CN109180837A - A method of adjusting Ago-Gel transparency - Google Patents
A method of adjusting Ago-Gel transparency Download PDFInfo
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- CN109180837A CN109180837A CN201810730413.3A CN201810730413A CN109180837A CN 109180837 A CN109180837 A CN 109180837A CN 201810730413 A CN201810730413 A CN 201810730413A CN 109180837 A CN109180837 A CN 109180837A
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Abstract
The present invention relates to a kind of methods for adjusting Ago-Gel transparency, include the following steps: A, agarose is dissolved in deionized water, it is configured to the agarose solution that mass concentration is 3%~11% (w/v), adjusts PH to 6.5~10.5 with sodium hydroxide solution；B, enetutanedioic acid anhydride derivative is configured to succinic anhydride derivative aqueous isopropanol with the isopropanol of 5-10 times of quality, additive amount is the 1~6% of overall reaction system volume；C, succinic anhydride derivative aqueous isopropanol is added dropwise in agarose solution, it with sodium hydroxide solution maintenance system pH value is alkalescent in reaction process that control adds in 1h, is kept for 35~55 DEG C of temperature；D, pH value after reaction, is adjusted to 6.5-7.0 with hydrochloric acid solution, is washed and is dehydrated later；E, after dehydration, product is dried and is crushed, product is obtained.The more former agarose transparency of product of the invention improves, and fusion temperature, solution temperature and setting temperature reduce, and has preferable gel strength.
Description
Technical field
The present invention relates to a kind of methods for adjusting Ago-Gel transparency, belong to technical field of food biochemical industry.
Background technique
Agar is the polyose extracted from Gelidiaceae plant and fragrant plant mentioned in ancient texts section plant, mainly by agarose and a small amount of sulphur
Agar-agar composition, wherein agarose is the neutral polysaccharide part in agar, is the master for constituting agar product gel, thick stabilization property
Want ingredient.The extractive technique of agar and agarose large-scale application in industries such as food, medicine and chemical industry.Agarose with its compared with
High product purity, excellent gel characteristic and safety, in fields such as preparative separation medium, electrophoresis material, bio-microcapsules
It is widely applied.But since agar sugar product in the market is single, the product based on agarose derivative is few, greatly
Limit the further exploitation of agarose application.For it in the application of different field, the characteristic of agarose is proposed different
It is required that therefore, performing the derivatization modification to agarose, and then change the processing characteristics in its application, for widening agarose
Using having great importance.
In consideration of it, the present inventor carries out in-depth study to the above problem, there is this case generation then.
Summary of the invention
The purpose of the present invention is to provide a kind of method for adjusting Ago-Gel transparency, product made from this method exists
Higher transparency can be retained under gel state.
In order to achieve the above object, the present invention uses such technical solution:
A method of Ago-Gel transparency is adjusted, is included the following steps:
A, agarose is dissolved in deionized water, is configured to the agarose solution that mass concentration is 3%~11% (w/v),
PH to 6.5~10.5 is adjusted with sodium hydroxide solution；
B, enetutanedioic acid anhydride derivative additive amount is 1~6% (v/v) of overall reaction system volume, by alkenyl before reaction
Succinic anhydride derivative is configured to succinic anhydride derivative aqueous isopropanol with 5 times of isopropanol.
C, succinic anhydride derivative aqueous isopropanol is added dropwise in agarose solution, control adds in 1h, reacts
With sodium hydroxide solution maintenance system pH value it is alkalescent in journey, is kept for 35~55 DEG C of temperature；
D, pH value after reaction, is adjusted to 6.5-7.0 with hydrochloric acid solution, is washed and is dehydrated later；
E, after dehydration, product is dried and is crushed, product is obtained.
As a kind of preferred embodiment of the invention, the solubility of sodium hydroxide solution is 3% (w/ in step A and step C
v)。
As a kind of preferred embodiment of the invention, the solubility of hydrochloric acid solution is 1mol/L in step D.
As a kind of preferred embodiment of the invention, in step D, using successively being washed with deionized water and ethanol solution
It washs, the solubility of ethanol solution is 80% (v/v).
As a kind of preferred embodiment of the invention, drying temperature is 45 DEG C in step E.
