CN101885780B - Preparation method of starch based zinc-supplementing nutrient reinforcer - Google Patents
Preparation method of starch based zinc-supplementing nutrient reinforcer Download PDFInfo
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Abstract
The invention relates to a preparation method of a starch based zinc-supplementing nutrition enhancer, which comprises the steps of: firstly, preparing starch as raw materials into a starch milk by using an acetic acid-sodium acetate buffer solution, adding into amylase, reacting at 30-55 DEG C for 4-30h, neutralizing until the pH value is 6.0-6.5, washing, drying, crushing to obtain enzymolysis starch; preparing the obtained enzymolysis starch by using water to achieve the mass concentration of 70-82 percent, reacting at 60-120 DEG C for 10min-18h, cooling to room temperature, drying, crushing to obtain heat-moisture treated starch; preparing the heat-moisture treated starch into a starch milk by using a zinc acetate solution, stirring and reacting for 5-60h; and washing, drying, crushing to obtain a product. The invention is rich in zinc-containing trace elements, can be used as a zinc-supplementing nutrition enhancer of foods and health care products, has the benefits of improving the condition of insufficient acceptable daily intake of the trace elements required by life and ensuring the health of people, and is a functional food additive with high additional value.
Description
Technical field
The present invention relates to the working method of modified starch, specifically be meant the method for utilizing biotechnology, physical method and chemical process to combine to prepare starch zinc metal complex nutrition-fortifying agent.
Background technology
The Along with people's growth in the living standard, the unreasonable trace element intake that causes of diet formula is not enough, has brought serious threat for people's health, causes the growth year by year of diseases such as cardiovascular diseases, mellitus, tumour, cerebro-vascular diseases, senile anemia.Trace element is meant and accounts for human body weight below 1/1000, the element of everyone daily requirement amount below 100mg.19 beginnings of the century, it is found that trace element existence and effect in vivo.Discover that trace element mainly works through forming conjugated protein (like oxyphorase, CER etc.), enzyme, hormone and VITAMINs etc., wherein especially have more enzyme to rely on and work with loose combination of trace element.The discovery of metalloenzyme and metalloenzyme mixture proves that clearly trace element plays key effect in enzymatic reaction.Found at present to have that to plant trace element surplus iodine, iron, copper, zinc, selenium, cobalt, chromium, the manganese etc. 20 closely bound up with the life of body, institute is essential for human body.Over nearly 50 years, the research to micro-metals has obtained progress day by day rapidly in the world, is the research of metallic element supplement in the maximum work of application facet in recent years particularly.Metallic element is mainly derived from food and water, and these can be not enough because of the amount of metal that geographic difference causes from diet, absorbing, though inorganic metal salt as the supplement application of metal for many years; But the assimilated efficiency in human body is very low; And characteristic such as that sugared metal complex has is pollution-free, anionic property is nontoxic in the physiological pH scope, and human body can effectively utilize these metals ions; Therefore be as the fine selection of organism metal supplement, have the important biomolecule meaning.
The whole nation repeatedly nutrition survey shows that China resident ratio is easier to lack calcium, iron, zinc etc.; Zinc is carried out commander and the effective running of the various functions of supervision body and the maintenance of enzyme system and cell, is the essential substance of synthetic protein.It can command the contraction of muscle, help to form Regular Insulin, is the stabilised blood liquid status, keeps the important substance of acid in the body, makes the prostate gland normal operation, and is the important substance of reproductive development.
Starch is the important component that constitutes food as a kind of neutral polysaccharide, also is the main provider of body energy.Starch is the polymer that is made up of glucose unit, has great amount of hydroxy group, and the part and the complexing of metal ion that can be used as the proton supply under certain condition form the metal supplement, in food, use as nutrition-fortifying agent.At present domestic report to starch coordination of metal ion formation complex compound is not also seen.
Summary of the invention
The objective of the invention is to that to starch and complexing of metal ion reaction exists that long reaction time, reaction efficiency are low, the metal ion content shortcoming such as less of organic form in the complex compound; The weak points such as suitability for industrialized production that are unfavorable for starch metal complex supplementary provide that a kind of production efficiency is high, the preparation method of the starch metal complex nutrition-fortifying agent of good product quality.
Starch is a kind of polycrystalline polymkeric substance, comprises amylose starch and pulullan.Starch molecule has inflexible ring texture and stronger polarity, the intermolecular hydroxyl formation hydrogen bond that can associate again.Except sugar unit itself and metal salify and further the complexing, its molecule cavity also can be participated in complexing to starch.The present invention carries out structural modification to starch granules; Enlarge starch and metals ion contact area; Increase the spirane structure quantity of starch coordination reaction and improve the ability of hydroxyl oxygen atom, make preparing method's efficient height, the superior product quality of starch based zinc-supplementing as protophobe.
