CN107663241A - A kind of crosslinked starch of high resistant starch content and preparation method thereof - Google Patents
A kind of crosslinked starch of high resistant starch content and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of crosslinked starch of high resistant starch content and preparation method thereof, the resistance starch content of the crosslinked starch of the high resistant starch content>80%, substitution value>1.57*10‑4, reaction efficiency>70%, the crosslinked starch of the high resistant starch content is to be prepared by starch milk, carried out in microwave synthetic reaction work station made of the steps such as cross-linking reaction, centrifugation, suction filtration, washing, drying, crushing, sieving.Its resistance starch content of the crosslinked starch of the present invention is more than 80%, and substitution value is more than 1.57*10‑4, for reaction efficiency more than 70%, the increase of high resistant starch content significantly increases the healthcare function of crosslinked starch.
Description
【Technical field】
The invention belongs to technical field of modified starch, and in particular to the crosslinked starch and its system of a kind of high resistant starch content
Preparation Method.
【Background technology】
Resistant starch (Resistant Starch, RS) be it is a kind of can not be digested in the small intestine of healthy human, but energy
The starch and starch decomposition products of fermentation or Partial fermentation in large intestine.It is a variety of important that the digestion characteristics of resistant starch assign its
Physiological function, showing according to the study, resistant starch can produce some short chain fatty acids in large intestine by microbial fermentation metabolism, from
And contribute to the preventing and treating of colon cancer；Cholesterol can be effectively reduced, is advantageous to body weight control；Can preferably regulating and controlling blood sugar refer to
Number, therefore be advantageous to the preventing and treating of diabetes etc..Resistant starch is divided into by five classes according to the difference of starch property：Physically trapping forms sediment
Powder, particle resistant starch, aging starch, converted starch and starch-lipid composite starch.Converted starch (Modified
Starch) refer to the property for changing native starch using the means of physics, chemistry or enzyme, cut off, reset, aoxidized by molecule
Or substituent is introduced in starch molecule, the starch derivatives that property is optimized or possesses new property is prepared.Due to
Converted starch not only has good physiological function, also has the advantages that steady chemical structure, processing characteristics are excellent, therefore have
Good development potentiality.Cross-linking modified is a kind of conventional chemical modification method, and new chemical bond is introduced by using crosslinking agent
Make the stability of starch strengthen.Conventional crosslinking agent has expoxy propane, epoxychloropropane, sodium trimetaphosphate, calgon etc..
At present in domestic research, starch is modified using single crosslinking agent more, and uses traditional water bath heating more, these
Crosslinked starch resistance starch content prepared by method is low, time-consuming for production, power consumption is big, low production efficiency, so as to limit crosslinking
The industrialized production of starch and application.
【The content of the invention】
The invention provides a kind of crosslinked starch of high resistant starch content and preparation method thereof, to solve described problem.
To solve above technical problem, the present invention uses following technical scheme：
A kind of crosslinked starch of high resistant starch content, the resistant starch of the crosslinked starch of the high resistant starch content contain
Amount>80%, substitution value>1.57*10-4, reaction efficiency>70%.
Present invention also offers a kind of preparation method of the crosslinked starch of high resistant starch content, implement according to the following steps：
Starch and distilled water are mixed with starch emulsion A, by sodium tripolyphosphate-sodium trimetaphosphate multiple crosslinking agent, anhydrous sodium sulfate
Add in starch emulsion A, obtain starch emulsion B, adjust starch emulsion B system pH, stir, be placed on microwave synthetic reaction
Reacted in work station, after microwave reaction, the pH to 6.0-6.5 of starch emulsion is adjusted using 1mol/L HCl solution, handed over terminating
Connection reaction, is then centrifuged for, filters, washs, dries, crushes, sieves, and the crosslinked starch of high resistant starch content is made.
Preferably, the starch is potato starch.
Preferably, the starch emulsion A concentration is 28%-40%.
Preferably, the addition of the sodium tripolyphosphate-sodium trimetaphosphate multiple crosslinking agent is starch emulsion B content
10-15%, the content is in terms of starch on dry basis.