As a kind of preferred embodiment of the invention, the enetutanedioic acid anhydride derivative is dodecenylsuccinic acid acid anhydride or pungent
Enetutanedioic acid anhydride.
In the present invention, the introducing of alkenyl long chain hinders the bonding of streptavidin agarose hydrogen bond, it is suppressed that streptavidin agarose double helix
The formation of body beam, therefore higher transparency is still remained in gel state.The high grade of transparency product of this method preparation is as one
The functional agarose derivative of kind, is the intensive processing and utilization of agarose, improves the added value of agarose, provide one
New approaches.The present invention realizes the esterification modification of agarose using solvent method, and reaction condition is mild, simple process, high-efficient, easily
In realization work.The more former agarose transparency of product of the invention improves, and fusion temperature, solution temperature and setting temperature reduce, and
With preferable gel strength, a kind of New stablization or emulsifier can be used as.
Specific embodiment
In order to further explain the technical solution of the present invention, being described in detail below with reference to embodiment.
The indication test method used in the following example:
(1) transparency measures
The mass fraction that a certain amount of sample is made into is weighed as 1% solution, is placed in boiling water bath and dissolves by heating, fall while hot
Enter in cuvette, stand overnight at room temperature, reference (setting the light transmittance of deionized water as 100%) is made with deionized water, in 700nm
The light transmittance of spectrophotometric determination sample is used under wavelength.
(2) measurement of gel strength
1.5g modified sample is weighed, 100mL deionized water is added, is made into 1.5% hot solution.Pour into three respectively while hot
In weighing bottle (high 25mm, diameter 40mm), preservative film is covered after solidification to be cooled, in 20 DEG C of placement 15h.Then gel strength is used
Analyzer measures gel strength, is averaged.
(3) measurement of setting temperature
The sample solution that compound concentration is 1.5%.10mL is taken to pour into test tube (internal diameter 15mm), by perforated rubber stopper,
It is inserted into thermometer, mercury ball is made to be completely immersed in solution.(about 1 DEG C/min) agarose solution temperature is slowly reduced, until liquid level solidifies
It is motionless.Test tube is tilted 90 ° of angles by record, and temperature when liquid level does not have a significant change when thermometer is extracted.It tests, makes even three times
Mean value, the i.e. setting temperature of sample.
(4) measurement (fusing point) of fusion temperature
The solution that compound concentration is 1.5%.It takes 15mL to pour into test tube (internal diameter 22mm), passes through perforated rubber stopper, insertion
Thermometer makes mercury ball be completely immersed in solution.It is stood overnight after solution solidification.Putting 1 diameter is the stainless shot of 3mm in gel
Surface, heating water bath slowly increase the temperature of sample gel.When recording gel melt, steel ball drops down onto the temperature of test tube bottom suddenly
Degree.Experiment is averaged three times, i.e. the fusion temperature of sample.
(5) measurement of solution temperature
0.15g sample is weighed in 10mL test tube, 10mL deionized water is then added, after mixing evenly beyond the Great Wall with glass bar
Test tube plug is placed in water-bath, is heated up with the speed of 1 DEG C/15min, and the dissolution situation of sample in temperature-rise period is observed, until
It shakes test tube to adhere to without particle, solution clear, the as solution temperature of sample.
(6) measurement of viscosity
With deionized water product configuration at the solution of 1.5% (w/v), DV-C (No. 1 rotor, 50rpm) viscosity is used at 80 DEG C
Meter measurement solution viscosity (MPas) stablizes 30s and reads and record.
Embodiment 1:
It weighs 6g agarose to mix with appropriate amount of deionized water, 3% (w/v) agarose solution is made into, with 3% sodium hydroxide
The pH for adjusting solution is 8.5, under conditions of magnetic agitation, with constant pressure separatory funnel by 8mL dodecenylsuccinic acid acid anhydride (by it
It is diluted in the isopropanol of 5 times of volumes) it is slowly added dropwise into agarose solution, control adds in 1h, with 3% in reaction process
Sodium hydroxide solution maintenance system pH value be 8.5, keep 40 DEG C of temperature, mixing speed 350rpm, react 3h.To the end of reacting
Afterwards, system pH is adjusted to 6.5 or so with the hydrochloric acid solution of 1mol/L, is successively washed with deionized water and ethanol solution, set 45 DEG C
Drying in oven, and by after drying product crush, be sieved to get to white lipolysaccharide derivative.After measured, gel strength
223.3g/cm2, 31 DEG C of setting temperature, 62.3 DEG C of fusion temperature, 84.6 DEG C of solution temperature, transparency 94.5%, viscosity
7.77Mpa·s.
