CN102250259A - Low-crosslinking sweet potato starch phosphate and preparation method thereof - Google Patents

Low-crosslinking sweet potato starch phosphate and preparation method thereof Download PDF

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CN102250259A
CN102250259A CN 201110152924 CN201110152924A CN102250259A CN 102250259 A CN102250259 A CN 102250259A CN 201110152924 CN201110152924 CN 201110152924 CN 201110152924 A CN201110152924 A CN 201110152924A CN 102250259 A CN102250259 A CN 102250259A
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sweet potato
potato starch
starch
phosphoric acid
acid ester
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郑桂富
王永斌
张斌
马龙
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郑桂富
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Abstract

The invention relates to a low-crosslinking sweet potato starch phosphate of which the substitution value is (3.92-7.01)*10<-3>. The preparation method comprises the steps of crosslinking reaction between starch and crosslinking agent, filtration, water washing, drying and the like, wherein the starch is sweet potato starch, and the crosslinking agent is sodium trimetaphosphate; the ratio of the sweet potato starch to the sodium trimetaphosphate in parts by weight is (45-50):1; the crosslinking reaction conditions are as follows: the pH value is 10-12, and the temperature is 30-50 DEG C; and when the phosphorus content of the reaction product in the crosslinking reaction process is 0.075-0.134%, the crosslinking reaction is terminated. The low-crosslinking sweet potato starch phosphate has the advantages of fine thermal stability, gelation performance and freeze-thawing stability, low phosphorus content and no toxicity, is a good gelata, emulsifier, thickener and stabilizer for the food industry, and is applicable to different foods. When the existing pectin, gelatin and other raw materials are replaced with the low-crosslinking sweet potato starch phosphate, the material cost of food processing can be lowered, the competitive power of enterprises can be enhanced, and a new way can be found out for the deep processing of the sweet potato starch. The preparation method of the low-crosslinking sweet potato starch phosphate has the advantages of simple process and less equipment, thereby facilitating the industrial popularization.

Description

A kind of low cross-linking sweet potato starch phosphoric acid ester and preparation method thereof
Technical field
The present invention relates to a kind of low cross-linking sweet potato starch phosphoric acid ester and preparation method thereof.
Background technology
Starch is carried out sex change be meant the character of utilizing chemistry, physics or other method to change native starch (ative starch), it is more suitable in the requirement of using.Ative starch product of gained after sex change is called modified starch.
With starch be mixed in stir in the water oyster white, opaque suspension, be called starch milk.Stop to stir starch milk, starch then slowly precipitates.The reason that this phenomenon occurs is big and be insoluble to cold water and cause because of starch granules density.With the starch milk heating, be in the at first water-swelling of starch molecule of amorphous domain, and the crystallization Shu Yin that is in the starch granules has elasticity, still can keep grain pattern.Along with the rising of temperature and increasing of absorption moisture, the volume of starch granules expands gradually, when reaching certain temperature, contacts with each other between the starch granules of high level expansion, becomes translucent sticking silk fabric pasty state, is called starch paste.This phenomenon that is transformed into starch paste by starch milk is called gelatinization.Starch paste is not real solution, and it is that the starch granules of high level expansion is insoluble colloid and exists, but some amylose starch is dissolved in the water.
The temperature of starch generation gelatinization is called gelatinization point.Starch nearly all be form with starch paste in Applications in Food Industry, and the viscosity of starch paste is an important index.
Native starch is stuck with paste after cryogenic freezing, and intermolecular hydrogen bonding power is just recovered gradually, and starch molecule becomes new pencil crystalline structure, thereby the catabiosis of starch has taken place.Age of starch can influence food tissue structure and quality, and native starch can not become good food gelifying agent.
The freeze-thaw stability of starch paste is meant that starch paste after freezing after a while, take out and melts the character that still can keep original colloidal structure.Good freeze-thaw stability is extremely important character for the starch paste of using in the frozen product.
The starch paste of using in frozen product, requirement be long period freezing at low temperatures, perhaps multiple freezing, melt, food still can keep original weave construction and not change.
