the present invention pectin extraction rate is high；Product appearance is good, is not necessarily to decolorization；Solid-liquid ratio is small, substantially reduces the dosage of solvent and salt；The utilization rate of sunflower plate is effectively improved, realizes waste utilization, increases the added value of sunflower industry.
Description
Technical field
The invention belongs to pectous extracting method technical fields, and in particular to a kind of to extract fruit from sunflower blueness disk using salt
The method of glue.
Background technique
China's sunflower planting area is extensive, and sunflower plate is largely discarded, and environmental pollution and the wasting of resources are caused.Sunflower
Pectin of the disk containing 15-25%, it is resourceful, it is cheap and easy to get.Therefore Devoting Major Efforts To Developing China sunflower plate resource abundant, improves it
Utilization rate has certain social and economic implications.Sunflower pectin is with unique molecular structure, bioactivity and functionality
Natural polymer, discovery so far be always chemical industry, pharmacy and field of food research hotspot.A large amount of research work is dedicated to
Improving quality and raising yield, but the pectin of nearly 20-30% is inevitably degraded and is lost in decolorization.
Pectin is a kind of preferable polysaccharide of gelling, mainly by galacturonic acid with α -1-4 glucosides key connection, rich in polyhydroxy
Food, medicine and chemical industry every field is widely applied in base and carboxyl.The main and most basic structural unit of pectin such as Fig. 1 institute
The chemical structural formula shown also has the difference of fine structure because of the difference of pectin starting material, the difference of extraction process, but all answers
It is all this structural unit with type pectin, wherein there are three the structures that structural factor influences pectin, to influence its performance and answer
With field: the size of 1.n, that is, how many repetitive unit in the structure of pectin product, n is bigger, and the molecular weight of pectin is bigger,
It is provided with macromolecular property.The pectin of different range n value has different physicochemical properties, and application performance and range also accordingly change
Become.So the molecular weight of pectin and its distribution are the important characterization parameters of pectin, physicochemical property, the application of pectin decide
Matter and application field.2. ester group-COOCH3With content of the carboxy CO OH in pectin, pectin is certain, total ester group and carboxyl amount
Centainly.Ester group content is high-ester pectin higher than 50%, and under conditions of Controlled acidity and pol, gel easy to form is applied to
Every field.But must there are sucrose and strict control pH value at gel, there is the high-ester pectin measuring method of GB standard.When ester group contains
Amount is lower than 50%, is exactly low-ester pectin, and low-ester pectin has entirely different gelation mechanism, and low-ester pectin forms gel and do not depend on
The presence of sucrose, does not depend on solution acidity, it is only necessary to the presence of metal ion and certain molecular weight, so low-ester pectin is low
The good additive of sugared low-calorie diet.But the low-ester pectin of naturally occurring is less, and presently mainly high-ester pectin passes through drop ester
Technique obtains.But sunflower pectin is the source of natural low-ester pectin.Acid system and salt method can obtain molecular weight distribution not
Same low-ester pectin, is applied, has a extensive future.3. ester group-COOCH in pectin3With distribution side of the carboxy CO OH in pectin
Formula also influences pectin performance.
According to esterification degree difference, pectin is divided into low fat and two class high in fat, and esterification degree influences its application field and condition.Xiang
Certain herbaceous plants with big flowers disk is one of the important sources for extracting low-fat pectin, and sunflower dry pan is the unique raw material of current pectin extraction, after crushing not
It extracts to obtain pectin with technique.Salt formulation is also applied to the extraction of dry pan pectin, but gained slightly mention pectin color be dark-brown or
Brown, it is necessary to decolourize.It will affect pectin quality, reduce pectin extraction rate.
Sunflower dry pan is carried out drying by fresh sunflower plate or is obtained after drying for a long time, holds in natural drying process
Easily mouldy, dry that brown stain occurs, disk brown color, dark cellulose content is high, and a large amount of pigments introduce pectin in extraction, influences fruit
The color and sense organ of glue.So must all have decoloration process by the pectin extraction of raw material of sunflower dry pan.Currently, dry pan to
The salt extraction process of day certain herbaceous plants with big flowers pectin, solid-liquid ratio are greater than 1:30, and water consumption is larger.It is greater than 0.5% using salinity, organic salt is with material
Liquor ratio increases accordingly, the liquid handlings heavy workload such as filtering, alcohol precipitation.