Embodiment 2:
It weighs 22g agarose to mix with appropriate amount of deionized water, 11% (w/v) agarose solution is made into, with 3% hydroxide
The pH that sodium adjusts lotion is 8.5, and under conditions of magnetic agitation, 8mL octenyl succinic anhydride (is added dropwise with constant pressure separatory funnel
Before, the octenyl succinic anhydride of 8mL is diluted in the isopropanol of 40mL, similarly hereinafter) it is slowly added dropwise into agarose solution, it controls
Added in 1h, in reaction process with 3% sodium hydroxide solution maintenance system pH value be 8.5, keep 40 DEG C of temperature, stirring speed
350rpm is spent, 3h is reacted.To after reaction, system pH is adjusted to 6.5 or so with the hydrochloric acid solution of 1mol/L, successively spend from
Sub- water and ethanol solution washing, set 45 DEG C of drying in oven, and the product after drying is crushed, is sieved to get the fine jade of white is arrived
Lipolysaccharide derivative.After measured, gel strength 338.2g/cm2, 33 DEG C of setting temperature, 71.8 DEG C of fusion temperature, solution temperature 89.8
DEG C, transparency 84.4%, viscosity 7.96Mpas.
Embodiment 3:
It weighs 10g agarose to mix with appropriate amount of deionized water, 5% (w/v) agarose solution is made into, with 3% hydroxide
The pH that sodium adjusts lotion is 6.5, under conditions of magnetic agitation, with constant pressure separatory funnel by 8mL octenyl succinic anhydride (by it
It is diluted in the isopropanol of 5 times of volumes) it is slowly added dropwise into agarose solution, control adds in 1h, with 3% in reaction process
Sodium hydroxide solution maintenance system pH value be 6.5, keep 40 DEG C of temperature, mixing speed 350rpm, react 3h.To the end of reacting
Afterwards, it is successively washed with deionized water and ethanol solution, sets 45 DEG C of drying in oven, and the product after drying crushed, sieving, i.e.,
Obtain the agarose derivative of white.After measured, gel strength 692.8g/cm2, 37 DEG C of setting temperature, 81 DEG C of fusion temperature, molten
93.2 DEG C of temperature of solution, transparency 79.2%, viscosity 8.7Mpas.
Embodiment 4:
It weighs 10g agarose to mix with appropriate amount of deionized water, 5% (w/v) agarose solution is made into, with 3% hydroxide
The pH that sodium adjusts lotion is 10.5, (will by 8mL octenyl succinic anhydride with constant pressure separatory funnel under conditions of magnetic agitation
In its isopropanol for being diluted in 5 times of volumes) it is slowly added dropwise into agarose solution, control adds in 1h, uses in reaction process
3% sodium hydroxide solution maintenance system pH value is 10.5, is kept for 40 DEG C of temperature, mixing speed 350rpm, reacts 3h.Wait react
After, system pH is adjusted to 6.5 or so with the hydrochloric acid solution of 1mol/L, is successively washed, is set with deionized water and ethanol solution
45 DEG C of drying in oven, and by after drying product crush, be sieved to get to white agarose derivative.After measured, gel
Intensity 751.6g/cm2, 37.5 DEG C of setting temperature, 82 DEG C of fusion temperature, 94.6 DEG C of solution temperature, transparency 72.9%, viscosity
8.86Mpa·s.