Along with the fast development of industrial production technology, in the existing food-processing, what need is the modified starch with good thermal stability, gellifying property and freeze-thaw stability performance.Some character of ative starch can not satisfy the requirement of new installation and novel process operational condition, needs denaturing treatment, guarantees good effect.As: food-processing is more and more uses Refrigeration Technique, but the ative starch paste after freezing the retrogradation phenomenon can take place, and destroy the colloidal structure of food, thereby ative starch can not satisfy the requirement of these products.
In the existing food-processing, the large usage quantity of pectin, the agent of gelatin isogel, but the price of products such as pectin, gelatin is higher, thus strengthened the raw materials cost of food.
Summary of the invention
Technical problem to be solved by this invention provides a kind of low cross-linking sweet potato starch phosphoric acid ester with good thermal stability, gellifying property and freeze-thaw stability performance; A kind of preparation method of this low cross-linking sweet potato starch phosphoric acid ester is provided simultaneously, and this method technology is simple, and use equipment is few, is convenient to industrialization promotion.
For solving the problems of the technologies described above, the invention provides a kind of low cross-linking sweet potato starch phosphoric acid ester, this low cross-linking sweet potato starch phosphoric acid ester is prepared by the method that comprises following processing step: starch and linking agent are carried out crosslinking reaction, filtration, washing, drying and other steps, described starch is sweet potato starch, described linking agent is a Trisodium trimetaphosphate, can make described low cross-linking sweet potato starch phosphoric acid ester, its substitution value is (3.92-7.01) * 10 -3
For solving the problems of the technologies described above, the present invention also provides a kind of preparation method of low cross-linking sweet potato starch phosphoric acid ester, it comprises carries out crosslinking reaction, filtration, washing, drying and other steps with starch and linking agent, described starch is sweet potato starch, described linking agent is a Trisodium trimetaphosphate, can make described low cross-linking sweet potato starch phosphoric acid ester, its substitution value is (3.92-7.01) * 10 -3
Among the preparation method of low cross-linking sweet potato starch phosphoric acid ester of the present invention:
Described sweet potato starch is (45-50) with the ratio of the weight part of Trisodium trimetaphosphate: 1.
The condition of described crosslinking reaction: the pH value is that 10-12, temperature are 30-50 ℃, when the phosphorus content of reaction product in the crosslinking reaction process is 0.075-0.134%, finishes crosslinking reaction.
Adopt described crosslinking reaction condition, can obtain the low cross-linking sweet potato starch phosphoric acid ester that degree of crosslinking is lower, satisfy the food service industry needs.
The optimal conditions of described crosslinking reaction: the pH value is 10.2, temperature is 50 ℃, when the phosphorus content of reaction product in the crosslinking reaction process is 0.111%, finishes crosslinking reaction.
The performance of the sweet potato starch phosphoric acid ester that finishes crosslinking reaction under these conditions and make is best, is suitable as emulsifying agent, thickening material and the stablizer of foodstuffs industry most.
Starch reacts with the chemical reagent with two or more functional groups, forms etherificate or esterification key between the hydroxyl of different starch molecules and crosslinked, and the derivative of gained is called cross-linking starch.All have two or more functional groups, and can both be used as linking agent with the chemical reagent that two or more hydroxyls in the starch molecule react.Because Trisodium trimetaphosphate itself has three functional groups, nontoxicity and stability are not high, so the present invention adopts Trisodium trimetaphosphate as linking agent.
The chemical reaction that starch and Trisodium trimetaphosphate form cross-linking starch is an esterification process, and the principal reaction equation is:
Figure BDA0000066996480000031
The by product trisodium phosphate of above-mentioned crosslinking reaction can also play esterification with starch and generate starch phosphate one ester:
The NaH that this reaction generated 2PO 4Can play esterification with starch again and generate starch phosphate one ester:
Figure BDA0000066996480000033
By above reaction equation as can be seen, with the Trisodium trimetaphosphate is that the cross-linking starch (starch-phosphate) that linking agent is produced should mainly be the mixture of starch phosphate one ester and starch phosphate diester, but theoretically, also may contain a spot of starch phosphate three esters.
