CN106243242A - A kind of utilize degraded the solubilization technique method that Fructus Jujubae pectin is prepared in extraction from Fructus Jujubae Fructus Jujubae slag - Google Patents
A kind of utilize degraded the solubilization technique method that Fructus Jujubae pectin is prepared in extraction from Fructus Jujubae Fructus Jujubae slag Download PDFInfo
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- CN106243242A CN106243242A CN201610775084.5A CN201610775084A CN106243242A CN 106243242 A CN106243242 A CN 106243242A CN 201610775084 A CN201610775084 A CN 201610775084A CN 106243242 A CN106243242 A CN 106243242A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- 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
Abstract
The present invention is a kind of utilizes the degraded solubilization technique method that Fructus Jujubae pectin is prepared in extraction from Fructus Jujubae Fructus Jujubae slag, belongs to technical field of food biotechnology；Comprising the following steps, Fructus Jujubae slag pretreatment, demetalization ion, the multienzyme method of fractional steps is extracted, and first carries out cellulase, hemicellulose complex enzyme zymohydrolysis, then carries out protease, lipase complex enzyme zymohydrolysis, centrifugal, and decolouring concentrates, and is dried, prepares finished product；The present invention uses many enzyme extraction methods to combine chelating method and extracts Fructus Jujubae pectin；Obtain the specific Fructus Jujubae pectin product with enhancing human body immunity that a kind of purity is high, gelation is good, make full use of Fructus Jujubae and be worth, improve Fructus Jujubae resource utilization, reduce environmental pollution and the wasting of resources simultaneously；Through technology purification pectin products such as decolouring and membrance separation, product purity is high, and extraction ratio is high.
Description
Technical field
The present invention is a kind of utilizes the degraded solubilization technique method that Fructus Jujubae pectin is prepared in extraction from Fructus Jujubae Fructus Jujubae slag, belongs to food
Biological technical field.
Background technology
Pectin is one of composition of tissue substance cell wall, is present in the cellular layer between flanking cell wall, plays cell
The glutinous effect together of wall.The pectin of separate sources, its characteristic is the most each variant.Natural pectin is based on linear polysaccharide, contains
Having the chain structure formed from hundreds of to more than 1000 glycogen, mean molecule quantity is 500,000-150 ten thousand.The base of pectic backbone molecule
This composition is D-galacturonic acid, also has some natural neutral sugars such as rhamnose, arabinose, xylose, galactose, glucose etc.
Exist in pectin.Pectin is the white powder thing of yellowish, soluble in water, forms the tasteless solution of thickness, electronegative.
Pectin is a kind of natural polymer, has good gelling and emulsion stability effect, be widely used for food,
Medicine, daily use chemicals and textile industry.
It is reported, nearly 4.5 ten thousand t of annual requirement of whole world pectin, current China the most about consumes more than pectin 1500t,
Wherein 80% from external import.Pectin is as food additive, and its demand will be with annual 15% within considerable time
Speed increment.Because the price of import pectin is 1～2 times of domestic pectin price, so in the urgent need to low price, high-quality in Sheng Chaning
Domestic pectin, increase pectin yield, improve the target that pectin quality is China's pectin industry development, make full use of China's abundant
Pectin resource, produce high-quality pectin, meet domestic market demand, meet the developing direction of China's food additive industry.
Fructus Jujubae is the characteristic fruit of China, has long cultivation history, and red date nutrient is abundant and comprehensive, is that one has
The highest nutrition and the fruit of medical value.Fructus Jujubae Fructus Jujubae slag is the by-product after Fructus Jujubae processing, but due to function in Fructus Jujubae slag, Fructus Corni
Property content of material is relatively low causes extraction ratio low, process of extracting is complicated, and organic solvent used easily pollutes environment, simultaneously other big portions
Schizocarp glue polysaccharide can not make full use of, therefore can not widespread adoption in commercial production.In addition, owing to technology is weak, red
The exploitation of Fructus Jujubae processing byproduct Fructus Jujubae slag Fructus Corni, still in the primary stage, are mainly used as feed stripped or arrange as garbage
Put, cause environmental pollution and the wasting of resources.
In Fructus Jujubae, pectin resource content is the abundantest, especially at Fructus Corni and Fructus Jujubae slag.Red jujube fruit xanthan molecule amount exists
More than 2000kD (gellation pectin product high, stay-in-grade all concentrates in the scope that molecular weight is big), is far longer than it
The pectin molecule amount of his plant extract, research simultaneously shows that Fructus Jujubae pectin has the effect of certain enhancing human body immunity.Therefore choosing
With Fructus Jujubae Fructus Jujubae slag as the raw material of pectin extraction, gel effect can be obtained good, there is the specific pectin of enhancing human body immunity
Material.