Embodiment 5:
It weighs 10g agarose to mix with appropriate amount of deionized water, 5% (w/v) agarose solution is made into, with 3% hydroxide
The pH that sodium adjusts lotion is 8.5, under conditions of magnetic agitation, with constant pressure separatory funnel by 2mL octenyl succinic anhydride (by it
It is diluted in the isopropanol of 5 times of volumes) it is slowly added dropwise into agarose solution, control adds in 1h, with 3% in reaction process
Sodium hydroxide solution maintenance system pH value be 8.5, keep 40 DEG C of temperature, mixing speed 350rpm, react 3h.To the end of reacting
Afterwards, system pH is adjusted to 6.5 or so with the hydrochloric acid solution of 1mol/L, is successively washed with deionized water and ethanol solution, set 45 DEG C
Drying in oven, and by after drying product crush, be sieved to get to white agarose derivative.Pungent after measured, gel is strong
Spend 692.8g/cm2, 37 DEG C of setting temperature, 81 DEG C of fusion temperature, 93.2 DEG C of solution temperature, transparency 79.2%, viscosity
8.7Mpa·s.
Embodiment 6:
It weighs 10g agarose to mix with appropriate amount of deionized water, 5% (w/v) agarose solution is made into, with 3% hydroxide
The pH that sodium adjusts lotion is 8.5, (will by 12mL octenyl succinic anhydride with constant pressure separatory funnel under conditions of magnetic agitation
In its isopropanol for being diluted in 5 times of volumes) it is slowly added dropwise into agarose solution, control adds in 1h, uses in reaction process
3% sodium hydroxide solution maintenance system pH value is 8.5, is kept for 40 DEG C of temperature, mixing speed 350rpm, reacts 3h.Wait react
After, system pH is adjusted to 6.5 or so with the hydrochloric acid solution of 1mol/L, is successively washed, is set with deionized water and ethanol solution
45 DEG C of drying in oven, and by after drying product crush, be sieved to get to white agarose derivative.After measured, gel
Intensity 171.7g/cm2, 29.7 DEG C of setting temperature, 58.6 DEG C of fusion temperature, 82.7 DEG C of solution temperature, transparency 97.5%, viscosity
7.54Mpa·s.
Embodiment 7:
It weighs 10g agarose to mix with appropriate amount of deionized water, 5% (w/v) agarose solution is made into, with 3% hydroxide
The pH that sodium adjusts lotion is 8.5, under conditions of magnetic agitation, with constant pressure separatory funnel by 8mL octenyl succinic anhydride (by it
It is diluted in the isopropanol of 5 times of volumes) it is slowly added dropwise into agarose solution, control adds in 1h, with 3% in reaction process
Sodium hydroxide solution maintenance system pH value be 8.5, keep 35 DEG C of temperature, mixing speed 350rpm, react 3h.To the end of reacting
Afterwards, system pH is adjusted to 6.5 or so with the hydrochloric acid solution of 1mol/L, is successively washed with deionized water and ethanol solution, set 45 DEG C
Drying in oven, and by after drying product crush, be sieved to get to white agarose derivative.After measured, gel strength
576.0g/cm2, 34 DEG C of setting temperature, 74.2 DEG C of fusion temperature, 92.6 DEG C of solution temperature, transparency 81.3%, viscosity
8.26Mpa·s.
Embodiment 8:
It weighs 10g agarose to mix with appropriate amount of deionized water, 5% (w/v) agarose solution is made into, with 3% hydroxide
The pH that sodium adjusts lotion is 8.5, under conditions of magnetic agitation, with constant pressure separatory funnel by 8mL octenyl succinic anhydride (by it
It is diluted in the isopropanol of 5 times of volumes) it is slowly added dropwise into agarose solution, control adds in 1h, with 3% in reaction process
Sodium hydroxide solution maintenance system pH value be 8.5, keep 55 DEG C of temperature, mixing speed 350rpm, react 3h.To the end of reacting
Afterwards, system pH is adjusted to 6.5 or so with the hydrochloric acid solution of 1mol/L, is successively washed with deionized water and ethanol solution, set 45 DEG C
Drying in oven, and by after drying product crush, be sieved to get to white agarose derivative.After measured, gel strength
234.3g/cm2, 30.6 DEG C of setting temperature, 63.6 DEG C of fusion temperature, 83.6 DEG C of solution temperature, transparency 91.4%, viscosity
7.76Mpa·s.
In the present invention, 1% (w/v) indicates that agarose containing 1g (solute) in 100ml deionized water, 1% (v/v) indicate
Solute containing 1ml in 100ml solvent.Wherein agarose, sodium hydroxide solution are in terms of (w/v), and concentration of alcohol is in terms of (v/v).