Use the Trisodium trimetaphosphate cross-linking starch, prepare in the process of starch-phosphate, with the carrying out of crosslinking reaction in the method for the invention, starch milk viscosity increases gradually, starch milk viscosity reaches maximum behind certain hour, continues to prolong cross-linking reaction time, and then the viscosity of starch milk begins to descend.The crosslinking degree of sweet potato starch phosphoric acid ester increases with the prolongation in reaction times.Test shows, when reaction is carried out can getting highly cross-linked sweet potato starch phosphoric acid ester when 20h is above, and also not gelatinization of boiling water heating.
The substitution value of sweet potato starch phosphoric acid ester is directly proportional with its phosphorus content.Along with the growth of cross-linking reaction time, the phosphorus content of sweet potato starch phosphoric acid ester constantly increases.It should be noted that in the sweet potato ative starch and contain phosphorus that by analysis, phosphorus content is 0.035% in the sweet potato ative starch.The relation of the phosphorus content of the cross-linking reaction time of sweet potato starch and sweet potato starch phosphoric acid ester sees Table 1.Data from table 1 can find out that along with the growth of cross-linking reaction time, the phosphorus content of sweet potato starch phosphoric acid ester constantly increases.
Table 1
Figure BDA0000066996480000034
As seen, the big ball that is shaped as of sweet potato ative starch is joining a plurality of beads on one's body from Fig. 1-1 and Fig. 1-2.After further study, these beads form in the starch granules developmental process, contact comparatively closely, and are face contact, and under the effect of external force such as stirrings, grinding, obscission is also not obvious on one's body from big ball for these beads.
Can find that by Fig. 2-1 and Fig. 2-2 the bead quantity that is associated on the one hand on the big spheroid reduces, and has occurred less indenture on the other hand on spherome surface.After these phenomenons showed the reaction of sweet potato ative starch and Trisodium trimetaphosphate, having taken place at the regional area of particle surface can obvious observed variation.Simultaneously, owing to sweet potato ative starch particle causes separating between large and small spheroid with chemical reaction between Trisodium trimetaphosphate.Isolating reason between large and small spheroid occurring, may be microsphere with big spheroid is former linked to each other by intermolecular hydrogen bond before this, when between Trisodium trimetaphosphate and starch molecule during the generation crosslinking reaction, and original hydrogen bond rupture, thus cause the separation of large and small spheroid.
Can find that by Fig. 3-1 and Fig. 3-2 bead that is associated on the big spheroid all comes off.On the bead that splits away off and original big spherome surface, all can find out tangible indenture, and these phenomenons are more more obvious than performance among Fig. 2-1 and Fig. 2-2, and this has supported that further the variation and the separation between large and small spheroid that are taken place about the sweet potato starch particle surface are because the deduction that chemical reaction caused between sweet potato starch particle and Trisodium trimetaphosphate.
From Fig. 4-1 and Fig. 4-2 as can be seen, the microsphere that originally was connected on the big spheroid in the sweet potato starch phosphoric acid ester particle almost completely comes off.
From Fig. 5-1-Fig. 5-4 as can be seen, the sweet potato ative starch is after Trisodium trimetaphosphate is crosslinked, and formed low cross-linking sweet potato starch phosphoric acid ester particulate polarisation cross is clear and easy to see.Therefore, low cross-linking sweet potato starch phosphoric acid ester particulate ordered structure remains unchanged, and in other words, after Trisodium trimetaphosphate and sweet potato ative starch are cross-linked to form the sweet potato starch phosphoric acid ester, does not obviously destroy its particulate crystalline structure.
The low cross-linking sweet potato starch phosphoric acid ester that makes according to preparation method of the present invention has following characteristics:
1, has good thermal stability.
Viscosity measurement used in the present invention: accurately take by weighing butt sample 27.00g, it is 450g (mass concentration ω=6%) that adding distilled water makes its total mass, mix and be placed in the Erlenmeyer flask, begin to heat up from room temperature, temperature rise rate is controlled to be 1.5 ℃/min, be warming up to 95 ℃, measure the viscosity behind 95 ℃ and the 95 ℃ insulation 30min respectively, and then be cooled to 50 ℃ and measure 50 ℃ and the 50 ℃ viscosity after being incubated 30min respectively with the rate of temperature fall of 1.5 ℃/min.
