CN103266143A - Method for preparing compound amino acid chelated zinc by utilizing cold-pressed sesame-seed cake zymolyte - Google Patents
Method for preparing compound amino acid chelated zinc by utilizing cold-pressed sesame-seed cake zymolyte Download PDFInfo
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Abstract
The invention discloses a method for preparing compound amino acid chelated zinc by utilizing cold-pressed sesame-seed cake zymolyte. The method comprises the steps: by taking cold-pressed sesame-seed cakes as raw materials, adding 0.033-0.250g/g of papain under the conditions that the temperature is 40-80 DEG C and pH is 5.0-9.0, and carrying out enzymolysis to cold-pressed sesame-seed cake protein for 2-8hours to obtain compound amino acid; by taking the compound amino acid and soluble zinc salt as raw materials, stirring the compound amino acid and soluble zinc salt in water medium for reaction according to the mole ratio of (5.00-1.00):1, thus obtaining the compound amino acid chelated zinc. The raw material cold-pressed sesame-seed cake on the market is low in price, the prepared amino acid chelated zinc meets the requirement on the physiological conditions, thus not only being capable of meeting the demand of organism on zinc, but also being capable of providing amino acid for the organism.
Description
Technical field
The present invention relates to food technology, nutrition-fortifying agent field, relate to a kind of method of utilizing cold press sesame-send cake zymolyte and zinc salt chelating to prepare nutrition-fortifying agent specifically.
Background technology
Zinc has biochemical functions widely in vivo, and grows closely relatedly, is called as " bioelement ".The pregnant woman lacks zinc influence embryo growth and development, can cause fetal anomaly seriously the time; Zinc deficiency in children can cause pica, causes immunologic function to reduce, and influences intelligence growth, and mental disorder can appear in severe patient; Lack zinc children height and weight and often be lower than normal child of the same age, severe patient has nanism; Therefore, zinc has special nutritive value to baby, children, teenager, pregnant woman etc.
The most of children of China, pregnant woman etc. are the nutritional type zn deficiencie of various degrees.Units such as China Preventive Medicial Science Institute find that to 19 preschool children of provinces and cities hair sampling Detection of China children's zinc content of about 60% is lower than normal value.Up-to-date pertinent data report, China has 80% people to lack element zinc approximately.
Sesame-send cake is the byproduct after the til seed oil expression, wherein protein content is 38%～50%, but sesame residues is mainly as fertilizer or animal-feed at present, even abandon as waste material, the nutritive value of sesame protein and economic worth do not obtain sufficient development and utilization, cause the wasting of resources and environmental pollution.
Microelements aminophenol chelated is as a kind of novel humatite element additive, compares with simple metal organic acid salt (as zinc gluconate) with traditional inorganic salt (as zinc sulfate) to have the following advantages:
1. safety is non-stimulated to stomach, and palatability is better;
2. the specific absorption height has improved trace element retaining and release action in body, the bioavailability height;
3. good stability under the physiological environment in vivo, have anti-interference, alleviate the antagonistic action between the mineral substance;
4. can supply with body essential efficient trace element and amino acid simultaneously.
At present, the zinc supplementation product is to be the s-generation zinc-supplementing of representative with the Zinc Gluconate mostly on the China market, and about amino-acid chelate as the product of zinc supplementation reinforcer seldom, " preparation method of chelates of zinc threonine " disclosed as Chinese patent 200810106871.6, this method is to be raw material with pure Threonine and soluble zinc salt, according to the heated and stirred reaction in water medium of certain ratio, obtain the inner complex of Threonine; Chinese patent 200910222122.4 discloses " a kind of preparation method of zinc-glycine chelate proliposome ", this method mainly is to adopt reverse phase evaporation to prepare the zinc-glycine chelate nanometer liposome, prepares zinc-glycine chelate proliposome by lyophilize then.The patent of these amino-acid chelate preparations is main raw material with the single amino acid expensive, that purity is higher, and function singleness can only be replenished a seed amino acid, and because on the high side, ordinary consumer is difficult for accepting.Be not the correlation technique of the zinc supplementation product of feedstock production zinc-amino acid chelate relevant for the aminoacids complex with cheap vegetable-protein hydrolysis gained also at present.
Summary of the invention
Purpose of the present invention is just providing a kind of cheap raw material of selecting for use, production safety, cheap zinc element nutrition-fortifying agent---utilize cold press sesame-send cake zymolyte to prepare the method for composite aminoacid chelating zinc, solve problems such as existing zinc supplementation agent is big to the stomach influence, palatability is poor, expensive.Utilize new technology of the present invention not only can obtain cheap zinc element nutrition-fortifying agent, can also realize taking full advantage of of sesame-send cake, and in zinc supplementation, replenish multiple amino acids.This has significance to the utilization ratio that improves the coldly-squeezed sesame oil processing byproduct and the present situation of improving present China zinc supplementation product.