Preferably, in the sodium tripolyphosphate-sodium trimetaphosphate multiple crosslinking agent, sodium tripolyphosphate and sodium trimetaphosphate
Ratio is (1-30)：(70-99).
Preferably, the addition of the anhydrous sodium sulfate is the 8-11% of starch emulsion B content, and the content is done with starch
Base meter.
Preferably, the starch emulsion B systems pH is 9-13.
Preferably, 40~55 DEG C, microwave power 450-500W of the microwave temperature, microwave reaction time are 1-2min.
Preferably, the centrifugal rotational speed is 3000r/min.
The invention has the advantages that：
(1) crosslinked starch of the invention for preparing high resistant starch content exists using multiple crosslinking agent, multiple crosslinking agent
Play and act synergistically in cross-linking process, cross-linking reaction efficiency can be significantly improved；
(2) present invention is crosslinked using microwave equipment, and compared to traditional heating water bath equipment, microwave equipment, which has, to be added
The features such as hot uniform, speed is fast, power consumption is low；
(3) crosslinked starch being prepared with the method for the present invention, its resistance starch content are more than 80%, and substitution value is more than
1.57*10-4, for reaction efficiency more than 70%, the increase of high resistant starch content significantly increases the healthcare function of crosslinked starch；
(4) crosslinked starch being prepared with the method for the present invention, its dilation and solubility are low, heat endurance and shearing resistance
It is good to cut stability, is not susceptible to aging of bringing back to life, therefore, crosslinked starch of the invention has good processing characteristics, is handed over for broadening
The application for joining starch provides foundation.
【Embodiment】
It is specifically described with reference to specific embodiment.
Embodiment 1
Accurately weigh 25g farinas (butt) to mix with distilled water, the starch emulsion that concentration is 40% is prepared
A, by 12% sodium tripolyphosphate-sodium trimetaphosphate (sodium tripolyphosphate：Sodium trimetaphosphate=20:80) multiple crosslinking agent and 10%
Anhydrous sodium sulfate is added in starch milk, and wherein addition obtains starch emulsion B in terms of starch on dry basis, adjusts starch emulsion B bodies
It is that pH is 9, stirs, place in microwave synthetic reaction work station, react 2min at 45 DEG C, power setting 450W is micro-
In ripple course of reaction, while magnetic agitation is carried out to ensure the uniformity of heating.It is molten using 1mol/L HCl after microwave reaction
Liquid adjusts the pH to 6.0 of starch emulsion, to terminate cross-linking reaction, then centrifuges, filters, washes under 3000r/min centrifuge
Wash, dry, crush, sieve, the Crosslinked Potato Starch of high resistant starch content is made.
Embodiment 2
Accurately weigh 25g farinas (butt) to mix with distilled water, the starch milkiness that concentration is 40% is prepared
Liquid, by 10% sodium tripolyphosphate-sodium trimetaphosphate (sodium tripolyphosphate：Sodium trimetaphosphate=20:80) multiple crosslinking agent and 10%
Anhydrous sodium sulfate is added in starch milk, and wherein addition obtains starch emulsion B in terms of starch on dry basis, adjusts starch emulsion B bodies
It is that pH is 10, stirs, place in microwave synthetic reaction work station, 1.8min, power setting 500W are reacted at 50 DEG C,
During microwave reaction, while magnetic agitation is carried out to ensure the uniformity of heating.After microwave reaction, using 1mol/L HCl
Solution adjusts the pH to 6.2 of starch emulsion, to terminate cross-linking reaction, then centrifuge, filter under 3000r/min centrifuge,
Washing, drying, crush, sieving, the Crosslinked Potato Starch of high resistant starch content is made.
Embodiment 3
Accurately weigh 25g farinas (butt) to mix with distilled water, the starch milkiness that concentration is 30% is prepared
Liquid, by 10% sodium tripolyphosphate-sodium trimetaphosphate (sodium tripolyphosphate：Sodium trimetaphosphate=10:90) multiple crosslinking agent and 10%
Anhydrous sodium sulfate is added in starch milk, and wherein addition obtains starch emulsion B in terms of starch on dry basis, adjusts starch emulsion B bodies
It is that pH is 11, stirs, place in microwave synthetic reaction work station, 1.2min, power setting 500W are reacted at 50 DEG C,
During microwave reaction, while magnetic agitation is carried out to ensure the uniformity of heating.After microwave reaction, using 1mol/L HCl
Solution adjusts the pH to 6.5 of starch emulsion, to terminate cross-linking reaction, then centrifuge, filter under 3000r/min centrifuge,
Washing, drying, crush, sieving, the Crosslinked Potato Starch of high resistant starch content is made.