But pectin has difficult decolouring, the feature of difficult purification in Fructus Jujubae.In Fructus Jujubae, red pigment is relatively deep, containing much more relatively
Calcium, iron ion, and calcium, iron ion have the strongest sealing process to pectin, are unfavorable for pectin dissolution (de-envelope in the presence of it
Close ion), Fructus Jujubae pectin has chelated substantial amounts of calcium ion in cell, simultaneously with cellulose, protein, lipid material and shallow lake
Amylaceous substances etc. form threadiness space structure with covalent bond, non-covalent bond form, make pectin be difficult to be dissolved out.Meanwhile, Fructus Jujubae
Possibly together with a large amount of liposoluble constituents in pectin, the purification of pectin is had a great impact (defat pledge).But common soda acid
Pectin substance in Fructus Jujubae can not be extracted by extraction method completely, but also can destroy the molecular structure of pectin substance.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, technical problem to be solved to be to provide a kind of utilization degraded solubilization technique
The method that Fructus Jujubae pectin is prepared in extraction from Fructus Jujubae Fructus Jujubae slag, obtains that a kind of purity is high, gelation is good has enhancing human body immunity
Specific Fructus Jujubae pectin product；Use Fructus Jujubae Fructus Jujubae slag to extract pectin product, make full use of Fructus Jujubae and be worth, improve Fructus Jujubae resource
Utilization rate.
For solving above-mentioned technical problem, the technical solution adopted in the present invention is: a kind of utilization degraded solubilization technique is from red
The method that in Fructus Jujubae Fructus Jujubae slag, Fructus Jujubae pectin is prepared in extraction, comprises the following steps:
The first step, Fructus Jujubae slag pretreatment, sterilizing；By broken for Fructus Jujubae ground-slag, cross 100 mesh sieves, add 95% alcohol reflux 20min of volume,
Be filtered to remove ethanol, with distilled water flushing Fructus Jujubae slag to cleaning mixture colourless, 60 DEG C dry after standby；
In Fructus Jujubae slag tissue in addition to containing abundant pectin, possibly together with decomposing the pectase system of pectin, including pectinesterase,
Pectin lyases etc., live if not carrying out pretreatment enzyme denaturing, during heating extraction, and the tral sugar side chains on pectin molecule,
Will be degraded in a large number and eliminate, make the molecular weight of pectin diminish, space structure changes, and then cause extraction ratio and quality
Reduce.So general first pretreatment Fructus Jujubae slag before extraction pectin, to reach to inactivate the purpose of pectase.
Second step, demetalization ion；Use EDTA chelating agen auxiliary law, the Fructus Jujubae slag specimen product obtained of upper step are joined
In the EDTA solution of 0.05mol/L, making liquid-solid ratio is 24:1(L/kg), Extracting temperature 35 DEG C, time 3-4h, obtain extracting solution；
Containing relatively many calcium, iron ion in Fructus Jujubae cell, and calcium, iron ion have the strongest sealing process to pectin, and it exists
In the case of be unfavorable for pectin dissolution (de-close ion), meanwhile, the existence of metal ion can produce suppression to the effect of enzyme and make
With.Therefore before using Enzymatic Extraction pectin, so chelating agen is first used to be separated from pectin structure by Ga ion.
3rd step, the multienzyme method of fractional steps is extracted；First carry out cellulase, hemicellulose complex enzyme zymohydrolysis, by said extracted liquid
Carrying out cellulase, hemicellulose complex enzyme zymohydrolysis, obtaining optimal enzymatic hydrolysis condition by orthogonal test is: with cellulase:
The compound enzyme of hemicellulase 1.2:1 mixing, temperature 45 C, pH4.5, enzyme dosage are 0.8%, extraction time 4-5h；
Carry out protease, lipase complex enzyme zymohydrolysis again, after above-mentioned enzyme digestion reaction terminates, reacting liquid temperature be adjusted to 55 DEG C,
PH6, joins in reactant liquor by papain and lipase in the ratio of 1:1, and enzyme dosage is 1.0%, and extraction time is 3-
4h.Obtain enzymatic pectin hydrolysate；
At present, the extracting method of pectin mainly has acid extraction method, enzyme lifting manipulation, microbe fermentation method etc..Acid its principle of lifting manipulation is to adopt
With diluted acid, the water-insoluble Pectin, proto in pericarp membrane being hydrolyzed to water soluble pectin, pectin productivity can reach more than 26%, but carry
During taking, pectin molecule can occur local to hydrolyze, and reduces pectin relative molecular mass, thus affects pectin yield and quality,
As extracted process, use higher temperature and heating for a long time, make the pectin in raw material inevitably be deformed and divide
Solve broken ring, second-rate.Additionally, due to extracting solution viscosity is big, it is slow to filter, thus result in production cycle length, efficiency low；Enzyme extraction
Method is the extracting method that natural extract field quickly grows in recent years, with tradition alkaline process and acid system compared with, have extraction time short,
Product quality is high and saves the advantages such as energy consumption, but owing to the requirement of enzyme is differed by different material, therefore adds technical difficulty.This
Outward, single enzyme system extracts, and can not extract pectin substance completely and cause extraction ratio low.Therefore use multienzyme step by step arithmetic side
Method, uses different enzyme systems according to the structure substep of pectin, makes Fructus Jujubae pectin isolate from its fibrous reticular structure completely
Come.