Purpose of the present invention can realize by following technique measures:
Method of the present invention adopts following step to realize:
A, sesame-send cake pre-treatment: get the cold press sesame-send cake and pulverize with pulverizer, cross 60 mesh sieves, use organic solvent soaking extraction, make the oil length of sesame meal be down to below 4% desolventizing then;
B, proteins extraction: press solid-liquid ratio 1:13 ~ 20 and add tap water, regulating pH with alkali is 9.5 ~ 10.5, dissolves 3 ~ 4h under 50 ~ 60 ℃ condition, centrifugal, gets supernatant liquor, and it is 4.0 ~ 4.5 that supernatant liquor is regulated pH with hydrochloric acid, leaves standstill, and centrifugal, drying obtains protein powder;
C, proteolysis: get protein powder and mix with tap water by mass fraction 3% ~ 6%, under 85 ~ 95 ℃ of conditions, handle 30min, be 5.0 ~ 9.0 with alkali conditioned reaction pH, under 40 ~ 80 ℃ of conditions, add papoid according to the ratio of 0.033 ~ 0.250g/g, enzymolysis 2 ~ 8h, the heating 10 ~ 20min enzyme that goes out is handled, centrifugal, get supernatant liquor and measure degree of hydrolysis;
D, chelating: according to the mol ratio 5.00 ~ 1.00:1 of aminoacids complex and zinc element, under 20 ~ 90 ℃ condition, stir, and adding soluble zinc salt, slowly adding alkali conditioned reaction pH simultaneously is 6.0 ~ 8.0, and the reaction times is 1 ~ 3h, after reaction solution is cooled to normal temperature, centrifugal, drying is pulverized, and makes composite aminoacid chelating zinc.
Used organic solvent is taken from any one in ether, sherwood oil or the normal hexane among the step a of the present invention.
The centrifugation condition of carrying out after dissolving 3 ~ 4h under 50 ~ 60 ℃ the condition described in the step b of the present invention is at the centrifugal 10min of 2000 ~ 4000r/min; After getting supernatant liquor and regulating pH and be 4.0 ~ 4.5 with hydrochloric acid, time of repose is 20 ~ 60min, and centrifugal condition is at the centrifugal 5 ~ 15min of 2000 ~ 4000r/min.
Zinc salt of the present invention can be any one in zinc sulfate and crystalline hydrate, zinc nitrate and crystalline hydrate thereof, zinc acetate and crystalline hydrate thereof, zinc phosphate and crystalline hydrate thereof, zinc borate and crystalline hydrate thereof or the zinc chloride.
Alkali of the present invention is any one solid alkali in sodium hydroxide, sodium bicarbonate, yellow soda ash, potassium hydroxide or the salt of wormwood; Or the concentration corresponding with above-mentioned solid alkali is the alkali lye of 0.1 ~ 0.2mol/L.
After reaction solution described in the d step of the present invention is cooled to normal temperature, can directly carry out centrifugally to reaction solution, drying is pulverized, and makes composite aminoacid chelating zinc; Or add methyl alcohol, ethanol or acetone organic solvent and precipitate extraction, centrifugation, washing, drying is pulverized and is obtained product.
Zinc element nutrition-fortifying agent of the present invention is compared with original technology, has following beneficial effect:
A) cost of material is cheap, conveniently is easy to get, and products obtained therefrom is cheap;
B) processing condition gentleness is difficult for producing toxic substance, Product Safety height;
C) this hydrolytic process amino acid is not destroyed, and provides zinc simultaneously, amino acid and polypeptide etc. can for the eater;
D) the products obtained therefrom good palatability does not have influence to stomach, the bioavailability height.
Embodiment
The present invention is further described below with reference to embodiment, but does not limit the present invention.
