CN101935355B - Preparation method of high-content resistant starch - Google Patents
Preparation method of high-content resistant starch Download PDFInfo
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- CN101935355B CN101935355B CN2010102464854A CN201010246485A CN101935355B CN 101935355 B CN101935355 B CN 101935355B CN 2010102464854 A CN2010102464854 A CN 2010102464854A CN 201010246485 A CN201010246485 A CN 201010246485A CN 101935355 B CN101935355 B CN 101935355B
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Abstract
The present invention relates to a preparation method of high-content resistant starch. The invention aims to solve the technical problems of selecting a new cross-linking reagent, shortening reaction time, reducing reagent amount and cost and increasing product yield. The preparation method comprises the following steps of: (1) adding 0.5-3 percent of inorganic acid into starch milk with starch content of 35-42 percent, stirring, and neutralizing by using alkali until a pH value is 5.0-7.5; (2) adding 1-5 percent of salt into the debranching starch milk, regulating a pH value of 10.0-11.5 by using alkali, slowly stirring, adding 0.01-0.10 percent of phosphorus oxychloride, and regulating a pH value of 5.5-7.5 to obtain crosslinked starch filter cake; (3) pasting; (4) cooling a pasted substance to room temperature, then, refrigerating the pasted substance for 8-16 hours at the temperature of 0-4 DEG C or stirring the pasted substance for 6 to 8 hours at the temperature of 4 DEG C, and cooling the pasted substance to the room temperature; and (5) filtering, drying, crashing and screening to obtain the product.
Description
Technical field
The present invention relates to the preparation method of a kind of high-content Resistant starch (RS).This method is a raw material with common starch, and the method that combines by physics and chemical modification prepares high-load Resistant starch (RS).
Background technology
Starch is carbohydrate important in the human diet, also is the main source of needed by human body energy.For a long time, starch is considered to always and can be digested fully in human body, and up to 1981, Anderson found that first starch in the food is by small intestine and not by complete digestion.Nineteen eighty-three, Britain physiologist Flans Englyst at first is defined as this part starch " Resistant starch (Resistant Starch is called for short RS) ".Grain dense tissue in the world's was defined as it " non-absorbent starch and degraded product thereof in normal health person's small intestine in 1992.”
Studies show that the food that adds Resistant starch has better outward appearance, quality, local flavor and taste than the food that adds traditional food fibre.The particulate Resistant starch can improve the swelling property and the fragility of some food, especially Resistant starch has more importantly physiological function than traditional food fibre to HUMAN HEALTH: as lose weight, relax bowel, the controlling blood sugar balance, control " three height ", diseases such as prevention gallbladdergallstonecholetithiasis and duodenal ulcer.
U.S. Pat 3,729,380, European patent EP-A-0564893, EP-A-0688872 all adopt the debranching factor method to carry out enzyme and handle, and be used for reducing the ratio of amylopectin, but the resistant starch content of gained generally are no more than 60%; Chinese patent CN101555286A discloses and has a kind ofly prepared Resistant starch with orthophosphoric acid salt by esterification, and the resistant starch content of gained is more than 75%; It is raw material that Chinese patent CN1740202A discloses with the W-Gum, makes the synthetic indigestibility starch of linking agent single stage method with Trisodium trimetaphosphate, and wherein the indigestibility starch content is 85%, but entire reaction technology need be more than 30 hours, and energy consumption is bigger; Other are as preparation methods such as extruding puffing method, microwave bulking method more complicated all, and the Resistant starch yield is low.
Summary of the invention
The technical issues that need to address of the present invention are: select new cross-linking reagent, shorten the reaction times, reduce reagent dosage, reduce cost, improve the product yield.