Summary of the invention
The present invention for the defects of sunflower plate pectin extraction at this stage, provide it is a kind of using salt from sunflower blueness disk
The middle method for extracting pectin.
The present invention is realized by following technical solution: a method of pectin being extracted from sunflower blueness disk using salt, with
Sunflower blueness disk is raw material, and enzyme deactivation 15-22min in >=95 DEG C of thermostat water baths filters, discards enzyme deactivation liquid；With feed liquid in precipitating
Than distilled water is added for 1:5-15, solid oxalic acid ammonium or sodium citrate is added, controls reaction system mesoxalic acid ammonium or sodium citrate
Concentration extracted for 0.2-1.0%, Extracting temperature be 80-90 DEG C, extraction time 20-60min；Filtering, filtrate decompression rotation
Turn distillation, is concentrated into 0.3-0.5 times of original solution volume, the sunflower plate extracting solution being concentrated；Concentrate is carried out with ethyl alcohol
Precipitating, is obtained by filtration pectin after standing, and gained pectin wash 1-2 dehydration sieving with dehydrated alcohol, naturally dry or 40 DEG C with
Lower drying, crushes to obtain pectin powder.
The de- fresh sunflower plate of seed several times with clear water rinsing removes silt, dust, drains, be cut into the block of 0.8-1.5cm；
The water content of the fresh sunflower plate is 80-90%.It is preferred that: the de- fresh sunflower plate of seed several times with clear water rinsing removes mud
Husky, dust, drains, is cut into the block of 1.0cm.
It is filtered after enzyme deactivation with 150-300 mesh nylon cloth；300-500 mesh nylon cloth filters after alcohol precipitation is stood；60 are crossed after dehydration
Mesh.It is filtered at >=70 DEG C after the completion of extraction.The temperature of the vacuum distillation is 60-70 DEG C.Used in ethanol precipitation
The ethyl alcohol that concentration of alcohol is 90% or more, dosage are 1-3 times of the volume of the concentrated liquid, and alcohol precipitation sequence is that extracting solution imports in ethyl alcohol, alcohol
The heavy time is 20-24h.The esterification degree 20 ~ 34% of pectin obtained, 500 KD-100 KD of molecular weight ranges.
The water on the sunflower plate surface of cleaning is drained, combination water and the Free water variation of sunflower are little.Green disk is unable to powder
It is broken, it will affect and filter in next step, green disk block diameter influences recovery rate.The filtration temperature is not less than 70 DEG C, is lower than 70 DEG C, extracts
Liquid retrogradation, sad filter, loss are big.It is 9.2 ~ 36.7% that 1.2 ~ 11.0%(of recovery rate of the pectin, which is converted into dry pan recovery rate),
Color is white or light yellow.
Blueness disk selection of the invention is without rotten, no brown stain.The color of green disk is also related to the color of product.Green disk contains naturally
Water is not less than 80%, and during the dry dehydration of green disk, one side pectin has apparent structure change, another aspect pectin
Color can deepen.Early period lot of experiment validation, green disk natural moisture content is higher, and the extraction process of pectin is more stable, product color
Pool and yield can guarantee.
Green disk stripping and slicing, simple process.From principle is extracted, raw material particle size is smaller, and easier and solvent contact, extraction is got over
It is easy to carry out.But green disk water content is big, after crushing, color can brown stain quickly, color burn.And crush easily at pureed, it is unfavorable for
The operations such as subsequent filtering.Partial size, which is greater than 1.5cm, also can be obtained product, but yield can increase with partial size and be reduced, and partial size is very little
It is not easy to filter, influences enzyme deactivation and subsequent technique.In salt technique, the dissolution of green disk is worse than sour technique, so in order to guarantee to extract
Rate, and subsequent workshop section is taken into account, partial size 0.8-1.5cm is controlled, is most preferably 1cm.Green disk is harder and enzymatic activity therein is higher, and goes out
The process of enzyme is also the process for allowing the shell of block stock and cavernous body to shrink.So enzyme-removal temperature is 95 DEG C or more, the time is
15-30 min, partial size are reduced, and the enzyme deactivation time is reduced.