The viscosity data that the sweet potato ative starch of mass concentration ω=6% and low cross-linking starch-phosphate thereof are stuck with paste sees Table 2.Can find out that from table 2 behind insulation 30min under 95 ℃ and 50 ℃, compare with the viscosity variation that the sweet potato ative starch is stuck with paste, the viscosity variation that low cross-linking sweet potato starch phosphoric acid ester is stuck with paste is less; Simultaneously, with the reduction of temperature, the viscosity that low cross-linking sweet potato starch phosphoric acid ester is stuck with paste raises very fast.Therefore, low cross-linking sweet potato starch phosphoric acid ester is compared with the sweet potato ative starch, has the stability of better heat paste and cold paste, and this just provides more wide space for low cross-linking sweet potato starch phosphoric acid ester in Application in Food Industry.
Table 2
Annotate: μ t: the viscosity in the time of t ℃; μ t*: the viscosity behind t ℃ of insulation 30min
2, has good gellifying property.
Studies show that the internal cause that forms gel is that shape of molecule has asymmetry, shape of molecule is more asymmetric, forms gel more easily.Sweet potato ative starch and linking agent Trisodium trimetaphosphate are generated the low cross-linking starch-phosphate through suitable after crosslinked.When crosslinked, at least two hydroxyls in linking agent and per two the adjacent starch molecules react, like this, different starch molecule cross bracings is got up, add the phosphate group of new introducing, both increase the hydrophilic ability of starch molecule, increased the asymmetry of molecule again, thereby improved the gel stability of starch paste greatly.
Gelometry: accurately take by weighing a certain amount of starch sample in the 100mL beaker, adding distil water is made into certain density starch milk, heating 20min makes its complete gelatinization in boiling water bath, taking-up is left standstill to room temperature and is put into thermostat container, taking out behind the storage 16h under 10 ℃ of conditions, with the hand beaker that reverses, take out gelinite, estimate its elasticity, transparency, the square glass plate that with the length of side is 2.25cm again is the end, progressively adds counterweight, the maximum weight (g) that can bear when measuring gelinite to debacle, be gel-strength, the gel-strength judgement criteria sees Table 3.
Table 3
Figure BDA0000066996480000052
2.1 the concentration of low cross-linking sweet potato starch phosphoric acid ester is to the influence of gel-strength
Accurately weighing sweet potato starch phosphoric acid ester 6.00,7.00,8.00,9.00,10.00,11.00,12.00g put into the 100mL beaker respectively, then, carry out gel-strength according to above-mentioned gelometry and measure, and measurement result is seen Fig. 6.
Sweet potato starch phosphoric acid ester (DS=5.81 * 10 -3) mass concentration and the comprehensive evaluation of gel situation see Table 4.
Table 4
From Fig. 6 and table 4 as can be seen, sweet potato starch phosphoric acid ester (DS=5.81 * 10 -3) gel-strength increase with starch concentration, and both are roughly linear.The reason that this phenomenon occurs is that the intensity that has increased gel networks causes owing to the increase along with starch content in the starch paste.
2.2pH value is to the influence of the gel-strength of low cross-linking sweet potato starch phosphoric acid ester paste
Native starch is stuck with paste owing to the fragility of granule does not have gelation.The sweet potato ative starch is after Trisodium trimetaphosphate is crosslinked, and formed low cross-linking sweet potato starch phosphoric acid ester is stuck with paste has gelation preferably.Owing to use the food of gelifying agent often to be sour environment, therefore be necessary to study of the influence of pH value to the gel-strength of low cross-linking sweet potato starch phosphoric acid ester paste.
The pH value to the research method of the gel-strength influence that low cross-linking sweet potato starch phosphoric acid ester is stuck with paste is: at first, prepare the buffer system of different pH values, then, accurately take by weighing 10.00g low cross-linking sweet potato starch phosphoric acid ester respectively and put into the 200mL beaker, the buffered soln that adds different pH values, the starch-phosphate of the different pH of preparation mass concentration ω=10% is stuck with paste, and carries out gel-strength according to above-mentioned gelometry then and measures.
The pH value sees Table 5 to the test-results of the gel-strength influence that low cross-linking sweet potato starch phosphoric acid ester is stuck with paste.