(1) cellulase, hemicellulase: most of pectic substances are with covalent bond or the form of non-covalent bond and cell
The macromole such as the cellulose of wall, hemicellulose associate, and they are mutually associated by secondary key with other cell wall polymer simultaneously
Form fibrous space structure.
(2) protease and lipase: containing rich in protein, lipoid material in Fructus Jujubae, these materials are all with covalency
The form of key or non-covalent bond is combined in pectin structure, causes pectin water solublity to decline.
4th step, centrifugal；The enzymatic pectin hydrolysate 15000r/min that 3rd step obtains is centrifuged 5min, remove insoluble matter and
Enzyme agent, obtains pectin extracting soln.
Remove insoluble matter and enzyme agent, but after enzymolysis and extraction, enzymolysis solution can incorporate the miscellaneous of the little molecules such as pigment
Matter, needs through technology purification pectin products such as decolouring and membrance separation.
5th step, decolouring；The D900 type decolorizing resin processed is loaded in the chromatographic column that specification is 600mm × 50mm,
Charge weight is the 2/3 of pillar height, and regulation pH value is 6 standby, the pectin extracting soln that the 4th step is obtained at ambient temperature, with
Being decoloured by resin under the flow velocity of 200mL/h, after collecting decolouring, pectin extracting soln is standby；
In Fructus Jujubae, red pigment is relatively deep, has the feature of difficult decolouring, although Ethanol Treatment can go out part surface in the first step
Pigment, but most pigment molecular there is also and Fructus Jujubae slag kind, along with the extraction of pectin is dissolved in enzymolysis solution, has influence on
The purity of pectin.Therefore need to select suitable discoloration method to decolour.
Selection Flavonoids by Macroporous Adsorption Resin decolours, and the method disposal ability is big, and decolouring capacity is high, can remove various different color
Element, can use with repeated regeneration, and service life is long, and cost is low, reduces the chemical substance pollution to pectin.
6th step, concentrates；Use the ultrafilter membrane of 5 kinds of PSPPs (300KD, 100KD, 30KD, 10KD, 5KD)
Components apart pectin, under room temperature condition, inlet pressure 70kPa, outlet pressure 30kPa, by pectin extracting soln after decolouring through following
Ring pump is sequentially inputted in the membrane module that molecular weight is descending, obtain after ultra-filtration and separation more than 300KD, 300KD-100KD,
100KD-30KD, 30KD-10KD, 10KD-5KD and less than 5KD six part pectin sample liquid；
Use membrane separation concentration method.The method of being concentrated in vacuo is easily caused pectin solution brown stain, affects quality, therefore uses membrane separation concentration
Method, the method can be isolated glucide and other low molecular compounds from pectin extracting soln selectively, thus obtain
To high-quality pectin, this technology is simply efficient, the maintenance of low-carbon environment-friendly, beneficially equipment and the holding to pectin fine quality, with
Time can get the pectin product of different molecular weight ranges according to different membrane molecule amounts, the pectin product of different molecular weight has not
Same effect, and gellation pectin product high, stay-in-grade all concentrates in the scope that molecular weight is big.
7th step, is dried；Employing spray dryer is dried, by the pectin sample liquid of different component 130 DEG C～160 DEG C of winks
Time atomization drying obtain the pectin finished product of different molecular weight；Dried product sieves powder through 60 mesh sieves, i.e. obtains different molecular weight
Jelly powder；
The quality of pectin is had important impact, main drying means to have cold drying, spray dried by the dry technology of pectin
Dry and vacuum lyophilization three kinds.The pectin product dissolubility that wherein cold drying obtains is poor, and color and luster is relatively deep, vacuum lyophilization
There is the shortcomings such as big, time length that consume energy.Therefore selection spray drying method, this method can obtain without precipitation byte spray drying technology
Product, products obtained therefrom powder is little, and dissolubility is good, low cost.
8th step, prepares finished product；The pectin selecting the hyperfiltration membrane assembly of more than 100KD to separate, obtains molecular weight and is more than
The Fructus Jujubae pectin finished product of 100KD.