For salt technique, ammonium oxalate and sodium citrate are all applied to sunflower pectin extraction, and it is also that pectin is most classical that salt, which mentions,
With traditional method.Two kinds of salt all individually can be used for extracting pectin, and it is available to day to control solid-liquid ratio, temperature and time
Certain herbaceous plants with big flowers pectin.Existing extracting method, best solid-liquid ratio is between 1:40-1:50, and Extracting temperature is higher than 90 DEG C, and the dosage of salt is with dense
Degree calculates.But technique before is all only to measure the recovery rate of pectin, obtains the crude product of pectin, has not focused on the color of pectin
Whether structure substantially stationary pectin is obtained under pool and process conditions used, and fixed structure just secures application range.This salt
It mentions in technique, solid-liquid ratio is up to original 30%, and water consumption significantly reduces.Salinity is controlled, water consumption reduces, then salt
Dosage significantly reduces.Extracting temperature is 80-90 DEG C, most preferably 85 DEG C；Extraction time is 20-60 min, most preferably 45min；Temperature
Degree increases, and the time lengthens, and the influence to yield is not significant, but pectin color is deepened.
Salt of the present invention mentions under process conditions, and conceivable is that molecular weight is big, avoids degradation chain rupture as far as possible
Pectin, while guaranteeing in process conditions the color of pectin as far as possible.This part high molecular pectin has centainly in acid condition
Thickening and gelling, so extract terminate, feed liquid separate when, it is necessary to strict control separation temperature.Temperature is lower than 70 degree, liquid
Obvious retrogradation, pectin gelling, is unfavorable for separating, the peculiar physicochemical property of the larger pectin of this molecular weight in extracting solution.
Step is concentrated under reduced pressure, the control of temperature is the color to guarantee pectin.Temperature is higher, and thickening efficiency is higher, but mentions
Take liquid color that can significantly deepen.The viscosity that salt mentions pectin solution mentions pectin solution lower than acid, and mobility is more preferable.So concentration
Multiple is controlled in 0.3-0.5, is conducive to subsequent alcohol precipitation, save the cost.
In the step of alcohol precipitation, it is necessary to be that will be cooled to room temperature concentrate below to be slowly added into 90-95% ethyl alcohol, add
Sample sequence cannot change.In alcohol precipitation step, concentrate temperature is high, is added in ethyl alcohol, and effect is unobvious, is unfavorable for pectin precipitation.
So concentrate is at least cooled to room temperature.If ethyl alcohol is added in extracting solution, the pectin being precipitated is at vermicelli shape, Er Qieshi
Part is precipitated, and alcohol precipitation is ineffective.So Loading sequence wants strict control when alcohol precipitation.According to alcohol precipitation principle, ethyl alcohol and extracting solution
Alcohol precipitation fixing fabric structure when, ethanol consumption is bigger to be conducive to the pectin that macromolecular is precipitated.This technique optimum amount is 1.2-1.6 times
Ethyl alcohol.The selection of drying condition is in order to avoid pectin color burn.
The pectin product of the above physicochemical property, gelling are slightly poor.Soft gel can be formed in gelatinization, can be used for making
Standby medicinal colloidal bismuth pectin.It can also be used for hypoglycemic, reducing blood lipid, can be also used for releasing lead poisoning, Medicament for Alcoholism, the health cares such as meal replacement powder
Product.In short, this products application is in the field not being strict with to pectin gelling.
Compared with existing sunflower plate pectin extraction technology, operation of the present invention is simple, and experimental procedure is few, without at decoloration
Reason, pectin extraction rate is high, and purity is high, appearance is good, extracts pectin using fresh sunflower blueness disk, and pectin yield is high, and solid-liquid ratio is small,
It is at low cost, it is readily produced industrialization.