Table 5
As can be seen from Table 5, the formed gel of low cross-linking sweet potato starch phosphoric acid ester all can stable existence under acid, neutral, weak basic condition, and intensity height, performance are good.
Test shows that the formed starch paste of sweet potato ative starch is all unstable in whole process, and this is a little less than being highly brittle because of the native starch granule, in water, will disintegrate through heating continuously or stirring, thus strength degradation; And through the crosslinked formed low cross-linking sweet potato starch phosphoric acid ester of Trisodium trimetaphosphate, owing to have the existence of cross-link bond, make the starch granule just so not fragile, frangible, and shearing, high temperature and the acid destruction that causes are had stronger resistivity, thereby show intensity height, the good stability of gel.
2.3 the gel-strength that ionogen and low cross-linking sweet potato starch phosphoric acid ester are stuck with paste relation
Accurately take by weighing some parts of 10.00g low cross-linking sweet potato starch phosphoric acid ester, put into the 200mL beaker respectively, the electrolyte solution that adds different concns then successively, use the distilled water constant volume, make that electrolyte concentration reaches 0.10,0.20,0.30,0.40 respectively, 0.50mol/L, low cross-linking sweet potato starch phosphoric acid ester mass concentration ω=10%, pH value of solution=7 are carried out gel-strength according to above-mentioned gelometry then and are measured.
The test-results of the gel-strength relation that ionogen and low cross-linking sweet potato starch phosphoric acid ester are stuck with paste is shown in Table 6.Ionogen mainly shows on the negatively charged ion the influence of gel strength.As can be seen from Table 6, putting in order of negatively charged ion gel-strength influence that low cross-linking sweet potato starch phosphoric acid ester is stuck with paste is C 4H 4O 6 2->C 6H 5O 7 3->CH 3COO ->Cl ->NO 3 ->Br ->I -
Table 6
Figure BDA0000066996480000071
Said sequence is consistent with these ionic hydratabilities.Test finds that for ionogen of the same race, when electrolyte concentration was less than or equal to 0.30mol/L in the system, various ionogen all can impel the sweet potato starch phosphoric acid ester to stick with paste the formation of gel.This is because of the increase with electrolyte concentration, and the hydration of electrolyte ion itself strengthens, and has increased reticulated structure, so gel-strength strengthens.When electrolyte concentration during greater than 0.30mol/L, continue to increase electrolytical concentration, then the sweet potato starch phosphoric acid ester gel-strength of sticking with paste descends, and this is owing to electrolytical salting out causes.
Usually, electrolytical concentration is all lower in the food raw material, and therefore, the ionogen in the food is little to the influence of the gel-strength of low cross-linking sweet potato starch phosphoric acid ester.
2.4 the relation of the gel-strength that nonelectrolyte and low cross-linking sweet potato starch phosphoric acid ester are stuck with paste
Accurately take by weighing some parts of 10.00g low cross-linking sweet potato starch phosphoric acid ester, put into the 200mL beaker respectively, in different beakers, add successively then 2.00,4.00,6.00,8.00,10.00 with the different nonelectrolytes of 12.00g, use the distilled water constant volume, make the mass concentration of various nonelectrolytes reach 2%, 4%, 6%, 8%, 10% and 12% respectively, low cross-linking sweet potato starch phosphoric acid ester mass concentration ω=10%, pH value of solution=7 are carried out gel-strength according to above-mentioned gelometry then and are measured.
Several different nonelectrolytes and low cross-linking sweet potato starch phosphoric acid ester (DS=5.81 * 10 -3) relation of gel-strength is as shown in table 7.
Table 7
Figure BDA0000066996480000081
As can be seen from Table 7, along with the adding of various nonelectrolytes, the variation in strength of gel in the system is not obvious, and the gained gel all is strong gel, and its elasticity and stability are all better.Therefore, the gel property influence that nonelectrolyte such as widely used various carbohydrates is stuck with paste low cross-linking sweet potato starch phosphoric acid ester in the foodstuffs industry is less.
3, has good freeze-thaw stability performance.