The object of the invention is realized through following technical scheme:
A kind of preparation method of starch based zinc-supplementing comprises the steps:
(1) to use acetate-sodium acetate buffer to be made into mass concentration be 15～40% milk of starch to starch material, and regulate pH value to 4.0～6.5; Add glycase, consumption is that every gram dry starch adds glycase 30～600u, under 30～55 ℃ of temperature, reacted 4～30 hours, and the pH to 6.0 that neutralizes～6.5, washing, drying gets enzymolysis starch after the pulverizing; Said glycase is one or both the mixture in AMS, saccharifying enzyme and the Pullulanase;
(2) the enzymolysis starch water furnishing mass concentration that step (1) is obtained is 70～82%, places encloses container, reacts 10 minutes～18 hours down at 60～120 ℃, is cooled to room temperature, and drying gets wet heat treatment starch after the pulverizing;
(3) it is 5～25% milk of starch that the wet heat treatment starch that step (2) is obtained uses acetic acid zinc solution to be made into mass percent, and the acetate zinc concentration is 0.2～3.0mol/L, regulates pH value to 5.0～9.0, and stirring reaction is 5～60 hours under 30～55 ℃ of temperature;
(4) pH to 5.8～6.8 that neutralize, washing, drying, after the pulverizing product.
In order to realize the present invention better, when said (1) step adding glycase was two kinds, glycase added successively; Said (4) step earlier with the deionized water filter wash repeatedly, does not have free zinc when washing in solution; Step (1), (2) and (4) described drying are to be dried to moisture content at 40～50 ℃ to be lower than 14%; Step (1), (3) and (4) described pH regulate through adding hydrochloric acid or sodium hydroxide solution; The further preferred 0.05-0.2mol/L of the concentration of hydrochloric acid or sodium hydroxide solution.
The present invention compared with prior art has following advantage and beneficial effect:
(1) adopt the collaborative wet heat treatment technology of biological enzymolysis to the starch material modification of making amendment; Enlarge starch and metals ion contact area; Increase the spirane structure quantity of starch coordination reaction and improve the ability of hydroxyl oxygen atom, improved reaction efficiency, reduced cost as protophobe; Through measure finding, starch through pre-treatment after the starch zinc complex nutrition-fortifying agent that obtains of refabrication, its zinc metal content surpasses 10%, the zinc content of every gram dry starch reaches 152 milligrams.
(2) the present invention has production efficiency height, quality product advantages of higher.
Embodiment
For better understanding the present invention, the present invention is done explanation further below in conjunction with embodiment.The present invention has many successful embodiment, enumerates six concrete embodiment below, but the scope that the present invention requires to protect is not limited to the scope that embodiment representes.
Embodiment 1
A kind of preparation method of starch based zinc-supplementing comprises the steps:
The first step is regulated yam starch breast mass concentration to 15% with acetate-sodium acetate buffer; The pH value is 4.5, and temperature is 30 ℃, adds AMS (BAN 480L; Novi believes (China) Investment Co., Ltd) and saccharifying enzyme (Dextrozyme DXW, letter (China) Investment Co., Ltd of Novi); Every gram dry starch adds the AMS and the saccharifying enzyme of 30u of 400u, react 4 hours, with the sodium hydroxide solution of the 0.1mol/L pH to 6.2 that neutralizes, washs, and being dried to moisture content at 50 ℃ is 12%, must enzymolysis starch after the pulverizing.
The second step water is regulated enzymolysis starch quality concentration to 82%, is enclosed in the container, and reaction is 20 minutes under 100 ℃ of temperature, cool to room temperature, and being dried to moisture content at 45 ℃ is 14%, gets wet heat treatment starch after the pulverizing.
It is 20% milk of starch that the 3rd step used acetic acid zinc solution to be made into mass percent the starch of wet heat treatment, and the acetate zinc concentration is 0.2mol/L, and with the salt acid for adjusting pH value to 6.0 of 0.1mol/L, stirring reaction is 30 hours under 55 ℃ of temperature.
The 4th step is with the sodium hydroxide solution of the 0.1mol/L pH to 6.8 that neutralizes, washing, and being dried to moisture content at 40 ℃ is 12.5%, must product after the pulverizing.Washing is earlier with the deionized water filter wash repeatedly, in solution, does not have free zinc.Show that through mensuration the zinc content of every gram dry starch reaches 123 milligrams in the product.