Fresh sunflower plate water content is high, significantly reduces the solid-liquid ratio of extraction process, reduces the dosage of salt.Work is proposed with salt
Skill extracts pectin from fresh sunflower plate, directly obtains white or light yellow sunflower plate pectin product.Fresh sunflower is green
Disk water content is up to 70 ~ 90%, can reduce extraction solid-liquid ratio, effectively saves the dosage of water and salt, reduces energy consumption.It is of the invention former
Expect that utilization rate is high, production cost is low, be easy to industrialize, post-processing is simple, safe and simple sunflower plate pectin extraction method.
Detailed description of the invention
Fig. 1 is the main and most basic structural unit of pectin；Fig. 2 is that the sunflower pectin of green disk ammonium oxalate technique is infrared
Spectrogram；Fig. 3 is the sunflower pectin infrared spectrogram of green disk sodium citrate technique；Fig. 4 is the gel chromatography of sunflower pectin
Figure；Fig. 5 is the pectin that dry pan degree of gelation is 90-95；Fig. 6 is the green disk pectin that degree of gelation is 95-100.
Specific embodiment
Combined with specific embodiments below, claim of the invention is described further, but is not limited to these implementations
Example.
Embodiment 1: a method of pectin being extracted from sunflower blueness disk using salt, comprising the following steps:
Step (1): choosing the de- fresh sunflower plate of seed, several times with clear water rinsing, removes silt, dust, drains, it is described it is fresh to
The water content of day certain herbaceous plants with big flowers disk is 80-90%；
Step (2): green disk stripping and slicing, block diameter are 0.8cm；
Step (3): blocky sunflower blueness disk is put into 95 DEG C or more enzyme deactivation 15min in thermostat water bath, with 150 mesh nylon cloth mistakes
Filter, filter cake are spare；
Step (4): using gained filter cake in step (3) as raw material is extracted, being added distilled water by solid-liquid ratio 1:15, and concentration, which is added, is
0.3% ammonium oxalate carries out pectin extraction to raw material, extracts 60min at 80 DEG C；
Step (5): filtering, slag-liquid separation collect filtrate；
Step (6): by gained 70 DEG C of decompression rotary distillations of filtrate in step (5), it is concentrated into 0.5 times of original solution volume, is obtained
The sunflower plate extracting solution of concentration；
Step (7): the ethyl alcohol for being 90% or more by concentrate concentration obtained in step (6), dosage are the 1- of the volume of the concentrated liquid
3 times of progress alcohol precipitations, alcohol precipitation sequence are that extracting solution imports in ethyl alcohol, and the alcohol precipitation time is for 24 hours.Fruit is obtained by filtration with 500 mesh nylon cloths
Gained pectin is washed 3 dehydrations with dehydrated alcohol, crosses 60 meshes by glue, and 40 DEG C or less drying crush to obtain pectin powder.
Embodiment 2: a method of pectin being extracted from sunflower blueness disk using salt, comprising the following steps: green disk is cut into
The block of 1.0cm；Blocky sunflower blueness disk is put into 95 DEG C or more enzyme deactivation 18min in thermostat water bath, is filtered with 200 mesh nylon cloths,
Filter cake is spare；Distilled water is added as raw material is extracted, by solid-liquid ratio 1:5 in filter cake, and the ammonium oxalate that concentration is 0.2% is added to raw material
Pectin extraction is carried out, extracts 45min at 85 DEG C；Filtering, 60 DEG C of decompression rotary distillations of filtrate are concentrated into the 0.3 of original solution volume
Times, the sunflower plate extracting solution being concentrated；The ethyl alcohol for being 90%-95% with concentration, dosage are 1.2-1.6 times of the volume of the concentrated liquid
Alcohol precipitation is carried out, alcohol precipitation sequence is that extracting solution imports in ethyl alcohol, and the alcohol precipitation time is 22h.Pectin is obtained by filtration with 300 mesh nylon cloths,
Gained pectin is washed into 2 dehydrations with dehydrated alcohol, crosses 60 meshes, naturally dry crushes to obtain pectin powder.Remaining method is the same as real
Apply 1 the method for example.