The testing method of freeze-thaw stability generally be with starch paste through cryogenic freezing for some time, heat up again thaw after, observe it and can keep original gel form, repeated multiple times is until gel layering bleed.The number of times of freeze thawing is many more, shows that the freeze-thaw stability of starch paste is good more.
Testing method used in the present invention is: take by weighing a certain amount of sweet potato starch, the starch milk of furnishing mass concentration ω=6%, in boiling water bath, heat gelatinization, be cooled to room temperature, pour in the plastic cup, after adding a cover, put into-15 ℃ freezer compartment of refrigerator, freezing diel (24 hours) takes out under room temperature and thaws naturally, observes the stability state of sticking with paste.Then, put into again refrigerator freezing repeatedly, thaw, till the colloidal structure of sticking with paste destroys (have in the colloidal structure clear water separate out or become spongy).Write down freezing and number of times that thaw.The freeze-thaw stability of sticking with paste is represented with the freezing number of times of aforesaid operations.
The sweet potato starch phosphoric acid ester is stuck with paste the freezing number of times under the pH=7 condition, lists in the table 8.
Table 8
Figure BDA0000066996480000082
As can be seen from Table 8, the freeze-thaw stability of sweet potato starch phosphoric acid ester paste changes with the variation of substitution value.When low degree of substitution, along with the increase of substitution value, freezing number of times increases, and when substitution value continued to increase, freezing number of times descended on the contrary.In the substitution value scope of being studied, the freeze-thaw stability that the sweet potato starch phosphoric acid ester is stuck with paste is stronger than its ative starch.
The reason that above-mentioned phenomenon occurs is under the situation than low crosslinking degree, owing to the crosslinked sweet potato starch molecular weight that makes between the sweet potato starch molecule suitably increases, in the process of heating gelatinization, the sweet potato starch molecular chain is fully unfolded, and easily forms the netted gel structure of stable and stereoscopic.In addition, the bound phosphate groups that modified-reaction is introduced in the sweet potato starch molecule is a hydrophilic radical, also is to hinder gel to separate out the major cause of free-water.Therefore, the freeze-thaw stability of low cross-linking sweet potato starch phosphoric acid ester paste improves with the increase of substitution value.But when substitution value continued to increase, then crosslinking reaction became obviously to the restraining effect of sweet potato starch gelatinization, and the extent of hydration of sweet potato starch molecule is weakened, thereby the freeze-thaw stability that sweet potato starch is stuck with paste reduces.Further studies show that, when crosslinking degree acquires a certain degree, because the intensity of the formed chemical bond of crosslinking reaction is far above hydrogen bond, strengthened the intensity of sweet potato starch grain pattern, thereby suppress described particulate expansion, gelatinization, when this restraining effect is strengthened to a certain degree, can suppress described particle and in boiling water, expand, make it can not gelatinization.
The freeze-thaw stability of starch paste also can be by examining the aspects such as elasticity, shaping situation and synersis situation of sticking with paste.Table 9 sticks with paste for the sweet potato ative starch of mass concentration ω=6% and sweet potato starch phosphoric acid ester paste is preserved 24h in-15 ℃ refrigerator-freezer, after taking-up is thawed, by the aspects such as elasticity, shaping situation and synersis situation of corresponding paste being carried out the result of comprehensive evaluation.
Table 9
Figure BDA0000066996480000091
The shown test-results of table 9 is consistent with the test-results of table 8, and they all show, DS=5.81 * 10 -3The sweet potato starch phosphoric acid ester have good freeze-thaw stability.
In sum, low cross-linking sweet potato starch phosphoric acid ester of the present invention has good thermal stability, gellifying property and freeze-thaw stability performance, its phosphorus content is low, nontoxic, is good gelifying agent, emulsifying agent, thickening material and the stablizer of foodstuffs industry, is suitable for using in the different foods.Use low cross-linking sweet potato starch phosphoric acid ester of the present invention to replace raw materials such as existing pectin, gelatin, can reduce the raw materials cost of food-processing, strengthen enterprise competitiveness.The yield of sweet potato of China is higher, uses the present invention to find a new outlet as the deep processing of sweet potato starch.The preparation method of low cross-linking sweet potato starch phosphoric acid ester of the present invention, its technology is simple, and use equipment is few, is convenient to industrialization promotion.