Owing to the pectin substance of high molecular has more excellent gelation and stability, therefore select molecular weight more than 100KD
Hyperfiltration membrane assembly separation pectin, obtain molecular weight more than the Fructus Jujubae pectin substance of 100KD.
Described a kind of utilize the degraded solubilization technique method that Fructus Jujubae pectin is prepared in extraction from Fructus Jujubae Fructus Jujubae slag, the 8th step institute
Obtaining Fructus Jujubae pectin finished product, for faint yellow or light brown powder, loss on drying is 5.43 w% ± 0.12, sulfur dioxide: 32.21
Mg/kg ± 0.24, acid insoluble ash: 0.73 w% ± 0.03, total galacturonic acid: 89.96 w% ± 0.64, lead: 0.35 mg/
kg±0.02。。
A kind of described degraded solubilization technique method that Fructus Jujubae pectin is prepared in extraction from Fructus Jujubae Fructus Jujubae slag that utilizes, the 6th step,
Concentrate Fructus Jujubae pectin and be concentrated mainly on macromolecule part, reach more than 90%；Its middle-molecular-weihydroxyethyl reaches 78.24% more than 300KD
Above, 300KD-100KD part accounts for more than 14.31%.
Compared with prior art the invention have the advantages that.
1, the nutritive value that Fructus Jujubae pectin is unique, in Fructus Jujubae, pectin resource content is the abundantest, especially at Fructus Corni and
Fructus Jujubae slag.At more than 2000kD, (it is big that gellation pectin product high, stay-in-grade all concentrates on molecular weight to red jujube fruit xanthan molecule amount
In the range of), it being far longer than the pectin molecule amount that other plant extracts, research simultaneously shows that Fructus Jujubae pectin has certain enhancing
The effect of immunity of organism.
2, the present invention uses many enzyme extraction methods to combine chelating method and extracts Fructus Jujubae pectin；Obtain that a kind of purity is high, gelation is good
The specific Fructus Jujubae pectin product with enhancing human body immunity.
3, use Fructus Jujubae Fructus Jujubae slag to extract pectin product, Fructus Jujubae can be made full use of and be worth, improve Fructus Jujubae resource utilization.With
Time reduce environmental pollution and the wasting of resources.
4, use multienzyme step-by-step extracting method, use different enzyme systems according to the structure substep of pectin, make Fructus Jujubae pectin complete
Complete separates from its fibrous reticular structure.First carry out cellulase, hemicellulose complex enzyme zymohydrolysis, destroy the sky of material
Between structure, be more beneficial for next step and destroy covalent bond or non covalent bond structure；Carry out protease, lipase complex enzyme zymohydrolysis again,
Pectin is made to spin off from space structure completely.
5, through technology purification pectin products such as decolouring and membrance separation, product purity is high, and extraction ratio is high.
6, being concentrated mainly on macromolecule part due to Fructus Jujubae pectin, reach more than 90%, molecular weight accounts for more than 300KD's
Great majority, reach 78.24%, next to that 300KD-100KD part, account for 14.31%.Therefore it is big to obtain molecular weight by membrane separation technique
Fructus Jujubae pectin substance in 100KD.
7, process low temperature, pollution-free is extracted.Whole extraction process is except the TRANSIENT HIGH TEMPERATURE being spray-dried, and temperature is all not less than 60
DEG C, it is to avoid the high temperature impact on pectin quality.The most whole process do not adds any chemical substance, it is to avoid chemical substance
Pollution to pectin.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of utilize degraded the solubilization technique method that Fructus Jujubae pectin is prepared in extraction from Fructus Jujubae Fructus Jujubae slag, comprise the following steps:
The first step, Fructus Jujubae slag pretreatment, sterilizing；By broken for Fructus Jujubae ground-slag, cross 100 mesh sieves, add 95% alcohol reflux 20min of volume,
Be filtered to remove ethanol, with distilled water flushing Fructus Jujubae slag to cleaning mixture colourless, 60 DEG C dry after to obtain Fructus Jujubae slag specimen product standby；
Second step, demetalization ion；Use EDTA chelating agen auxiliary law, the Fructus Jujubae slag specimen product obtained of upper step are joined
In the EDTA solution of 0.05mol/L, making liquid-solid ratio is 24:1(L/kg), Extracting temperature 35 DEG C, time 3h, obtain extracting solution；
3rd step, the multienzyme method of fractional steps is extracted；First carry out cellulase, hemicellulose complex enzyme zymohydrolysis, said extracted liquid is carried out
Cellulase, hemicellulose complex enzyme zymohydrolysis, enzymatic hydrolysis condition is: with cellulase: being combined of hemicellulase 1.2:1 mixing
Enzyme, temperature 45 C, pH4.5, enzyme dosage are the 0.8% of extracting solution quality, and extraction time is 4h, obtains reactant liquor；
Carrying out protease, lipase complex enzyme zymohydrolysis again, reacting liquid temperature is adjusted to 55 DEG C, pH6, by papain and fat