Embodiment 1:
(1) gets the cold press sesame-send cake and pulverize with pulverizer, cross 60 mesh sieves, leach repeatedly with ether and reduce in the sesame meal about fat content to 1.6%, remove ether;
(2) solid-liquid ratio 1:20, regulating pH with the sodium hydroxide solution of 0.1mol/L is 10.0; Be put in 50 ℃ of water-baths, middling speed stirs 4h; The centrifugal 15min of 4500r/min gets supernatant liquor, and regulating pH with the hydrochloric acid of 0.1mol/L is 4.5, leave standstill behind the 1h again with the centrifugal 20min of 4500r/min, and abandoning supernatant, the gained white precipitate is protein; Use distilled water flushing, after vacuum-drying, pulverizer are pulverized, cross 80 mesh sieves, obtain protein powder;
(3) get protein powder and mix with tap water by mass fraction 5%, handle 30min for 90 ℃.Regulating pH with sodium hydroxide solution is 7.0,50 ℃ of water-baths, adds papoid according to the ratio of 0.08g/g, enzymolysis 4h, the boiling water bath 10min enzyme that goes out, and the centrifugal 15min of 4500r/min gets supernatant liquor and surveys degree of hydrolysis with ninhydrin colorimetry;
(4) according to measuring the aminoacids complex quality of coming out, press mass ratio 2:4.42(and zinc mol ratio 2:1) add Zinc vitriol, regulating pH with sodium hydroxide solution is 7.0, at room temperature stirs 60min.Regulate pH with sodium hydroxide solution and be 7.0, centrifugal, get precipitation, use absolute ethanol washing, suction filtration, vacuum-drying 10h, Universalpulverizer is pulverized the back and is crossed 100 mesh sieves, obtains composite aminoacid chelating zinc, and wherein zinc content 15.6%, zinc chelation percent 99.3%.
Embodiment 2:
(1) gets the cold press sesame-send cake and pulverize with pulverizer, cross 60 mesh sieves, leach repeatedly with normal hexane and reduce in the sesame meal about fat content to 1.6%, remove normal hexane;
(2) solid-liquid ratio 1:20, regulating pH with the potassium hydroxide solution of 0.1mol/L is 10.0.Be put in the water-bath 50 ℃, middling speed stirs, 4 hours.Centrifugal 15min gets supernatant liquor under the 4500r/min rotating speed.Regulating pH with the hydrochloric acid of 0.1mol/L is 4.5, leaves standstill behind the 1h again with the centrifugal 20min of 4500r/min, and the gained white precipitate is protein, take out and use distilled water flushing, and vacuum-drying, Universalpulverizer is pulverized, and mistake 80 mesh sieves obtain protein powder;
(3) get protein powder and mix with tap water by mass fraction 5%, handle 30min for 90 ℃.Regulating pH with solution of potassium carbonate is 7.0,50 ℃ of water-baths, adds papoid according to the ratio of 0.08g/g, enzymolysis 3h, the boiling water bath 10min enzyme that goes out; The centrifugal 15min of 4500r/min gets supernatant liquid and surveys degree of hydrolysis with ninhydrin colorimetry;
(4), according to the quality that detects aminoacids complex, press mass ratio 3:4.42(and zinc mol ratio 3:1) add Zinc vitriol, regulating pH with solution of potassium carbonate is 7,60min under the condition of stirring at room.Regulate pH with solution of potassium carbonate and be 7.0, centrifugal, get precipitation, use absolute ethanol washing, suction filtration, vacuum-drying 10h, Universalpulverizer is pulverized, and crosses 100 mesh sieves, obtains composite aminoacid chelating zinc, and chelating zinc zinc content is 11.2%, zinc chelation percent 99.6%.
Embodiment 3:
(1) gets the cold press sesame-send cake and pulverize with pulverizer, cross 60 mesh sieves, leach repeatedly with sherwood oil and reduce in the sesame meal about fat content to 1.6%, remove sherwood oil;
(2) solid-liquid ratio 1:20, regulating pH with the potassium hydroxide solution of 0.1mol/L is 10.0.Be put in the water-bath 50 ℃, middling speed stirs, 4 hours.Centrifugal 15min gets supernatant liquor under the 4500r/min rotating speed.Regulating pH with the hydrochloric acid of 0.1mol/L is 4.5, leaves standstill behind the 1h again with the centrifugal 20min of 4500r/min, and the gained white precipitate is protein, take out and use distilled water flushing, and vacuum-drying, Universalpulverizer is pulverized, and mistake 80 mesh sieves obtain protein powder;
(3) get protein powder and mix with tap water by mass fraction 5%, handle 30min for 90 ℃.Regulating pH with sodium hydroxide solution is 7.0,50 ℃ of water-baths, adds papoid according to the ratio of 0.16g/g, enzymolysis 2h, the boiling water bath 10min enzyme that goes out; The centrifugal 15min of 4500r/min gets supernatant liquid and surveys degree of hydrolysis with ninhydrin colorimetry;
(4), according to the quality that detects aminoacids complex, press mass ratio 3:1.55(and zinc mol ratio 3:1) add zinc chloride, regulating pH with potassium hydroxide solution is 7.0,60min under the condition of stirring at room.Regulate pH with potassium hydroxide solution and be 7.0, centrifugal, get precipitation, use absolute ethanol washing, suction filtration, vacuum-drying 10h, Universalpulverizer is pulverized, and crosses 100 mesh sieves, obtains composite aminoacid chelating zinc, and chelating zinc zinc content is 11.3%, zinc chelation percent 99.4%.