The preparation method of high-content Resistant starch of the present invention (RS) is characterized in that as follows:
1) starch is taken off in preparation: it is 35 ~ 42% starch milk that starch is made into starch content, under 30 ~ 40 ℃ of temperature, normal pressure, add the mineral acid of (in dry starch) 0.5% ~ 3%, stirred 1 ~ 4 hour, be neutralized to obtain taking off behind pH=5.5 ~ 7.5 with alkali then and prop up a starch milk; Described starch comprises W-Gum, tapioca (flour), yam starch etc., and described mineral acid is selected from hydrochloric acid, sulfuric acid, phosphoric acid, boric acid, sodium hydrogen phosphate, and described alkali is selected from sodium hydroxide, yellow soda ash, sodium bicarbonate, salt of wormwood, saleratus;
2) the crosslinked starch filter cake of preparation: in taking off a starch milk, add 1% ~ 5% salt (in dry starch), described salt is selected from sodium-chlor, sodium sulfate, sal epsom, vitriolate of tartar; Use adjusting PH with base=10.0 ~ 11.5 then, slowly stir and add 0.01% ~ 0.10% phosphorus oxychloride (in dry starch) down, at room temperature stirring reaction is 1 ~ 6 hour, is neutralized to pH=5.5 ~ 7.5, after filtration and washing with alkali again, obtains crosslinked starch filter cake;
3) gelatinization: crosslinked starch filter cake is added the starch milk that water is made into (in dry starch) 35% ~ 42%,, make Resistant starch (RS) and stick with paste 95 ~ 120 ℃ of following gelatinizations of temperature 2 ~ 5 hours;
4) freezing: the Resistant starch (RS) that obtains is stuck with paste, is inserted in the container, be cooled to room temperature after, then or insert 0 ℃ ~ 4 ℃ freezing 8 ~ 16 hours of refrigeration chamber, perhaps keep stirring 6 ~ 8 hours at 4 ℃ refrigeration chamber, at room temperature placed again 4 ~ 6 hours;
5) at last after filtration, dry, pulverize, sieving obtains Resistant starch (RS) product.
In the step 1), acid can make the starch polymer chain rupture become many glucose units, is similar to amylose starch.Take off the side reaction principle as shown in the formula:
Step 2) principle of crosslinking as shown in the formula:
。
Product of the present invention can be used in the bakeries such as bread, biscuit, cookies, cake, substitutes 30% ~ 40% flour or wheat-flour, thereby strengthens the physiological function of this based food, and common food is promoted to protective foods, reaches the effect of fat-reducing, diseases prevention.
The present invention compared with prior art has following advantage:
(1) broken through external RS commonly used
1, RS
2, RS
3, RS
4The preparation method, with RS
3Physically modified and RS
4Chemical modification combine, the content of total dietary fiber is brought up to more than 86%;
(2) adopt freezing stirring, quickened the aging crystallisation process of starch, shortened the process time;
(3) adopt phosphorus oxychloride as cross-linking reagent, compare as cross-linking reagent with the phosphoric acid salt (comprising Trisodium trimetaphosphate, tripoly phosphate sodium STPP, Sodium hexametaphosphate 99 etc.) of routine, shortened the reaction times greatly, and reagent dosage is little, cost is lower.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Following experimental procedure is applied among the whole embodiment:
The assay of Resistant starch: get 1g Resistant starch sample and be dissolved in the phosphate buffer solution of 20ml pH=6.0, add high temperature resistant α-amylase (320U) 30min that in 90 ℃ of constant temperature oscillators, vibrates, centrifugal 10 ~ 15 min of 3000rpm, remove supernatant liquor, the acetate-sodium acetate buffer and the 0.1ml glucuroide (10000U/ml) that add 20 ml pH=5.0,60 ℃ of water-bath vibration 30min, centrifugal, remove supernatant liquor, wash centrifugal (3 times repeatedly), add 4mol/l KOH dissolving, adjust pH=6.0, add high temperature resistant α-amylase (320U) 30min that in 90 ℃ of constant temperature oscillators, vibrates, cooling, adjust pH=5.0, add the 0.1ml glucuroide, 60 ℃ of water-bath vibration 1h, wash centrifugal repeatedly, collect supernatant liquor, be settled to 100 ml, adopt 3,5-dinitrosalicylic acid method is measured reducing sugar, and the result takes advantage of 0.9 content that is Resistant starch (RS).