Fat enzyme joins in reactant liquor in the ratio of 1:1, and the total amount of enzyme is the 1.0% of reactant liquor quality, and extraction time is 4h, obtains fruit
Glue enzymolysis solution；
4th step, centrifugal；The enzymatic pectin hydrolysate 15000r/min that 3rd step obtains is centrifuged 5min, removes insoluble matter and enzyme
Agent, obtains pectin extracting soln；
5th step, decolouring；The D900 type decolorizing resin processed is loaded in the chromatographic column that specification is 600mm × 50mm, loads
2/3 that amount is pillar height, regulation pH value is 6 standby, the pectin extracting soln that the 4th step is obtained at ambient temperature, with
Being decoloured by resin under the flow velocity of 200mL/h, after collecting decolouring, pectin extracting soln is standby；
6th step, concentrates；Use 5 kinds of hyperfiltration membrane assemblies of PSPP (300KD, 100KD, 30KD, 10KD, 5KD)
Separating pectin, under room temperature condition, inlet pressure 70kPa, outlet pressure 30kPa, after decolouring, pectin extracting soln is through circulating pump
Be sequentially inputted in the membrane module that molecular weight is descending, obtain after ultra-filtration and separation more than 300KD, 300KD-100KD,
100KD-30KD, 30KD-10KD, 10KD-5KD and less than 5KD six part pectin sample liquid；
7th step, is dried；Employing spray dryer is dried, by the pectin sample liquid of different component at 130 DEG C～160 DEG C of instantaneous mists
Change the pectin finished product being dried to obtain different molecular weight；Dried product sieves powder through 60 mesh sieves, i.e. obtains different molecular weight pectin
Powder；
8th step, prepares finished product；The pectin selecting the hyperfiltration membrane assembly of more than 100KD to separate, obtains molecular weight more than 100KD's
Fructus Jujubae pectin finished product.
Gained Fructus Jujubae pectin finished product, for faint yellow or light brown powder, loss on drying is 5.43 w% ± 0.12, titanium dioxide
Sulfur: 32.21 mg/kg ± 0.24, acid insoluble ash: 0.73 w% ± 0.03, total galacturonic acid: 89.96 w% ± 0.64, lead:
0.35 mg/kg±0.02。。
Embodiment 2
A kind of utilize degraded the solubilization technique method that Fructus Jujubae pectin is prepared in extraction from Fructus Jujubae Fructus Jujubae slag, comprise the following steps:
The first step, Fructus Jujubae slag pretreatment, sterilizing；By broken for Fructus Jujubae ground-slag, cross 100 mesh sieves, add 95% alcohol reflux of certain volume
20min, is filtered to remove ethanol, with distilled water flushing Fructus Jujubae slag to cleaning mixture colourless, 60 DEG C dry after standby；
Second step, demetalization ion；Use EDTA chelating agen auxiliary law, the Fructus Jujubae slag specimen product obtained of upper step are joined
In the EDTA solution of 0.05mol/L, making liquid-solid ratio is 24:1(L/kg), Extracting temperature 35 DEG C, time 4h, obtain extracting solution；
3rd step, the multienzyme method of fractional steps is extracted；First carry out cellulase, hemicellulose complex enzyme zymohydrolysis, said extracted liquid is carried out
Cellulase, hemicellulose complex enzyme zymohydrolysis, enzymatic hydrolysis condition is: with cellulase: being combined of hemicellulase 1.2:1 mixing
Enzyme, temperature 45 C, pH4.5, enzyme dosage are 0.8%, and extraction time is 5h；
Carrying out protease, lipase complex enzyme zymohydrolysis again, reacting liquid temperature is adjusted to 55 DEG C, pH6, by papain and fat
Fat enzyme joins in reactant liquor in the ratio of 1:1, and enzyme dosage is 1.0%, and extraction time is 3h, obtains enzymatic pectin hydrolysate；
4th step, centrifugal；The enzymatic pectin hydrolysate 15000r/min that 3rd step obtains is centrifuged 5min, removes insoluble matter and enzyme
Agent, obtains pectin extracting soln；
5th step, decolouring；The D900 type decolorizing resin processed is loaded in the chromatographic column that specification is 600mm × 50mm, loads
2/3 that amount is pillar height, regulation pH value is 6 standby, the pectin extracting soln that the 4th step is obtained at ambient temperature, with
Being decoloured by resin under the flow velocity of 200mL/h, after collecting decolouring, pectin extracting soln is standby；
6th step, concentrates；Use the hyperfiltration membrane assembly of 5 kinds of PSPPs (300KD, 100KD, 30KD, 10KD, 5KD)
Separating pectin, under room temperature condition, inlet pressure 70kPa, outlet pressure 30kPa, after decolouring, pectin extracting soln is through circulating pump
Be sequentially inputted in the membrane module that molecular weight is descending, obtain after ultra-filtration and separation more than 300KD, 300KD-100KD,
100KD-30KD, 30KD-10KD, 10KD-5KD and less than 5KD six part pectin sample liquid；
7th step, is dried；Employing spray dryer is dried, by the pectin sample liquid of different component at 130 DEG C～160 DEG C of instantaneous mists
Change the pectin finished product being dried to obtain different molecular weight；Dried product sieves powder through 60 mesh sieves, i.e. obtains different molecular weight pectin
Powder；
8th step, prepares finished product；The pectin selecting the hyperfiltration membrane assembly of more than 100KD to separate, obtains molecular weight more than 100KD's
Fructus Jujubae pectin finished product.
