CN101319053A - Method for preparing fatty acid stephanoporate starch ester and application thereof - Google Patents
Method for preparing fatty acid stephanoporate starch ester and application thereof Download PDFInfo
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- CN101319053A CN101319053A CNA2008101244972A CN200810124497A CN101319053A CN 101319053 A CN101319053 A CN 101319053A CN A2008101244972 A CNA2008101244972 A CN A2008101244972A CN 200810124497 A CN200810124497 A CN 200810124497A CN 101319053 A CN101319053 A CN 101319053A
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Abstract
The invention relates to a method for preparing fatty acid porous starch ester and an application of the fatty acid porous starch ester, belonging to the modified starch technical field. The method performs enzymolysis on native starch at first to prepare porous starch, and then performs acidolysis and esterification for composition of modified starch, so as to prepare fatty acid porous starch ester products with low degree of substitution. The products have strong adsorptivity which is greatly improved compared with porous starch prepared by single acidolysis and starch ester prepared by single esterification, and can be applied in various fields of foodstuff, for example, the products can be used as a microcapsule material and used as an absorbent for absorbing various functional substances such as pennyroyal, edible essence, pigment, olive oil, probiotics and so on. By adoption of the fatty acid porous starch ester for absorbing a target substance, the function of slow release can be reached and the service efficiency can be improved. The method has the advantages that: the method takes the porous starch as a raw material and performs secondary esterification modification on the porous starch with strong adsorptivity; the whole reaction process is simple to operate and easy to implement and has small environmental pollution; and the products prepared have superior performance.
Description
Technical field
A kind of preparation method of fatty acid stephanoporate starch ester and application are carried out enzymolysis to ative starch earlier, are prepared into porous-starch, then carry out acidolysis and esterification composite modified starch, belong to technical field of modified starch.
Technical background
Fatty acid starch ester is the esterified prod that is obtained by starch and derivative thereof and lipid acid, fatty acid methyl ester, lipid acid acyl chlorides or fatty acid anhydride reaction.Because the introducing of the organic carbochain of hydrophobicity, the hydrophobicity of esterification starch increases, and can improve its absorption property greatly.It can be applied in a plurality of fields in the food, as doing the microcapsule material, is used as sorbent material etc.Also less to the porous-starch being that raw material carries out the report of modification once more, having only usefulness phosphorus oxychloride such as Xu Zhong is that linking agent prepares the esterification and crosslinking porous-starch, and Liu Xiong etc. is an esterifying agent esterification porous-starch etc. with the dodecenylsuccinic anhydride.And about being esterifying agent with the longer chain fatty acid, porous-starch yet there are no report so far for the denatured technology of the synthetic stearic acid stephanoporate starch ester of raw material dry method.
Summary of the invention
The objective of the invention is: providing a kind of is raw material with starch, is prepared into porous-starch by the prozyme effect, is raw material again with the porous-starch then, and the method for esterification synthetic fatty acid stephanoporate starch ester at high temperature directly takes place for lipid acid and porous-starch.Owing in reaction, add acid as catalyzer, can make porous-starch acidolysis in reaction process, thereby help the introducing of longer chain fatty acid.The solvent of dehydrated alcohol as esterifying agent used in this reaction, under stirring condition can with the porous-starch thorough mixing, after stoving process in, dehydrated alcohol can volatilize fully, can not cause any detrimentally affect to reaction.
Technical scheme of the present invention: a kind of preparation method of fatty acid stephanoporate starch ester,
(1) first enzymolysis ative starch is prepared into porous-starch: take by weighing ative starch by prescription, Sodium phosphate dibasic-the citrate buffer solution that adds most pH 4.6 in the prescription is sized mixing, take by weighing saccharifying enzyme and α-Dian Fenmei and be made into prozyme liquid with damping fluid remaining in the prescription, saccharifying enzyme wherein: the volume ratio of α-Dian Fenmei consumption is 3: 1, prozyme liquid is all transferred to stirring reaction 24h in the starch suspension, add the sodium hydroxide stopped reaction, gained suspension is centrifugal, centrifugal back gained starch is also centrifugal with distilled water wash, place 50 ℃ of loft drier to be dried to constant weight gained starch, pulverize with pulverizer, promptly get porous-starch; Described prescription is:
Ative starch is in butt quality 100g
Damping fluid, by volume 200mL
Prozyme liquid, by volume 15～20mL
(2) acidolysis then and esterification modification porous-starch: with the porous-starch is raw material, esterifying agent is dissolved in the anhydrous ethanol solvent of heat, add acid by prescription, slowly add to the esterifying agent that is dissolved in alcohol solvent in the porous-starch, constantly stir, after the slurry that obtains is crossed 10 mesh sieves, dry ethanol down in 50 ℃, regulating moisture content is 18%～24%, obtains uniform mixed reactant; Described prescription is:
Above-mentioned self-control porous-starch is in butt quality 100g
Dehydrated alcohol, by volume 60～100mL
Esterifying agent is in butt quality 2～4g
Acid, 0.02～0.10g in mass
Water is used to regulate moisture content, by volume 0～50mL
(3) dry process reaction: the mixed reactant that obtains places pressure kettle, or places electric drying oven with forced convection, adopts high temperature to react, and temperature of reaction is 130～150 ℃, and the reaction times is 3～5h.