Product form of the invention is not limited to the present embodiment, anyone carries out suitably changing or repair for similar thinking to it
Decorations, all should be regarded as not departing from patent category of the invention.
Claims (6)
1. a kind of method for adjusting Ago-Gel transparency, which comprises the steps of:
A, agarose is dissolved in deionized water, is configured to the agarose solution that mass concentration is 3%~11% (w/v), uses hydrogen
Sodium hydroxide solution adjusts PH to 6.5~10.5；
B, enetutanedioic acid anhydride derivative additive amount is 1~6% (v/v) of overall reaction system volume, by allyl butyrate two before reaction
Anhydride ester derivs are configured to succinic anhydride derivative aqueous isopropanol with 5 times of isopropanol.
C, succinic anhydride derivative aqueous isopropanol is added dropwise in agarose solution, control adds in 1h, in reaction process
It is alkalescent with sodium hydroxide solution maintenance system pH value, is kept for 35~55 DEG C of temperature；
D, pH value after reaction, is adjusted to 6.5-7.0 with hydrochloric acid solution, is washed and is dehydrated later；
E, after dehydration, product is dried and is crushed, product is obtained.
2. a kind of method for adjusting Ago-Gel transparency as described in claim 1, it is characterised in that: step A and step C
The solubility of middle sodium hydroxide solution is 3% (w/v).
3. a kind of method for adjusting Ago-Gel transparency as claimed in claim 2, it is characterised in that: hydrochloric acid in step D
The solubility of solution is 1mol/L.
4. a kind of method for adjusting Ago-Gel transparency as claimed in claim 3, it is characterised in that: in step D, use
It is successively washed with deionized water and ethanol solution, the solubility of ethanol solution is 80% (v/v).
5. a kind of method for adjusting Ago-Gel transparency as claimed in claim 4, it is characterised in that: dried in step E
Temperature is 45 DEG C.
6. such as a kind of method for adjusting Ago-Gel transparency described in any one of claim 1 to 5, it is characterised in that: institute
Stating enetutanedioic acid anhydride derivative is dodecenylsuccinic acid acid anhydride or octenyl succinic anhydride.
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| CN109942727A (en) * | 2019-04-23 | 2019-06-28 | 福建省绿麒食品胶体有限公司 | A kind of preparation method and applications with pH responsiveness agar |
| CN110003362A (en) * | 2019-04-23 | 2019-07-12 | 福建省绿麒食品胶体有限公司 | A kind of preparation method of the modified agar of high grade of transparency high-gel strength |
| CN110003361A (en) * | 2019-04-23 | 2019-07-12 | 绿新（福建）食品有限公司 | A kind of preparation method of high-quality agar |
| CN110479184A (en) * | 2019-08-05 | 2019-11-22 | 华侨大学 | A kind of agar glycosyl emulsifier and its preparation method and application |
| CN111995699A (en) * | 2020-09-18 | 2020-11-27 | 集美大学 | Method for preparing agarose |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109942727A (en) * | 2019-04-23 | 2019-06-28 | 福建省绿麒食品胶体有限公司 | A kind of preparation method and applications with pH responsiveness agar |
| CN110003362A (en) * | 2019-04-23 | 2019-07-12 | 福建省绿麒食品胶体有限公司 | A kind of preparation method of the modified agar of high grade of transparency high-gel strength |
| CN110003361A (en) * | 2019-04-23 | 2019-07-12 | 绿新（福建）食品有限公司 | A kind of preparation method of high-quality agar |
| CN110003361B (en) * | 2019-04-23 | 2021-11-09 | 绿新（福建）食品有限公司 | Preparation method of high-quality agar |
| CN110479184A (en) * | 2019-08-05 | 2019-11-22 | 华侨大学 | A kind of agar glycosyl emulsifier and its preparation method and application |
| CN110479184B (en) * | 2019-08-05 | 2021-09-07 | 华侨大学 | Agarose-based emulsifier and preparation method and application thereof |
| CN111995699A (en) * | 2020-09-18 | 2020-11-27 | 集美大学 | Method for preparing agarose |
| CN111995699B (en) * | 2020-09-18 | 2022-07-19 | 集美大学 | Method for preparing agarose |
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