Sweet potato starch described in the preparation method of the present invention, Trisodium trimetaphosphate are commercially available product.
Description of drawings
Photo when Fig. 1-the 1st, sweet potato ative starch particle amplify 300 times under scanning electronic microscope.
Fig. 1-2 is the photo of sweet potato ative starch particle when amplifying 3000 times under scanning electronic microscope.
Fig. 2-the 1st, substitution value are 3.92 * 10 -3The photo of sweet potato starch phosphoric acid ester particle when under scanning electronic microscope, amplifying 2500 times.
Fig. 2-the 2nd, substitution value are 3.92 * 10 -3The photo of sweet potato starch phosphoric acid ester particle when under scanning electronic microscope, amplifying 3500 times.
Fig. 3-the 1st, substitution value are 5.81 * 10 -3The photo of sweet potato starch phosphoric acid ester particle when under scanning electronic microscope, amplifying 2500 times.
Fig. 3-the 2nd, substitution value are 5.81 * 10 -3The photo of sweet potato starch phosphoric acid ester particle when under scanning electronic microscope, amplifying 3500 times.
Fig. 4-the 1st, substitution value are 7.01 * 10 -3The photo of sweet potato starch phosphoric acid ester particle when amplifying 300 times.
Fig. 4-the 2nd, substitution value are 7.01 * 10 -3The photo of sweet potato starch phosphoric acid ester particle when amplifying 3000 times.
Fig. 5-the 1st, sweet potato ative starch form photo under polarizing microscope.
Fig. 5-the 2nd, substitution value are 3.92 * 10 -3The form photo of sweet potato starch phosphoric acid ester under polarizing microscope.
Fig. 5-the 3rd, substitution value are 5.81 * 10 -3The form photo of sweet potato starch phosphoric acid ester under polarizing microscope.
Fig. 5-the 4th, substitution value are 7.01 * 10 -3The form photo of sweet potato starch phosphoric acid ester under polarizing microscope.
Fig. 6 is that substitution value is 5.81 * 10 -3The mass concentration of sweet potato starch phosphoric acid ester and the test-results of gel-strength relation.
Embodiment
Below can further be well understood to the present invention by embodiment given below.But they are not limitation of the invention.
Embodiment one:
Get the 160g sweet potato starch, add the solution of winning in the water of the 325mL be dissolved with the 3.3g Trisodium trimetaphosphate, the pH value of this solution is adjusted into 10.2 with sodium carbonate solution (5mol/L), get second solution, second solution is heated to 50 ℃ and make it at 50 ℃, carry out crosslinking reaction under the whipped state, when the phosphorus content of reaction product in the crosslinking reaction process is 0.111%, finish crosslinking reaction, adopt horizontal scraper discharging centrifuge to filter to reaction product then, centrifuge speed is 1550-2600r/min, the filter residue that filtration is obtained is washed then, pH value to filter residue is 6.7 o'clock, under 75-80 ℃ of condition filter residue is carried out drying, can obtain substitution value is 5.81 * 10 -3Low cross-linking sweet potato starch phosphoric acid ester.
Embodiment two:
Get the 148.5g sweet potato starch, add the solution of winning in the water of the 325mL be dissolved with the 3.3g Trisodium trimetaphosphate, the pH value of this solution is adjusted into 11.0 with sodium carbonate solution (5mol/L), get second solution, second solution is heated to 30 ℃ and make it at 30-50 ℃, carry out crosslinking reaction under the whipped state, when the phosphorus content of reaction product in the crosslinking reaction process is 0.075%, finish crosslinking reaction, adopt horizontal scraper discharging centrifuge to filter to reaction product then, centrifuge speed is 1550-2600r/min, the filter residue that filtration is obtained is washed then, pH value to filter residue is 6.7 o'clock, under 75-80 ℃ of condition filter residue is carried out drying, can obtain substitution value is 3.92 * 10 -3Low cross-linking sweet potato starch phosphoric acid ester.