Embodiment 1
1) 100 parts of W-Gums add 170 parts of water and stir, and add the hydrochloric acid of 1 part of 2mol/l then, remain on 30 ℃ of following stirring reactions 3 hours, then make with the alkali neutralization and take off a starch;
2) taking off in the starch milk above-mentioned, stir 0.002 part of sodium-chlor of adding protective material down, is 4% sodium hydroxide solution accent PH=10.0 then with concentration, then slowly adds 0.02 part of phosphorus oxychloride, keeps about PH=10.0 stirring reaction 3 hours.After reaction finishes, through neutralization, filtration and washing, obtain crosslinked starch filter cake again;
3) will obtain crosslinked starch filter cake, and drop into again in the reactor, and add the starch milk of water furnishing 38%, and be heated to 100 ℃, gelatinization 3 hours makes Resistant starch (RS) and sticks with paste, and then puts into plastic tank, is cooled to room temperature;
4) with chilled starch paste, insert 4 ℃ freezing 12 hours of refrigeration chamber, at room temperature placed again 4 hours;
5) at last after filtration, dry, pulverize, sieving obtains Resistant starch (RS) finished product, resistant starch content is 86.3% after measured.
Embodiment 2
1) 100 portions of tapioca (flour)s add 170 parts of water and stir, and add the hydrochloric acid of 2 parts of 2mol/l then, remain on 35 ℃ of following stirring reactions 3 hours, and then make and take off a starch with the alkali neutralization,
2) taking off in the starch milk above-mentioned, stir 0.002 part of sodium sulfate of adding protective material down, is 4% sodium carbonate solution accent PH=10.5 then with concentration, then slowly adds 0.03 part of phosphorus oxychloride, keeps about PH=10.5 stirring reaction 4 hours.After reaction finishes, through neutralization, filtration and washing, obtain crosslinked starch filter cake again,
3) will obtain crosslinked starch filter cake, and drop into again in the reactor, and add the starch milk of water furnishing 39%, and be heated to 110 ℃, gelatinization 3 hours makes Resistant starch (RS) and sticks with paste, and then puts into wooden barrel, is cooled to room temperature,
4) with chilled starch paste, the refrigeration chamber of inserting 4 ℃ stirred 8 hours fast, at room temperature placed again 6 hours,
5) at last after filtration, dry, pulverize, sieving obtains Resistant starch (RS) finished product, resistant starch content is 86.6% after measured.
Embodiment 3
1) 100 parts of yam starchs add 160 parts of water and stir, and add the sulfuric acid of 0.5 part of 2mol/l then, remain on 40 ℃ of following stirring reactions 2 hours, then make with the alkali neutralization and take off a starch;
2) taking off in the starch milk above-mentioned, stir 0.003 part of sodium-chlor of adding protective material down, is 4% sodium hydroxide solution accent PH=11.0 then with concentration, then slowly adds 0.05 part of phosphorus oxychloride, keeps about PH=11.0 stirring reaction 2 hours.After reaction finishes, through neutralization, filtration and washing, obtain the cross-linking starch filter cake again;
3) will obtain crosslinked starch filter cake, and drop into again in the reactor, and add the starch milk of water furnishing 40%, and be heated to 115 ℃, gelatinization 3 hours makes Resistant starch (RS) and sticks with paste, and then puts into wooden barrel, is cooled to room temperature;
4) with chilled starch paste, the refrigeration chamber of inserting 4 ℃ stirred 10 hours fast, at room temperature placed 6 hours again;
5) at last after filtration, dry, pulverize, sieving obtains Resistant starch (RS) finished product, resistant starch content is 87.0% after measured.