Embodiment 4
Accurately weigh 25g farinas (butt) to mix with distilled water, the starch milkiness that concentration is 35% is prepared
Liquid, by 12% sodium tripolyphosphate-sodium trimetaphosphate (sodium tripolyphosphate：Sodium trimetaphosphate=30:70) multiple crosslinking agent and 10%
Anhydrous sodium sulfate is added in starch milk, wherein addition in terms of starch on dry basis, obtain starch emulsion B, regulation starch emulsion B
System pH is 11, is stirred, and places in microwave synthetic reaction work station, 2min, power setting 450W are reacted at 45 DEG C,
During microwave reaction, while magnetic agitation is carried out to ensure the uniformity of heating.After microwave reaction, using 1mol/L HCl
Solution adjusts the pH to 6.5 of starch emulsion, to terminate cross-linking reaction, then centrifuge, filter under 3000r/min centrifuge,
Washing, drying, crush, sieving, the Crosslinked Potato Starch of high resistant starch content is made.
Bound phosphorus, resistance starch content, substitution value, reaction efficiency, the paste for the crosslinked starch that the present invention is prepared
The measure for changing characteristic is carried out by the following method：
(1) bound phosphorus
To understand the phosphorus content combined after crosslinking with farina molecule, using GB/T 22427-2008《Starch and its
Derivative phosphorus total content determines》In method the bound phosphorus of farina is measured.Phosphorus in crosslinked starch is total
The percentage that content accounts for sample quality with sample phosphorus gross mass represents that calculation formula is as follows：
In formula：
Δ p --- sample phosphorus total content, %；
m1--- the phosphorus quality of the sample liquid determined from standard curve, unit are microgram (μ g)；
V0--- the determined volume of sample liquid, unit are milliliter (mL)；
m0--- the quality of test specimen, unit are gram (g)；
V1--- for the aliquot volume of the sample liquid of measure, unit is milliliter (mL).
(2) resistance starch content
With reference to AOAC methods (Enzymatic Digestion Resistant Starch in Starch and Plant
Materials.Arlington,VA:Association of Official Analytical Chemists(AOAC),
2002) resistant starch of farina is digested, using 3,5- dinitrosalicylics acid system, (Xue Hui cassavas resist after enzymolysis
Property starch preparation and property research, He'nan University of Technology, 2013) glucose content is measured.
(3) substitution value
The content of phosphorus is combined in the every 100g starch of substitution value reflection, its calculation formula is as follows：
In formula：
np--- the amount (n of the material of phosphorus is combined in per 100g starchp=Δ p/31)
162 --- the molal weight of dehydrated glucose；
100 --- the quality of dried starch sample, unit g；
102——NaPO3 2-Molal weight.
(4) reaction efficiency
Reaction efficiency is worth being actual DS and theoretical DS (assuming that all there occurs anti-with starch for the whole crosslinking agents added
Should) ratio, its calculation formula is as follows：
(5) it is gelatinized property measure
Using RAPID VISCO analyzer (Rapid Visco Analyzer, RVA) to farina and crosslinked starch
Effect On Gelatinization Characteristics are measured.Prepared to obtain 10% starch milk with distilled water, be placed into after starch milk is sufficiently stirred quick viscous
Spend in analyzer, rise to 50 DEG C by room temperature and keep 1min, 95 DEG C are risen in 3.67min, keep 2.5min, be then lowered into
50 DEG C and 2min is kept, record gelatinization point, peak viscosity, MV minium viscosity, abatement value, final viscosity and the retrogradation of this process
Value.