Embodiment three:
Get the 165g sweet potato starch, add the solution of winning in the water of the 325mL be dissolved with the 3.3g Trisodium trimetaphosphate, the pH value of this solution is adjusted into 12.0 with sodium carbonate solution (5mol/L), get second solution, second solution is heated to 40 ℃ and make it at 30-50 ℃, carry out crosslinking reaction under the whipped state, when the phosphorus content of reaction product in the crosslinking reaction process is 0.134%, finish crosslinking reaction, adopt horizontal scraper discharging centrifuge to filter to reaction product then, centrifuge speed is 1550-2600r/min, the filter residue that filtration is obtained is washed then, pH value to filter residue is 6.7 o'clock, under 75-80 ℃ of condition filter residue is carried out drying, can obtain substitution value is 7.01 * 10 -3Low cross-linking sweet potato starch phosphoric acid ester.
Above-described only is three kinds of embodiments of the present invention.Should be pointed out that for the person of ordinary skill of the art under the prerequisite that does not break away from the principle of the invention, can also make conspicuous some conversion or alternative and remodeling, these also should be considered as belonging to protection scope of the present invention.

Claims (5)

1. the preparation method of a low cross-linking sweet potato starch phosphoric acid ester, comprise starch and linking agent are carried out crosslinking reaction, filtration, washing, drying and other steps, it is characterized in that: described starch is sweet potato starch, described linking agent is a Trisodium trimetaphosphate, can make described low cross-linking sweet potato starch phosphoric acid ester, its substitution value is (3.92-7.01) * 10 -3
2. the preparation method of a kind of low cross-linking sweet potato starch phosphoric acid ester according to claim 1 is characterized in that: described sweet potato starch is (45-50) with the ratio of the weight part of Trisodium trimetaphosphate: 1.
3. the preparation method of a kind of low cross-linking sweet potato starch phosphoric acid ester according to claim 1 and 2, it is characterized in that: the condition of described crosslinking reaction: the pH value is 10-12, temperature is 30-50 ℃, when the phosphorus content of reaction product in the crosslinking reaction process is 0.075-0.134%, finish crosslinking reaction.
4. the preparation method of a kind of low cross-linking sweet potato starch phosphoric acid ester according to claim 3, it is characterized in that: the condition of described crosslinking reaction: the pH value is 10.2, temperature is 50 ℃, when the phosphorus content of reaction product in the crosslinking reaction process is 0.111%, finish crosslinking reaction.
5. according to the low cross-linking sweet potato starch phosphoric acid ester of the preparation method of each described a kind of low cross-linking sweet potato starch phosphoric acid ester of claim 1 to 4 preparation.
CN 201110152924 2011-06-08 2011-06-08 Low-crosslinking sweet potato starch phosphate and preparation method thereof Pending CN102250259A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102987183A (en) * 2012-12-10 2013-03-27 上海大学 Starch-pectin composite and preparation method thereof
CN103122035A (en) * 2013-03-21 2013-05-29 河南科技学院 Starch phosphate with high viscidity stability and preparation method thereof
CN111163645A (en) * 2017-10-03 2020-05-15 罗盖特公司 Glass-like noodles made from low-crosslinked pea starch
CN114933661A (en) * 2022-06-27 2022-08-23 上海交通大学 Preparation method of sodium trimetaphosphate crosslinked starch

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN1545916A (en) * 2003-12-03 2004-11-17 西南农业大学 Production method of potato species micropore amylum

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN1545916A (en) * 2003-12-03 2004-11-17 西南农业大学 Production method of potato species micropore amylum

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102987183A (en) * 2012-12-10 2013-03-27 上海大学 Starch-pectin composite and preparation method thereof
CN102987183B (en) * 2012-12-10 2014-12-31 上海大学 Starch-pectin composite and preparation method thereof
CN103122035A (en) * 2013-03-21 2013-05-29 河南科技学院 Starch phosphate with high viscidity stability and preparation method thereof
CN111163645A (en) * 2017-10-03 2020-05-15 罗盖特公司 Glass-like noodles made from low-crosslinked pea starch
CN114933661A (en) * 2022-06-27 2022-08-23 上海交通大学 Preparation method of sodium trimetaphosphate crosslinked starch
CN114933661B (en) * 2022-06-27 2022-12-20 上海交通大学 Preparation method of sodium trimetaphosphate crosslinked starch

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