Embodiment 3: a method of pectin being extracted from sunflower blueness disk using salt, comprising the following steps: green disk is cut into
The block of 1.5cm；Blocky sunflower blueness disk is put into 95 DEG C or more enzyme deactivation 22min in thermostat water bath, is filtered with 300 mesh nylon cloths,
Filter cake is spare；Distilled water is added as raw material is extracted, by solid-liquid ratio 1:10 in filter cake, and the sodium citrate that concentration is 0.8% is added to original
Material carries out pectin extraction, extracts 20min at 90 DEG C；Filtering, 65 DEG C of decompression rotary distillations of filtrate are concentrated into original solution volume
0.4 times, the sunflower plate extracting solution being concentrated；The ethyl alcohol for being 90%-95% with concentration, dosage be 2 times of the volume of the concentrated liquid into
Row alcohol precipitation, alcohol precipitation sequence are that extracting solution imports in ethyl alcohol, and the alcohol precipitation time is 20h.Pectin is obtained by filtration with 400 mesh nylon cloths, it will
Gained pectin washs 1 dehydration with dehydrated alcohol, crosses 60 meshes, and naturally dry crushes to obtain pectin powder.Remaining method is the same as implementation
1 the method for example.
Embodiment 4: a method of pectin being extracted from sunflower blueness disk using salt, comprising the following steps: green disk is cut into
The block of 1.3cm；Blocky sunflower blueness disk is put into 95 DEG C or more enzyme deactivation 22min in thermostat water bath, is filtered with 200 mesh nylon cloths,
Filter cake is spare；Distilled water is added as raw material is extracted, by solid-liquid ratio 1:10 in filter cake, and the sodium citrate that concentration is 1.0% is added to original
Material carries out pectin extraction, extracts 60min at 83 DEG C；Filtering, 68 DEG C of decompression rotary distillations of filtrate are concentrated into original solution volume
0.4 times, the sunflower plate extracting solution being concentrated；The ethyl alcohol for being 90%-95% with concentration, dosage are 2.5 times of the volume of the concentrated liquid
Alcohol precipitation is carried out, alcohol precipitation sequence is that extracting solution imports in ethyl alcohol, and the alcohol precipitation time is 23h.Pectin is obtained by filtration with 500 mesh nylon cloths,
Gained pectin is washed into 3 dehydrations with dehydrated alcohol, crosses 60 meshes, 40 DEG C or less drying crush to obtain pectin powder.Remaining method
With 1 the method for embodiment.
Embodiment 5: a method of pectin being extracted from sunflower blueness disk using salt, comprising the following steps: green disk is cut into
The block of 1.1cm；Blocky sunflower blueness disk is put into 95 DEG C or more enzyme deactivation 22min in thermostat water bath, is filtered with 200 mesh nylon cloths,
Filter cake is spare；Distilled water is added as raw material is extracted, by solid-liquid ratio 1:5 in filter cake, and the sodium citrate that concentration is 0.7% is added to original
Material carries out pectin extraction, extracts 50min at 87 DEG C；Filtering, 70 DEG C of decompression rotary distillations of filtrate are concentrated into original solution volume
0.5 times, the sunflower plate extracting solution being concentrated；The ethyl alcohol for being 97% with concentration, dosage are that the isometric ethyl alcohol of concentrate carries out
Alcohol precipitation, alcohol precipitation sequence are that extracting solution imports in ethyl alcohol, and the alcohol precipitation time is 20h.Pectin is obtained by filtration with 300 mesh nylon cloths, by institute
It obtains pectin and washs 3 dehydrations with dehydrated alcohol, cross 60 meshes, 40 DEG C or less drying crush to obtain pectin powder.Remaining method is the same as real
Apply 1 the method for example.
Experimental example: pectin prepared by green disk ammonium oxalate technique carries out infrared detection, and infrared spectrum is shown in Fig. 2, produces in pectin
In the infrared spectrum of product, in 1000-3500 cm-1Absorption region in the due whole characteristic absorptions of display pectin structure, it was demonstrated that
The structure of pectin.And from 1000-1800cm-1Absorb the definitely fine structure of pectin, 1745 cm-1With 1630 cm-1It is ester group-COOCH in pectin structure respectively3With the characteristic absorption of carboxyl-COOH.The two characteristic absorption peaks can be passed through
Power judges that the pectin is high-ester pectin or low-ester pectin, can be with clear view to the pectin product from the infrared spectrum
The absorption of ester group absorptance carboxyl is obvious weak, and carboxyl absorption is strong and obvious, is judged as low-ester pectin, and esterification degree is lower.It is close
3500cm-1It is the absorption peak of-OH in pectin, 2800-2900cm-1It is the stretching absorbance of C-H, 1000-1400 cm-1It is in saccharide ring
The characteristic absorption of C-O key and ring.