Adopt the collaborative wet heat treatment technology of biological enzymolysis to the starch material modification of making amendment, biological enzymolysis can increase the specific surface area of starch, enlarges starch and metals ion contact area; Increase the reaction probability of reaction reagent and starch molecule; Wet heat treatment can improve the spirane structure quantity of starch coordination reaction and improve the ability of hydroxyl oxygen atom as protophobe, and the activation starch molecule has improved reaction efficiency; Reduce the usage quantity of reaction reagent, reduced cost.
Embodiment 2
A kind of preparation method of starch based zinc-supplementing comprises the steps:
It is 40% that the first step uses acetate-sodium acetate buffer to regulate tapioca(flour) breast mass concentration, and the pH value is 6.5, and temperature is 55 ℃; Add AMS (BAN 480L, letter (China) Investment Co., Ltd of Novi), every gram dry starch adds the AMS of 600u; Reacted 12 hours, with the hydrochloric acid of the 0.1mol/L pH to 6.0 that neutralizes, washing; Being dried to moisture content at 40 ℃ is 14%, gets enzymolysis starch after the pulverizing.
It is 75% that the second step water is regulated enzymolysis starch quality concentration, is enclosed in the container, and reaction is 10 minutes under 90 ℃ of temperature, cool to room temperature, and being dried to moisture content at 50 ℃ is 13%, gets wet heat treatment starch after the pulverizing.
It is 25% milk of starch that the 3rd step used acetic acid zinc solution to be made into mass percent the starch of wet heat treatment, and the acetate zinc concentration is 1.5mol/L, and using the sodium hydroxide solution of 0.1mol/L to regulate the pH value is 9.0, and stirring reaction is 60 hours under 45 ℃ of temperature.
The 4th step is with the hydrochloric acid of the 0.05mol/L pH5.8 that neutralizes, washing, and being dried to moisture content at 50 ℃ is 14%, must product after the pulverizing.Show that through mensuration the zinc content of every gram dry starch reaches 108 milligrams in the product.
Embodiment 3
A kind of preparation method of starch based zinc-supplementing comprises the steps:
It is 30% that the first step uses acetate-sodium acetate buffer to regulate the corn starch milk mass concentration, and the pH value is 4.0, and temperature is 50 ℃, adds AMS (BAN 480L; Letter (China) Investment Co., Ltd of Novi), every gram dry starch adds the AMS of 450u, reacts 8 hours, and enzyme goes out; Using the sodium hydroxide solution adjusting pH value of 0.1mol/L is 6.0, and temperature is 55 ℃, adds saccharifying enzyme (Dextrozyme DXW, letter (China) Investment Co., Ltd of Novi); Every gram dry starch adds the saccharifying enzyme of 30u, reacts 30 hours, with the sodium hydroxide solution of the 0.1mol/L pH to 6.5 that neutralizes; Washing, being dried to moisture content at 45 ℃ is 13%, gets enzymolysis starch after the pulverizing.
It is 70% that the second step water is regulated enzymolysis starch quality concentration, is enclosed in the container, and reaction is 15 minutes under 100 ℃ of temperature, cool to room temperature, and being dried to moisture content at 40 ℃ is 14%, gets wet heat treatment starch after the pulverizing.
It is 18% milk of starch that the 3rd step used acetic acid zinc solution to be made into mass percent the starch of wet heat treatment, and the acetate zinc concentration is 1.2mol/L, and using the sodium hydroxide solution of 0.1mol/L to regulate the pH value is 7.0, and stirring reaction is 30 hours under 40 ℃ of temperature.
The 4th step is with the hydrochloric acid of the 0.2mol/L pH6.5 that neutralizes, washing, and being dried to moisture content at 45 ℃ is 13.2%, must product after the pulverizing.Show that through mensuration the zinc content of every gram dry starch reaches 152 milligrams in the product.
Embodiment 4
A kind of preparation method of starch based zinc-supplementing comprises the steps:
It is 20% that the first step uses acetate-sodium acetate buffer to regulate wheat starch breast mass concentration, and the pH value is 4.8, and temperature is 45 ℃, adds saccharifying enzyme (Dextrozyme DXW, letter (China) Investment Co., Ltd of Novi); Every gram dry starch adds the saccharifying enzyme of 100u, react 18 hours, with the sodium hydroxide solution of the 0.1mol/L pH to 6.4 that neutralizes, washs, and being dried to moisture content at 42 ℃ is 13.8%, must enzymolysis starch after the pulverizing.