Gained Fructus Jujubae pectin finished product, for faint yellow or light brown powder, loss on drying be loss on drying be 5.43 w% ±
0.12, sulfur dioxide: 32.21 mg/kg ± 0.24, acid insoluble ash: 0.73 w% ± 0.03, total galacturonic acid: 89.96
W% ± 0.64, lead: 0.35 mg/kg ± 0.02..
Embodiment 3
A kind of utilize degraded the solubilization technique method that Fructus Jujubae pectin is prepared in extraction from Fructus Jujubae Fructus Jujubae slag, comprise the following steps:
The first step, Fructus Jujubae slag pretreatment, sterilizing；By broken for Fructus Jujubae ground-slag, cross 100 mesh sieves, add 95% alcohol reflux of certain volume
20min, is filtered to remove ethanol, with distilled water flushing Fructus Jujubae slag to cleaning mixture colourless, 60 DEG C dry after standby；
Second step, demetalization ion；Use EDTA chelating agen auxiliary law, the Fructus Jujubae slag specimen product obtained of upper step are joined
In the EDTA solution of 0.05mol/L, making liquid-solid ratio is 24:1(L/kg), Extracting temperature 35 DEG C, time 3.5h, obtain extracting solution；
3rd step, the multienzyme method of fractional steps is extracted；First carry out cellulase, hemicellulose complex enzyme zymohydrolysis, said extracted liquid is carried out
Cellulase, hemicellulose complex enzyme zymohydrolysis, enzymatic hydrolysis condition is: with cellulase: being combined of hemicellulase 1.2:1 mixing
Enzyme, temperature 45 C, pH4.5, enzyme dosage are 0.8%, and extraction time is 4.5h；
Carrying out protease, lipase complex enzyme zymohydrolysis again, reacting liquid temperature is adjusted to 55 DEG C, pH6, by papain and fat
Fat enzyme joins in reactant liquor in the ratio of 1:1, and enzyme dosage is 1.0%, and extraction time is 3.5h, obtains enzymatic pectin hydrolysate；
4th step, centrifugal；The enzymatic pectin hydrolysate 15000r/min that 3rd step obtains is centrifuged 5min, removes insoluble matter and enzyme
Agent, obtains pectin extracting soln；
5th step, decolouring；The D900 type decolorizing resin processed is loaded in the chromatographic column that specification is 600mm × 50mm, loads
2/3 that amount is pillar height, regulation pH value is 6 standby, the pectin extracting soln that the 4th step is obtained at ambient temperature, with
Being decoloured by resin under the flow velocity of 200mL/h, after collecting decolouring, pectin extracting soln is standby；
6th step, concentrates；Use the hyperfiltration membrane assembly of 5 kinds of PSPPs (300KD, 100KD, 30KD, 10KD, 5KD)
Separating pectin, under room temperature condition, inlet pressure 70kPa, outlet pressure 30kPa, after decolouring, pectin extracting soln is through circulating pump
Be sequentially inputted in the membrane module that molecular weight is descending, obtain after ultra-filtration and separation more than 300KD, 300KD-100KD,
100KD-30KD, 30KD-10KD, 10KD-5KD and less than 5KD six part pectin sample liquid；
7th step, is dried；Employing spray dryer is dried, by the pectin sample liquid of different component at 130 DEG C～160 DEG C of instantaneous mists
Change the pectin finished product being dried to obtain different molecular weight；Dried product sieves powder through 60 mesh sieves, i.e. obtains different molecular weight pectin
Powder；
8th step, prepares finished product；The pectin selecting the hyperfiltration membrane assembly of more than 100KD to separate, obtains molecular weight more than 100KD's
Fructus Jujubae pectin finished product.