Sunflower pectin prepared by green disk sodium citrate technique carries out infrared detection, and infrared spectrum is shown in Fig. 3, produces in pectin
In the infrared spectrum of product, in 1000-3500 cm-1Absorption region in show the due whole characteristic absorptions of pectin structure, card
The structure of bright pectin.And from 1000-1800cm-1Absorb the definitely fine structure of pectin, 1745 cm-1With 1630
cm-1It is ester group-COOCH in pectin structure respectively3With the characteristic absorption of carboxyl-COOH.The two characteristic absorption peaks can be passed through
Power judge that the pectin is high-ester pectin or low-ester pectin, can be produced with clear view to the pectin from this infrared spectrum
The ester group absorption of product is obvious very weak, and carboxyl absorption is strong and obvious, is judged as low-ester pectin, and esterification degree is lower.Close to 3500cm-1
It is the absorption peak of-OH in pectin, 1000-1400 cm-1It is the characteristic absorption of C-O key and ring in saccharide ring.
Experimental example 2: the esterification degree chemical analysis of product:
1. the esterification degree of titration measuring pectin:
0.5 g pectin sample to be measured is weighed in 250 mL conical flasks, the wetting of 1 mL dehydrated alcohol is added.100 mL are added without two
Carbonoxide water.After pectin is completely dissolved, 4 0.5% (g/mL) phenolphthalein indicators of drop are added, it is molten with 0.1 mol/L sodium hydroxide
Drop is fixed, and the sodium hydroxide volume of blank and sample consumption is denoted as V respectively0And V1.It is 0.5 that 20mL concentration is added into each sample liquid
After being vigorously stirred 15 min, 20 mL, 0.5 mol/L hydrochloric acid solution is added in the sodium hydroxide solution of mol/L.4 drops 0.5% are added
Phenolphthalein indicator, is titrated with 0.1 mol/L sodium hydroxide solution again, and the volume of sample consumption sodium hydroxide is denoted as V2.According to
Formula calculates pectin esterification degree.Esterification degree/%=(V2 / V1 + V2 - V0) × 100, the esterification degree of pectin under the technique
Range: 25-34 is typical low-ester pectin.
2. the esterification degree (national standard method) of titration measuring pectin:
Using the esterification degree in the analytical procedure measurement sample in state quality standard.Each pectin sample is accurately weighed first
5.0 g are separately added into 100 mL ethanol solution hydrochlorides, 10 min are sufficiently stirred in beaker.With the dry sand to constant weight
Core funnel (m0) filtering, and be washed till with ethyl alcohol without Cl-, m1 is weighed as after drying.Sample after accurately weighing 1/10 drying
Product are added the wetting of 2 mL dehydrated alcohols, it is abundant to add the distilled water that 100 mL newly boil in 250 mL conical flasks
Dissolution is added 2 drop phenolphthalein indicators, is titrated with 0.1 mol/L NaOH titrand, record the body of its consumption
Product V1(initial titre).The NaOH solution of 20.0 mL, 0.5 mol/L is added, be uniformly mixed and stands 15 min fruits
Glue is sufficiently saponified, and the HCl solution of 20.0 mL, 0.5 mol/L is added, and is uniformly mixed, is neutralized NaOH therein, then use
0.1 mol/LNaOH titrand is titrated, and the volume V of its consumption is recorded2(saponification titer).Total gala in sample
The calculation formula of glucuronic acid content and esterification degree difference is as follows: esterification degree/%=(V2 / V1 + V2) × 100,
Wherein, V1For initial titre, mL；V2To be saponified titer.The esterification range of pectin under the technique: 25-34 is typical
Low-ester pectin.