It is 80% that the second step water is regulated enzymolysis starch quality concentration, is enclosed in the container, and reaction is 18 hours under 60 ℃ of temperature, cool to room temperature, and being dried to moisture content at 45 ℃ is 11.6%, gets wet heat treatment starch after the pulverizing.
It is 5% milk of starch that the 3rd step used acetic acid zinc solution to be made into mass percent the starch of wet heat treatment, and the acetate zinc concentration is 3.0mol/L, and using the salt acid for adjusting pH value of 0.1mol/L is 5.0, and stirring reaction is 35 hours under 45 ℃ of temperature.
The 4th step is with the sodium hydroxide solution of the 0.1mol/L pH6.0 that neutralizes, washing, and being dried to moisture content at 40 ℃ is 12.2%, must product after the pulverizing.Show that through mensuration the zinc content of every gram dry starch reaches 95 milligrams in the product.
Embodiment 5
A kind of preparation method of starch based zinc-supplementing comprises the steps:
It is 30% that the first step uses acetate-sodium acetate buffer to regulate sweet potato starch breast mass concentration, and the pH value is 5.2, and temperature is 40 ℃, adds saccharifying enzyme (Dextrozyme DXW; Letter (China) Investment Co., Ltd of Novi), every gram dry starch adds the saccharifying enzyme of 150u, reacts 10 hours, and enzyme goes out; Using the salt acid for adjusting pH value of 0.1mol/L is 4.2, and temperature is 45 ℃, adds Pullulanase (Promozyme D2, letter (China) Investment Co., Ltd of Novi); Every gram dry starch adds the Pullulanase of 200u, reacts 25 hours, with the sodium hydroxide solution of the 0.1mol/L pH to 6.1 that neutralizes; Washing, being dried to moisture content at 45 ℃ is 13.3%, gets enzymolysis starch after the pulverizing.
It is 78% quality that the second step water is regulated the enzymolysis starch concentration, is enclosed in the container, and reaction is 1 hour under 120 ℃ of temperature, cool to room temperature, and being dried to moisture content at 48 ℃ is 12.5%, gets wet heat treatment starch after the pulverizing.
It is 15% milk of starch that the 3rd step used acetic acid zinc solution to be made into mass percent the starch of wet heat treatment, and the acetate zinc concentration is 2.0mol/L, and using the sodium hydroxide solution of 0.1mol/L to regulate the pH value is 7.5, and stirring reaction is 16 hours under 30 ℃ of temperature.
The 4th step is with the hydrochloric acid of the 0.1mol/L pH6.2 that neutralizes, washing, and being dried to moisture content at 45 ℃ is 12.6%, must product after the pulverizing.Show that through mensuration the zinc content of every gram dry starch reaches 119 milligrams in the product.
Embodiment 6
A kind of preparation method of starch based zinc-supplementing comprises the steps:
It is 35% that the first step uses acetate-sodium acetate buffer to regulate tapioca(flour) breast mass concentration, and the pH value is 5.0, and temperature is 50 ℃, adds AMS (BAN 480L; Letter (China) Investment Co., Ltd of Novi), every gram dry starch adds the AMS of 450u, reacts 12 hours, and enzyme goes out; Using the sodium hydroxide solution adjusting pH value of 0.1mol/L is 6.2, and temperature is 50 ℃, adds Pullulanase (Promozyme D2, letter (China) Investment Co., Ltd of Novi); Every gram dry starch adds the Pullulanase of 60u, reacts 22 hours, with the sodium hydroxide of the 0.1mol/L pH to 6.4 that neutralizes; Washing, being dried to moisture content at 45 ℃ is 13.8%, gets enzymolysis starch after the pulverizing.
It is 72% that the second step water is regulated enzymolysis starch quality concentration, is enclosed in the container, and reaction is 2 hours under 100 ℃ of temperature, cool to room temperature, and being dried to moisture content at 50 ℃ is 13.5%, gets wet heat treatment starch after the pulverizing.
It is 18% milk of starch that the 3rd step used acetic acid zinc solution to be made into mass percent the starch of wet heat treatment, and the acetate zinc concentration is 2.5mol/L, and using the sodium hydroxide solution of 0.1mol/L to regulate the pH value is 6.5, and stirring reaction is 5 hours under 30 ℃ of temperature.
The 4th step is with the sodium hydroxide solution of the 0.1mol/L pH6.6 that neutralizes, washing, and being dried to moisture content at 45 ℃ is 13.7%, must product after the pulverizing.Show that through mensuration the zinc content of every gram dry starch reaches 140 milligrams in the product.
As stated, can realize the present invention preferably.