Ative starch is selected W-Gum, wheat starch, Starch rice or potato starch for use.
Glucoamylase enzyme in the prozyme liquid is lived and is that it is 3000U/mL that 20000U/mL, α-Dian Fenmei enzyme live.
The esterifying agent that is used for the esterification sex change is a longer chain fatty acid, selects stearic acid, lauric acid, oleic acid, linolic acid, palmitinic acid or eicosanoic acid for use.
The catalyst acid that is used for acid hydrolysis is hydrochloric acid or acetic acid.
The application of the fatty acid stephanoporate starch ester of preparation is used as the various specific functional substance of adsorbents adsorb: as some composition in the spearmint oil in the food, pigment, fish oil and makeup and the medicine, to reach slow releasing function, prolong action effect.
Enzyme digestion reaction is to carry out at normal temperatures and pressures, and esterification then is to carry out under hot conditions.In dried preparation composite modified starch process, add acid as catalyzer, at high temperature carry out esterification, because acid hydrolysis makes porous-starch molecule in the easier replacement of lipid acid, make product have higher absorption property.
Beneficial effect of the present invention: the present invention is directed to the singularity requirement of food-processing industry, developed a kind of new production process and product innovation of modified starch targetedly to modified starch.Utilize prozyme to act on ative starch and prepare porous-starch, with dry method porous-starch is carried out acidolysis and esterification sex change then, in the porous-starch molecule, introduce longer chain fatty acid.Product has good characteristic aspect absorption property, the porous-starch molecule is because the introducing of long-chain fat acid groups, replace original hydrophilic oh group, the hydrophobicity of product increases, on the basis of original porous-starch because of the increase adsorptivity raising of specific area, absorption property further increases, the material that can make microcapsule is used for the micro encapsulation product, also can be used as the various specific functional substance of adsorbents adsorb such as some composition in the spearmint oil in the food, pigment, fish oil and makeup and the medicine, to reach slow releasing function, prolong action effect.This technology is dry method esterification porous-starch, and reaction process is simple to operate, and is easy to implement, and environmental pollution is little.
Description of drawings
Fig. 1 dried preparation fatty acid stephanoporate starch ester process schematic representation.
Embodiment
Embodiment 1: take by weighing 100g (butt) W-Gum, placing 170mL pH value is that 4.6 Sodium phosphate dibasics-citrate buffer solution is sized mixing, measure 15mL prozyme liquid simultaneously, be made into enzyme liquid with the 30mL damping fluid, pour stirring reaction 24h in the starch suspension into, add the sodium hydroxide stopped reaction, the centrifugal supernatant liquor of removing, washing is also dry, pulverizes, and promptly gets the porous-starch sample.
Take by weighing the 3g stearic acid, be dissolved in 60 ℃ of dehydrated alcohols of 60mL, slowly add in the 100g porous-starch (butt), add 0.06g hydrochloric acid, stir, obtain uniform mixture slurry, sieve, oven dry ethanol, adding water adjusting moisture massfraction is 20%, and the gained mixed reactant is placed pressure kettle, under 130 ℃, carry out esterification 3h, cooling is pulverized, and promptly gets stearic acid corn porous starch ester.
With prepared stearic acid stephanoporate starch ester and porous-starch, the ative starch performance compares, and sees Table 1.
The comparison of three kinds of starch oil absorbencies of table 1 and specific surface area
As can be seen from Table 1, significantly improve than porous-starch by the oil absorbency that porous-starch is carried out after the esterification treatment without esterification treatment.Owing to the effect of enzymolysis, the porous-starch particle surface forms a lot of micropores simultaneously, thereby specific surface area increases; And the stearic acid stephanoporate starch ester is because the adding of acid in reaction process has certain Degradation to starch, so specific surface area is bigger than porous-starch.
Embodiment 2: take by weighing 100g (butt) W-Gum, placing 160mL pH value is that 4.6 Sodium phosphate dibasics-citrate buffer solution is sized mixing, measure 18mL prozyme liquid simultaneously, be made into enzyme liquid with the 40mL damping fluid, pour stirring reaction 24h in the starch suspension into, add the sodium hydroxide stopped reaction, the centrifugal supernatant liquor of removing, washing is also dry, pulverizes, and promptly gets the porous-starch sample.