Embodiment 4
1) 100 parts of W-Gums add 150 parts of water and stir, and add the sulfuric acid of 0.5 part of 2mol/l then, remain on 30 ℃ of following stirring reactions 4 hours, then make with the alkali neutralization and take off a starch;
2) taking off in the starch milk above-mentioned, stir 0.005 part of sodium-chlor of adding protective material down, is 4% sodium hydroxide solution accent PH=11.5 then with concentration, then slowly adds 0.08 part of phosphorus oxychloride, keeps about PH=11.5 stirring reaction 6 hours.After reaction finishes, through neutralization, filtration and washing, obtain the cross-linking starch filter cake again;
3) will obtain crosslinked starch filter cake, and drop into again in the reactor, and add the starch milk of water furnishing 41%, and be heated to 95 ℃, gelatinization 4 hours makes Resistant starch (RS) and sticks with paste, and then puts into plastic tank, is cooled to room temperature;
4) with chilled starch paste, place 0 ℃ freezing 16 hours of refrigeration chamber, at room temperature placed again 5 hours;
5) at last after filtration, dry, pulverize, sieving obtains Resistant starch (RS) finished product, resistant starch content is 87.9% after measured.
Embodiment 5
1) 100 parts of yam starchs add 140 parts of water and stir, and add the phosphoric acid of 1.5 parts of 2mol/l then, remain on 35 ℃ of following stirring reactions 2 hours, then make with the alkali neutralization and take off a starch;
2) taking off in the starch milk above-mentioned, stir 0.004 part of sodium-chlor of adding protective material down, is 4% sodium hydrogen carbonate solution accent PH=11.2 then with concentration, then slowly adds 0.1 part of phosphorus oxychloride, keeps about PH=11.2 stirring reaction 3 hours.After reaction finishes, through neutralization, filtration and washing, obtain the cross-linking starch filter cake again;
3) will obtain crosslinked starch filter cake, and drop into again in the reactor, and add the starch milk of water furnishing 42%, and be heated to 100 ℃, gelatinization 4 hours makes Resistant starch (RS) and sticks with paste, and then puts into plastic tank, is cooled to room temperature;
4) with chilled starch paste, place 0 ℃ freezing 14 hours of refrigeration chamber, at room temperature placed again 5 hours;
5) at last after filtration, dry, pulverize, sieving obtains Resistant starch (RS) finished product, resistant starch content is 87.5% after measured.
Claims (2)
1. the preparation method of a high-content Resistant starch is characterized in that as follows:
1) starch is taken off in preparation: it is 35~42% starch milk that starch is made into starch content, under 30~40 ℃ of temperature, normal pressure, adding was stirred 1~4 hour in the mineral acid of dry starch 0.5%~3%, was neutralized to alkali then and obtained taking off a starch milk behind pH=5.5~7.5;
2) the crosslinked starch filter cake of preparation: in taking off a starch milk, adding is in the salt of dry starch 1%~5%, use adjusting PH with base=10.0~11.5 then, slowly stir the phosphorus oxychloride that adds down in dry starch 0.01%~0.10%, at room temperature stirring reaction is 1~6 hour, again with alkali be neutralized to pH=5.5~7.5, after filtration and the washing, obtain crosslinked starch filter cake;
3) gelatinization: crosslinked starch filter cake is added water be made into starch milk,, make Resistant starch (RS) and stick with paste 95~120 ℃ of following gelatinizations of temperature 2~5 hours in dry starch 35%~42%;
4) freezing: the Resistant starch that obtains is stuck with paste, is inserted in the container, be cooled to room temperature after, then or insert 0 ℃~4 ℃ freezing 8~16 hours of refrigeration chamber, perhaps keep stirring 6~8 hours at 4 ℃ refrigeration chamber, at room temperature placed again 4~6 hours;
5) at last after filtration, dry, pulverize, sieving obtains resistant starch product.
2. the preparation method of high-content Resistant starch according to claim 1, it is characterized in that the described starch of step 1) is selected from W-Gum, tapioca (flour), yam starch, described mineral acid is selected from hydrochloric acid, sulfuric acid, phosphoric acid, boric acid, and described alkali is selected from sodium hydroxide, yellow soda ash, salt of wormwood, saleratus; Step 2) described salt is selected from sodium-chlor, sodium sulfate, sal epsom, vitriolate of tartar.
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