The bound phosphorus of the crosslinked starch of table 1, resistance starch content, substitution value, reaction efficiency index
Note：Control sample in table is referred to using traditional immersion method (70 DEG C) and single crosslinking agent (sodium trimetaphosphate)
Preparation-obtained crosslinked starch.
As shown in Table 1, farina phosphorus content is 0.02%.In the crosslinked starch that embodiment 1,2,3,4 is prepared
Bound phosphorus difference it is little, but the bound phosphorus of potato ative starch is much larger than, while also greater than control sample
Bound phosphorus.But the bound phosphorus in the crosslinked starch in embodiment is below 0.4%, meets national standard and edible denaturation is formed sediment
The requirement of phosphorus is combined in powder.
As shown in Table 1, the resistance starch content of crosslinked starch prepared by embodiment 1,2,3,4 is far above farina
The crosslinked starch prepared with conventional method, show that using microwave equipment and multiple crosslinking agent obtaining for resistant starch can be significantly improved
Rate.
As shown in Table 1, the substitution value of the crosslinked starch in embodiment 1,2,3,4 and reaction efficiency are far above conventional method
The crosslinked starch of preparation, show using microwave equipment and multiple crosslinking agent can significantly improve cross-linking reaction reaction efficiency and
The substitution value of crosslinked starch.
The crosslinked starch RAPID VISCO measurement result of table 2
| Cross-linking method | Gelatinization point/DEG C | Peak viscosity/cP | MV minium viscosity/cP | Final viscosity/cP | Abatement value/cP | Recycled LDPE/cP |
| Farina | 67.8 | 4941 | 1999 | 2432 | 2942 | 433 |
| Control sample | 67.2 | 6600 | 5132 | 7546 | 1854 | 2414 |
| Embodiment 1 | 67.6 | 6998 | 6471 | 8396 | 1297 | 1925 |
| Embodiment 2 | 67.5 | 7523 | 6436 | 8434 | 1087 | 1998 |
| Embodiment 3 | 67.5 | 7886 | 6565 | 8286 | 1321 | 1721 |
| Embodiment 4 | 66.8 | 7261 | 6685 | 8176 | 576 | 1491 |
Note：Control sample in table is referred to using traditional immersion method (70 DEG C) and single crosslinking agent (sodium trimetaphosphate)
Preparation-obtained crosslinked starch.
Abatement value is the difference of peak viscosity and MV minium viscosity, as shown in Table 2, the friendship that embodiment 1,2,3,4 is prepared
The abatement value of connection starch is below the abatement value for the crosslinked starch that farina is prepared with conventional method, and this is due to hand over
The cross-bond formed in connection course of reaction between starch can make starch granules in high temperature with having been kept under shear conditions as far as possible
It is whole, the loss of viscosity is reduced, therefore relatively low abatement value means preferable heat endurance and shear stability.It is meanwhile compound
The heat endurance of crosslinked starch prepared by crosslinking agent microwave method is better than farina and conventional method system with shear stability
Standby obtained crosslinked starch.
Rise value is the difference of final viscosity and MV minium viscosity, as shown in Table 2, compared to farina, embodiment 1,
2nd, 3,4 and the rise value of crosslinked starch of control sample significantly improve, show cross-linking reaction make starch be easier to occur it is old
Change, but the rise value for the crosslinked starch being prepared in embodiment 1,2,3,4 is less than the crosslinked starch that conventional method is prepared
Rise value, show that aging less easily occurs using the crosslinked starch that is prepared of the present invention, and conventional method is prepared
Crosslinked starch be easier occur aging.
In summary it can be shown that compared with existing preparation method, method provided by the invention can obtain resistance shallow lake
The crosslinked starch of powder content, and reaction rate is fast, the time is short, energy-conserving and environment-protective.In addition, the crosslinked starch that the present invention is prepared
Heat endurance, shear resistant are preferable, have broad application prospects.
Above content is it cannot be assumed that present invention specific implementation is confined to these explanations, for the technical field of the invention
Those of ordinary skill for, under the premise of present inventive concept is not departed from, some simple deduction or replace can also be made, all should
When being considered as belonging to the scope of patent protection that is determined by the claims submitted of the present invention.