Gained Fructus Jujubae pectin finished product, for faint yellow or light brown powder, loss on drying be loss on drying be 5.43 w% ±
0.12, sulfur dioxide: 32.21 mg/kg ± 0.24, acid insoluble ash: 0.73 w% ± 0.03, total galacturonic acid: 89.96
W% ± 0.64, lead: 0.35 mg/kg ± 0.02..
Embodiment 4
A kind of utilize degraded the solubilization technique method that Fructus Jujubae pectin is prepared in extraction from Fructus Jujubae Fructus Jujubae slag, comprise the following steps:
The first step, Fructus Jujubae slag pretreatment, sterilizing；By broken for Fructus Jujubae ground-slag, cross 100 mesh sieves, add 95% alcohol reflux of certain volume
20min, is filtered to remove ethanol, with distilled water flushing Fructus Jujubae slag to cleaning mixture colourless, 60 DEG C dry after standby；
Second step, demetalization ion；Use EDTA chelating agen auxiliary law, the Fructus Jujubae slag specimen product obtained of upper step are joined
In the EDTA solution of 0.05mol/L, making liquid-solid ratio is 24:1(L/kg), Extracting temperature 35 DEG C, time 3h, obtain extracting solution；
3rd step, the multienzyme method of fractional steps is extracted；First carry out cellulase, hemicellulose complex enzyme zymohydrolysis, said extracted liquid is carried out
Cellulase, hemicellulose complex enzyme zymohydrolysis, enzymatic hydrolysis condition is: with cellulase: being combined of hemicellulase 1.2:1 mixing
Enzyme, temperature 45 C, pH4.5, enzyme dosage are 0.8%, and extraction time is 5h；
Carrying out protease, lipase complex enzyme zymohydrolysis again, reacting liquid temperature is adjusted to 55 DEG C, pH6, by papain and fat
Fat enzyme joins in reactant liquor in the ratio of 1:1, and enzyme dosage is 1.0%, and extraction time is 3h, obtains enzymatic pectin hydrolysate；
4th step, centrifugal；The enzymatic pectin hydrolysate 15000r/min that 3rd step obtains is centrifuged 5min, removes insoluble matter and enzyme
Agent, obtains pectin extracting soln；
5th step, decolouring；The D900 type decolorizing resin processed is loaded in the chromatographic column that specification is 600mm × 50mm, loads
2/3 that amount is pillar height, regulation pH value is 6 standby, the pectin extracting soln that the 4th step is obtained at ambient temperature, with
Being decoloured by resin under the flow velocity of 200mL/h, after collecting decolouring, pectin extracting soln is standby；
6th step, concentrates；Use the hyperfiltration membrane assembly of 5 kinds of PSPPs (300KD, 100KD, 30KD, 10KD, 5KD)
Separating pectin, under room temperature condition, inlet pressure 70kPa, outlet pressure 30kPa, after decolouring, pectin extracting soln is through circulating pump
Be sequentially inputted in the membrane module that molecular weight is descending, obtain after ultra-filtration and separation more than 300KD, 300KD-100KD,
100KD-30KD, 30KD-10KD, 10KD-5KD and less than 5KD six part pectin sample liquid；
7th step, is dried；Employing spray dryer is dried, by the pectin sample liquid of different component at 130 DEG C～160 DEG C of instantaneous mists
Change the pectin finished product being dried to obtain different molecular weight；Dried product sieves powder through 60 mesh sieves, i.e. obtains different molecular weight pectin
Powder；
8th step, prepares finished product；The pectin selecting the hyperfiltration membrane assembly of more than 100KD to separate, obtains molecular weight more than 100KD's
Fructus Jujubae pectin finished product.
Gained Fructus Jujubae pectin finished product, for faint yellow or light brown powder, loss on drying is 5.43 w% ± 0.12, titanium dioxide
Sulfur: 32.21 mg/kg ± 0.24, acid insoluble ash: 0.73 w% ± 0.03, total galacturonic acid: 89.96 w% ± 0.64, lead:
0.35 mg/kg±0.02。。
The present invention can summarize with other the concrete form without prejudice to the spirit or essential characteristics of the present invention.Therefore, nothing
Opinion is from the point of view of which point, and the embodiment above of the present invention all can only be considered the description of the invention and can not limit invention,
Claims indicate the scope of the present invention, and the scope of the present invention is not pointed out in above-mentioned explanation, therefore, with the present invention
The suitable implication of claims and scope in any change, be all considered as being included within the scope of the claims.