Claims (6)
1. the preparation method of a starch based zinc-supplementing is characterized in that comprising the steps:
(1) to use acetate-sodium acetate buffer to be made into mass concentration be 15～40% milk of starch to starch material, and regulate pH value to 4.0～6.5; Add glycase, consumption is that every gram dry starch adds glycase 30～600u, under 30～55 ℃ of temperature, reacted 4～30 hours, and the pH to 6.0 that neutralizes～6.5, washing, drying gets enzymolysis starch after the pulverizing; Said glycase is one or both the mixture in AMS, saccharifying enzyme and the Pullulanase;
(2) the enzymolysis starch water furnishing mass concentration that step (1) is obtained is 70～82%, places encloses container, reacts 10 minutes～18 hours down at 60～120 ℃, is cooled to room temperature, and drying gets wet heat treatment starch after the pulverizing;
(3) it is 5～25% milk of starch that the wet heat treatment starch that step (2) is obtained uses acetic acid zinc solution to be made into mass percent, and the acetate zinc concentration is 0.2～3.0mol/L, regulates pH value to 5.0～9.0, and stirring reaction is 5～60 hours under 30～55 ℃ of temperature;
(4) pH to 5.8～6.8 that neutralize, washing, drying, after the pulverizing product.
2. the preparation method of starch based zinc-supplementing according to claim 1, it is characterized in that: said starch material is tapioca(flour), yam starch, sweet potato starch, W-Gum or wheat starch.
3. the preparation method of starch based zinc-supplementing according to claim 1 is characterized in that: step (1) adds glycase when being two kinds, and glycase is to add successively.
4. the preparation method of starch based zinc-supplementing according to claim 1 is characterized in that: the said washing of step (4) does not have the zinc of dissociating for earlier with the deionized water filter wash repeatedly in solution.
5. the preparation method of starch based zinc-supplementing according to claim 1, it is characterized in that: step (1), (2) and (4) described drying are to be dried to moisture content at 40～50 ℃ to be lower than 14%.
6. the preparation method of starch based zinc-supplementing according to claim 1 is characterized in that: step (1), (3) and (4) described pH regulate through adding hydrochloric acid or sodium hydroxide solution.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104004105B (en) * | 2014-05-13 | 2016-08-17 | 华南理工大学 | A kind of preparation method of amylose soybean lecithin clathrate |
| CN104000069B (en) * | 2014-05-13 | 2016-03-02 | 华南理工大学 | A kind of preparation method of starch base nourishment intensifying agent with zinc enriched |
| CN104207142B (en) * | 2014-08-26 | 2015-12-02 | 华南理工大学 | The preparation method of a kind of zinc supplementation and the agent of toxin expelling nutrition and health care |
| CN105995947B (en) * | 2016-05-27 | 2019-10-18 | 华南理工大学 | A method of starch zinc complex nutrition fortifier is produced using impulse electric field |
| CN110194854A (en) * | 2019-05-21 | 2019-09-03 | 广西高源淀粉有限公司 | A kind of composite modified starch and preparation method thereof |
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| US4689228A (en) * | 1985-08-26 | 1987-08-25 | University Patents, Inc. | Enhanced absorption of dietary mineral components |
| CN1247861A (en) * | 1999-09-09 | 2000-03-22 | 天津市南大星运生物医药开发有限公司 | Zinc tablet |
| CN101331949A (en) * | 2008-07-16 | 2008-12-31 | 北京康比特体育科技股份有限公司 | Sports nutrient replenisher for promoting muscle synthesize |
| CN101716180A (en) * | 2009-11-06 | 2010-06-02 | 广西强寿药业集团有限公司 | Combined medicament for supplementing zinc and calcium and preparation method thereof |
| CN101715905A (en) * | 2009-11-20 | 2010-06-02 | 天津集合科技有限公司 | Microelement-supplementing pet food for dogs and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2051591B1 (en) * | 2006-08-07 | 2016-04-20 | Novozymes A/S | Enzyme granules for animal feed |
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Patent Citations (5)
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| US4689228A (en) * | 1985-08-26 | 1987-08-25 | University Patents, Inc. | Enhanced absorption of dietary mineral components |
| CN1247861A (en) * | 1999-09-09 | 2000-03-22 | 天津市南大星运生物医药开发有限公司 | Zinc tablet |
| CN101331949A (en) * | 2008-07-16 | 2008-12-31 | 北京康比特体育科技股份有限公司 | Sports nutrient replenisher for promoting muscle synthesize |
| CN101716180A (en) * | 2009-11-06 | 2010-06-02 | 广西强寿药业集团有限公司 | Combined medicament for supplementing zinc and calcium and preparation method thereof |
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