3. molecular weight and its distributional analysis of product:
Molecular weight and its distribution with efficient liquid phase size exclusion chromatography analysis sample, it is former according to the separation of size exclusion chromatography
Reason, the bigger substance of molecular weight more first pass through chromatographic column, are detected by the detector earliest.40.0 mg pectin sample of accurate weighing
10 mL mobile phases are added in conical flask in product, and mobile phase is 0.05 mol/L Na2SO4Conical flask is placed in 40 by solution
In DEG C water bath chader, until pectin is completely dissolved, then by the solution be placed in a centrifuge centrifugation (6000 rpm, 20
Min), 0.22 μm of filtering with microporous membrane of supernatant finally utilizes the microsyringe sample introduction chromatographic condition of 20 μ L: stream
Dynamic is mutually 0.5 mol/L Na2SO4, 30 DEG C of column temperature, gel chromatographic columns are stationary phase, and molecular weight is respectively 20KD, 62KD,
The glucan of 111KD, 310KD and 390KD make mark product, carry out sample measurement.The gel chromatography figure of reference standards, molecular weight is most
Big mark product (mark 400 KD of product), retention time is 13.58 min.The retention time of gained pectin product exists under the technique
12.15-14.12 min, the molecular weight of initial guess sample are all between 300-400 KD, the molecular weight ranges Mp of test
1.7-3.8X105D.Gel chromatography figure is as shown in Figure 4.
4. the degree of gelation of low-fat pectin is analyzed:
3g sample is first weighed, 15g sucrose is added, together addition 210ml is boiled (has added in water before in hot distilled water
5ml sodium citrate solution, 2.5ml citric acid solution), it boils together；Add the candy boiling of 75g；It is stirred continuously lower addition
12.5mlCaCl2 solution, boils, and constant weight to net weight 300g is poured into degree of gelation test cup, and after filling cup, it is small to stand 20-24
When, check gelling situation." U.S.'s food chemicals code " standard required standard degree of gelation is 100.Surveying degree of gelation is 100
± 5 be qualified products, and Chinese QB2484-2000 carries out degree of gelation test using the extracted pectin of dry pan, sees Fig. 5, degree of gelation
For 90-95；Pectin product prepared by the present invention is shown in Fig. 6.
In sample degree of gelation test process, CaCl is added2Solution, gelling phenomenon is obvious, and sample is once contact CaCl2Solution,
Gelling rapidly, solution retrogradation condensation.CaCl is added2Solution 8ml or more freezes at flexible glue, is added completely into 12.5mlCaCl2Solution,
To the cold at the soft gel of not mobility, can tentatively judge to make to be gelled good low-ester pectin.It imports in measuring cup while hot, mistake
Night is gelled 20-24 hours.Molding jelly can be poured out from gelling cup, test degree of gelation is greater than 95-100.Jelly is completely not
Denaturation, height are slightly sunk, and jelly base diameter slightly broadens, and can maintain a few hours, and gently squeeze to restore quickly.By jelly
It breaks into pieces, consistent internal structure, property is unified.By testing experience, CaCl can also be added by test process2The gelling of solution
Details judges degree of gelation.Solution can accelerate to be gelled to the cold, but can weaken gel strength, and jelly is made to become fragile, but still can reach
To 95 or more degree of gelation.Dry pan can turn yellow or even slight brown the product color of decoloration under the technique.And green disk pectin
Limpid no yellow.Fig. 5 is the product of dry pan salt technique, and solid-liquid ratio is that 1:25. Fig. 6 is present invention process products obtained therefrom, the two
Product degree of gelation all meets the requirements.But the jelly of Fig. 5 is yellow or slight brown, the transparency of Color influences jelly.The glue of Fig. 6
Freeze colorless and transparent, gloss is fine.So to consider color requirement when two kinds of products applications.
The degree of gelation calculation formula of low-ester pectin: degree of gelation=(600/w) × [2.00- (reading 10)/25.0]；Its
In: the taken pectin samples grams of W-, the sagging rate of reading-.Conversion factor=degree of gelation/standard degree of gelation=2.00- (reading+
4.5)/25.0 ；
The pectin product of the above physicochemical property, gelling are slightly poor.Soft gel can be formed in gelatinization, can be used for preparing medicine
Use colloidal bismuth pectin.It can also be used for hypoglycemic, reducing blood lipid, can be also used for releasing lead poisoning, Medicament for Alcoholism, the health care products such as meal replacement powder.Always
It, this products application is in the field not being strict with to pectin gelling and color.