Take by weighing the 3g stearic acid, be dissolved in 60 ℃ of dehydrated alcohols of 60mL, slowly add in the 100g porous-starch (butt), add 0.1g acetic acid, stir, obtain uniform mixture slurry, sieve, oven dry ethanol, adding water adjusting moisture massfraction is 20%, and the gained mixed reactant is placed pressure kettle, under 130 ℃, carry out esterification 3h, cooling is pulverized, and promptly gets stearic acid corn porous starch ester.
Embodiment 3
With the W-Gum is raw material, and stearic acid is an esterifying agent, 150 ℃ of esterification reaction temperatures, and all the other prescriptions and operational condition make finished product stearic acid porous W-Gum ester with embodiment 1 or embodiment 2.
Embodiment 4
With the W-Gum is raw material, and stearic acid is an esterifying agent, reaction time of esterification 5h, and all the other prescriptions and operational condition make finished product stearic acid porous W-Gum ester with embodiment 1 or embodiment 2.
Embodiment 5
With the wheat starch is raw material, and stearic acid is an esterifying agent, and all the other prescriptions and operational condition make finished product stearic acid porous wheat starch ester with embodiment 1 or embodiment 2.
Embodiment 6
Use lauric acid as esterifying agent, W-Gum is a raw material, and all the other prescriptions and operational condition make finished product lauric acid porous W-Gum ester with embodiment 1 or embodiment 2.
Claims (6)
1. the preparation method of a fatty acid stephanoporate starch ester is characterized in that
(1) first enzymolysis ative starch is prepared into porous-starch: take by weighing ative starch by prescription, Sodium phosphate dibasic-the citrate buffer solution that adds most pH 4.6 in the prescription is sized mixing, take by weighing saccharifying enzyme and α-Dian Fenmei and be made into prozyme liquid with damping fluid remaining in the prescription, saccharifying enzyme wherein: the volume ratio of α-Dian Fenmei consumption is 3: 1, prozyme liquid is all transferred to stirring reaction 24h in the starch suspension, add the sodium hydroxide stopped reaction, gained suspension is centrifugal, centrifugal back gained starch is also centrifugal with distilled water wash, place 50 ℃ of loft drier to be dried to constant weight gained starch, pulverize with pulverizer, promptly get porous-starch; Described prescription is:
Ative starch is in butt quality 100g
Damping fluid, by volume 200mL
Prozyme liquid, by volume 15～20mL
(2) acidolysis then and esterification modification porous-starch: with the porous-starch is raw material, esterifying agent is dissolved in the anhydrous ethanol solvent of heat, add acid by prescription, slowly add to the esterifying agent that is dissolved in alcohol solvent in the porous-starch, constantly stir, after the slurry that obtains is crossed 10 mesh sieves, dry ethanol down in 50 ℃, regulating moisture content is 18%～24%, obtains uniform mixed reactant; Described prescription is:
Above-mentioned self-control porous-starch is in butt quality 100g
Dehydrated alcohol, by volume 60～100mL
Esterifying agent is in butt quality 2～4g
Acid, 0.02～0.10g in mass
Water is used to regulate moisture content, by volume 0～50mL
(3) dry process reaction: the mixed reactant that obtains places pressure kettle, or places electric drying oven with forced convection, adopts high temperature to react, and temperature of reaction is 130～150 ℃, and the reaction times is 3～5h.
2. preparation method according to claim 1 is characterized in that ative starch selects W-Gum, wheat starch, Starch rice or potato starch for use.
3. preparation method according to claim 1 is characterized in that the glucoamylase enzyme 20000U/mL of being alive in the prozyme liquid, and the α-Dian Fenmei enzyme is lived and is 3000U/mL.
4. preparation method according to claim 1, the esterifying agent that it is characterized in that being used for the esterification sex change is a longer chain fatty acid, selects stearic acid, lauric acid, oleic acid, linolic acid, palmitinic acid or eicosanoic acid for use.
5. preparation method according to claim 1, the catalyst acid that it is characterized in that being used for acid hydrolysis is hydrochloric acid or acetic acid.
6. use the application of the fatty acid stephanoporate starch ester of the described method preparation of claim 1, it is characterized in that as the various specific functional substance of adsorbents adsorb: as some composition in the spearmint oil in the food, pigment, fish oil and makeup and the medicine, to reach slow releasing function, prolong action effect.
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- 2008-07-08 CN CN2008101244972A patent/CN101319053B/en not_active Expired - Fee Related
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