Claims (5)
1. one kind utilizes the degraded solubilization technique method that Fructus Jujubae pectin is prepared in extraction from Fructus Jujubae Fructus Jujubae slag, it is characterised in that include
Following steps:
The first step, Fructus Jujubae slag pretreatment, sterilizing；By broken for Fructus Jujubae ground-slag, cross 100 mesh sieves, add 95% alcohol reflux 20min, cross and filter
Remove ethanol, with distilled water flushing Fructus Jujubae slag to cleaning mixture colourless, 60 DEG C dry after to obtain Fructus Jujubae slag specimen product standby；
Second step, demetalization ion；Use EDTA chelating agen auxiliary law, the Fructus Jujubae slag specimen product obtained of upper step are joined
In the EDTA solution of 0.05mol/L, making liquid-solid ratio is 24 L:1kg, Extracting temperature 35 DEG C, and time 3-4h obtains extracting solution；
3rd step, the multienzyme method of fractional steps is extracted；First carry out cellulase, hemicellulose complex enzyme zymohydrolysis, said extracted liquid is carried out
Cellulase, hemicellulose complex enzyme zymohydrolysis, enzymatic hydrolysis condition is: with cellulase: being combined of hemicellulase 1.2:1 mixing
Enzyme, temperature 45 C, pH4.5, enzyme dosage are the 0.8% of extracting solution quality, and extraction time is 4-5h, obtains reactant liquor；
Carrying out protease, lipase complex enzyme zymohydrolysis again, reacting liquid temperature is adjusted to 55 DEG C, pH6, by papain and fat
Fat enzyme joins in reactant liquor in the ratio of 1:1, and the total amount of enzyme is the 1.0% of reactant liquor quality, and extraction time is 3-4h, obtains
Enzymatic pectin hydrolysate；
4th step, centrifugal；The enzymatic pectin hydrolysate 15000r/min that 3rd step obtains is centrifuged 5min, removes insoluble matter and enzyme
Agent, obtains pectin extracting soln；
5th step, decolouring；The D900 type decolorizing resin processed is loaded in the chromatographic column that specification is 600mm × 50mm, loads
2/3 that amount is pillar height, regulation pH value is 6 standby, the pectin extracting soln that the 4th step is obtained at ambient temperature, with
Being decoloured by resin under the flow velocity of 200mL/h, after collecting decolouring, pectin extracting soln is standby；
6th step, concentrates；Molecular cut off is used to be respectively 5 kinds of hyperfiltration membrane assemblies of 300KD, 100KD, 30KD, 10KD, 5KD
Separating pectin, under room temperature condition, inlet pressure 70kPa, outlet pressure 30kPa, after decolouring, pectin extracting soln is through circulating pump
Be sequentially inputted in the membrane module that molecular cut off is descending, obtain after ultra-filtration and separation more than 300KD, 300KD-100KD,
100KD-30KD, 30KD-10KD, 10KD-5KD and less than 5KD six part pectin sample liquid；
7th step, is dried；Employing spray dryer is dried, by the pectin sample liquid of different component at 130 DEG C～160 DEG C of instantaneous mists
Change the pectin finished product being dried to obtain different molecular weight；Dried product sieves powder through 60 mesh sieves, i.e. obtains different molecular weight pectin
Powder.
The most according to claim 1 a kind of utilize degraded solubilization technique extraction from Fructus Jujubae Fructus Jujubae slag prepare the side of Fructus Jujubae pectin
Method, it is characterised in that the pectin selecting the hyperfiltration membrane assembly of more than 100KD to separate, obtains the molecular weight red jujube fruit more than 100KD
Glue finished product.
The most according to claim 1 a kind of utilize degraded solubilization technique extraction from Fructus Jujubae Fructus Jujubae slag prepare the side of Fructus Jujubae pectin
Method, it is characterised in that concentrating Fructus Jujubae pectin and be concentrated mainly on macromolecule part, 100KD part is above reaches more than 90%.
The most according to claim 1 a kind of utilize degraded solubilization technique extraction from Fructus Jujubae Fructus Jujubae slag prepare the side of Fructus Jujubae pectin
Method, it is characterised in that its middle-molecular-weihydroxyethyl accounts for more than 78.24% more than 300KD, and 300KD-100KD part accounts for more than 14.31%.
The most according to claim 2 a kind of utilize degraded solubilization technique extraction from Fructus Jujubae Fructus Jujubae slag prepare the side of Fructus Jujubae pectin
Method, it is characterised in that gained Fructus Jujubae pectin finished product, for faint yellow or light brown powder, loss on drying is 5.43 w% ± 0.12,
Sulfur dioxide: 32.21 mg/kg ± 0.24, acid insoluble ash: 0.73 w% ± 0.03, total galacturonic acid: 89.96 w% ±
0.64, lead: 0.35 mg/kg ± 0.02.
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| CN108912242A (en) * | 2018-07-11 | 2018-11-30 | 淮阴工学院 | A method of extracting high degree of gelation pectin from the pomelo peel of Pingshan |
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