Embodiment described above is only used to illustrate the technical scheme of the present invention and not to limit it, all in spirit and original of the invention
Any modifications, equivalent replacements, and improvements etc. then done in range, should be included within the scope of the present invention.
Claims (9)
1. a kind of method for extracting pectin from sunflower blueness disk using salt, it is characterised in that: using sunflower blueness disk as raw material, >=
Enzyme deactivation 15-22min in 95 DEG C of thermostat water baths, filtering, discards enzyme deactivation liquid；Distillation is added for 1:5-15 with solid-liquid ratio in precipitating
Solid oxalic acid ammonium or sodium citrate is added in water, the concentration for controlling reaction system mesoxalic acid ammonium or sodium citrate be 0.2-1.0% into
Row extracts, and Extracting temperature is 80-90 DEG C, extraction time 20-60min；Filtering, filtrate decompression rotary distillation are concentrated into former molten
0.3-0.5 times of liquid product, the sunflower plate extracting solution being concentrated；Concentrate is precipitated with ethyl alcohol, is filtered after standing
To pectin, gained pectin washs 1-3 dehydration with dehydrated alcohol and is sieved, and naturally dry or 40 DEG C or less are dried, and crushes to obtain pectin
Powder.
2. a kind of method for extracting pectin from sunflower blueness disk using salt according to claim 1, it is characterised in that: de-
The fresh sunflower plate of seed several times with clear water rinsing removes silt, dust, drains, be cut into the block of 0.8-1.5cm；It is described it is fresh to
The water content of day certain herbaceous plants with big flowers disk is 80-90%.
3. a kind of method for extracting pectin from sunflower blueness disk using salt according to claim 2, it is characterised in that: de-
The fresh sunflower plate of seed several times with clear water rinsing removes silt, dust, drains, be cut into the block of 1.0cm.
4. a kind of method for extracting pectin from sunflower blueness disk using salt according to claim 1, it is characterised in that: go out
It is filtered after enzyme with 150-300 mesh nylon cloth；300-500 mesh nylon cloth filters after alcohol precipitation is stood；60 meshes are crossed after dehydration.
5. a kind of method for extracting pectin from sunflower blueness disk using salt according to claim 1, it is characterised in that: mention
Taking temperature is 85 DEG C, extraction time 45min；It is filtered at >=70 DEG C after the completion of extraction.
6. a kind of method for extracting pectin from sunflower blueness disk using salt according to claim 1, it is characterised in that: institute
The temperature for stating vacuum distillation is 60-70 DEG C.
7. a kind of method for extracting pectin from sunflower blueness disk using salt according to claim 1, it is characterised in that: second
The ethyl alcohol that alcohol precipitating concentration of alcohol used is 90% or more, dosage are 1-3 times of the volume of the concentrated liquid, and alcohol precipitation sequence is extracting solution
It imports in ethyl alcohol, the alcohol precipitation time is 20-24h.
8. a kind of method for extracting pectin from sunflower blueness disk using salt according to claim 7, it is characterised in that: second
The ethyl alcohol that alcohol precipitating concentration of alcohol used is 90%-95%, dosage are 1.2-1.6 times of the volume of the concentrated liquid.
9. a kind of method for extracting pectin from sunflower blueness disk using salt according to claim 1, it is characterised in that: institute
The esterification degree 20 ~ 34% of the pectin of acquisition, 500 KD-100 KD of molecular weight ranges.
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| CN110833194A (en) * | 2019-10-28 | 2020-02-25 | 中北大学 | Controlled-release sunflower disc low-ester pectin iron composite iron supplement and preparation method thereof |
| CN111349183A (en) * | 2020-04-22 | 2020-06-30 | 黑龙江八一农垦大学 | Pectin and its extraction method and preparation method |
| CN112159485A (en) * | 2019-09-20 | 2021-01-01 | 山东皇尊庄园山楂酒有限公司 | Hawthorn pectin extraction process and hawthorn product |
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