Claims (10)
- A kind of 1. crosslinked starch of high resistant starch content, it is characterised in that：The crosslinked starch of the high resistant starch content Resistance starch content>80%, substitution value>1.57*10-4, reaction efficiency>70%.
- A kind of 2. preparation method of the crosslinked starch of high resistant starch content according to claim 1, it is characterised in that：By such as Following steps are implemented：Starch and distilled water are mixed with starch emulsion A, by sodium tripolyphosphate-sodium trimetaphosphate composite crosslinking Agent, anhydrous sodium sulfate are added in starch emulsion A, obtain starch emulsion B, are adjusted starch emulsion B system pH, are stirred, and are placed Reacted in microwave synthetic reaction work station, after microwave reaction, the pH of starch emulsion is adjusted extremely using 1mol/L HCl solution 6.0-6.5, to terminate cross-linking reaction, it is then centrifuged for, filters, washs, dries, crushes, sieves, high resistant starch content is made Crosslinked starch.
- 3. the preparation method of the crosslinked starch of high resistant starch content according to claim 2, it is characterised in that：The starch For potato starch.
- 4. the preparation method of the crosslinked starch of high resistant starch content according to claim 2, it is characterised in that：The starch Latex A concentration is 28%-40%.
- 5. the preparation method of the crosslinked starch of high resistant starch content according to claim 2, it is characterised in that：The trimerization The addition of sodium phosphate-sodium trimetaphosphate multiple crosslinking agent is the 10-15% of starch emulsion B content, and the content is done with starch Base meter.
- 6. the preparation method of the crosslinked starch of high resistant starch content according to claim 2, it is characterised in that：The trimerization In sodium phosphate-sodium trimetaphosphate multiple crosslinking agent, the ratio of sodium tripolyphosphate and sodium trimetaphosphate is (1-30)：(70-99).
- 7. the preparation method of the crosslinked starch of high resistant starch content according to claim 2, it is characterised in that：It is described anhydrous The addition of sodium sulphate is the 8-11% of starch emulsion B content, and the content is in terms of starch on dry basis.
- 8. the preparation method of the crosslinked starch of high resistant starch content according to claim 2, it is characterised in that：The starch Emulsion B systems pH is 9-13.
- 9. the preparation method of the crosslinked starch of high resistant starch content according to claim 2, it is characterised in that：The microwave 40~55 DEG C, microwave power 450-500W of temperature, microwave reaction time are 1-2min.
- 10. the preparation method of the crosslinked starch of high resistant starch content according to claim 2, it is characterised in that：It is described from Heart rotating speed is 3000r/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111643730A (en) * | 2020-07-14 | 2020-09-11 | 华熙生物科技股份有限公司 | Preparation method and application of crosslinked hyaluronic acid gel for injection |
| CN111657498A (en) * | 2020-05-25 | 2020-09-15 | 华南理工大学 | High heat-resistant slowly digestible and resistant starch prepared by cell wall crosslinking and production method thereof |
| CN112176778A (en) * | 2020-09-25 | 2021-01-05 | 张淑玲 | Paper-plastic production process of one-step forming environment-friendly packaging box |
| CN113861300A (en) * | 2021-09-15 | 2021-12-31 | 华南理工大学 | Chemical cross-linked starch with slow gas production characteristic and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2771048C1 (en) * | 2020-10-29 | 2022-04-25 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Липецкий государственный технический университет" | Method for producing phosphorylated resistant starch |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111657498A (en) * | 2020-05-25 | 2020-09-15 | 华南理工大学 | High heat-resistant slowly digestible and resistant starch prepared by cell wall crosslinking and production method thereof |
| CN111643730A (en) * | 2020-07-14 | 2020-09-11 | 华熙生物科技股份有限公司 | Preparation method and application of crosslinked hyaluronic acid gel for injection |
| CN112176778A (en) * | 2020-09-25 | 2021-01-05 | 张淑玲 | Paper-plastic production process of one-step forming environment-friendly packaging box |
| CN113861300A (en) * | 2021-09-15 | 2021-12-31 | 华南理工大学 | Chemical cross-linked starch with slow gas production characteristic and preparation method and application thereof |
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