Embodiment 4:
(1) gets the cold press sesame-send cake and pulverize with pulverizer, cross 60 mesh sieves, leach repeatedly with sherwood oil and reduce in the sesame meal about fat content to 1.6%, remove sherwood oil;
(2) solid-liquid ratio 1:20, regulating pH with the sodium hydroxide solution of 0.1mol/L is 10.0.Be put in the water-bath 50 ℃, middling speed stirs, 4 hours.Centrifugal 15min gets supernatant liquor under the 4500r/min rotating speed.Regulating pH with the hydrochloric acid of 0.1mol/L is 4.5, leaves standstill behind the 1h again with the centrifugal 20min of 4500r/min, and the gained white precipitate is protein, take out and use distilled water flushing, and vacuum-drying, Universalpulverizer is pulverized, and mistake 80 mesh sieves obtain protein powder;
(3) get protein powder and mix with tap water by mass fraction 5%, handle 30min for 90 ℃.Regulating pH with sodium carbonate solution is 7.0,50 ℃ of water-baths, adds papoid according to the ratio of 0.10g/g, enzymolysis 3h, the boiling water bath 10min enzyme that goes out; The centrifugal 15min of 4500r/min gets supernatant liquid and surveys degree of hydrolysis with ninhydrin colorimetry;
(4), according to the aminoacids complex quality of measure, press mass ratio 2:2.82(and zinc mol ratio 2:1) the adding zinc acetate, pH is 7.0 with the sodium carbonate solution adjusting, at room temperature stirs 60min.Regulate pH with sodium carbonate solution and be 7.0, centrifugal, get precipitation, use absolute ethanol washing, suction filtration, vacuum-drying 10h, Universalpulverizer is pulverized the back and is crossed 100 mesh sieves, obtains composite aminoacid chelating zinc, and wherein zinc content 14.6%, zinc chelation percent 99.3%.
Claims (6)
1. preparation method who utilizes cold press sesame-send cake enzymolysis to prepare composite aminoacid chelating zinc, it is characterized in that: described method adopts following step to realize:
A, sesame-send cake pre-treatment: get the cold press sesame-send cake and pulverize with pulverizer, cross 60 mesh sieves, use organic solvent soaking extraction, make the oil length of sesame meal be down to below 4% desolventizing then;
B, proteins extraction: press solid-liquid ratio 1:13 ~ 20 and add tap water, regulating pH with alkali is 9.5 ~ 10.5, dissolves 3 ~ 4h under 50 ~ 60 ℃ condition, centrifugal, gets supernatant liquor, and it is 4.0 ~ 4.5 that supernatant liquor is regulated pH with hydrochloric acid, leaves standstill, and centrifugal, drying obtains protein powder;
C, proteolysis: get protein powder and mix with tap water by mass fraction 3% ~ 6%, under 85 ~ 95 ℃ of conditions, handle 30min, be 5.0 ~ 9.0 with alkali conditioned reaction pH, under 40 ~ 80 ℃ of conditions, add papoid according to the ratio of 0.033 ~ 0.250g/g, enzymolysis 2 ~ 8h, the heating 10 ~ 20min enzyme that goes out is handled, centrifugal, get supernatant liquor and measure degree of hydrolysis;
D, chelating: according to the mol ratio 5.00 ~ 1.00:1 of aminoacids complex and zinc element, under 20 ~ 90 ℃ condition, stir, and adding soluble zinc salt, slowly adding alkali conditioned reaction pH simultaneously is 6.0 ~ 8.0, and the reaction times is 1 ~ 3h, after reaction solution is cooled to normal temperature, centrifugal, drying is pulverized, and makes composite aminoacid chelating zinc.
2. the preparation method of composite aminoacid chelating zinc according to claim 1, it is characterized in that: used organic solvent is taken from any one in ether, sherwood oil or the normal hexane among the step a.
3. the preparation method of composite aminoacid chelating zinc according to claim 1 is characterized in that: the centrifugation condition of carrying out after dissolving 3 ~ 4h under 50 ~ 60 ℃ the condition described in the step b is at the centrifugal 10min of 2000 ~ 4000r/min; After getting supernatant liquor and regulating pH and be 4.0 ~ 4.5 with hydrochloric acid, time of repose is 20 ~ 60min, and centrifugal condition is at the centrifugal 5 ~ 15min of 2000 ~ 4000r/min.
4. the preparation method of composite aminoacid chelating zinc according to claim 1, it is characterized in that: described zinc salt can be any one in zinc sulfate and crystalline hydrate, zinc nitrate and crystalline hydrate thereof, zinc acetate and crystalline hydrate thereof, zinc phosphate and crystalline hydrate thereof, zinc borate and crystalline hydrate thereof or the zinc chloride.
5. the preparation method of composite aminoacid chelating zinc according to claim 1, it is characterized in that: described alkali is any one solid alkali in sodium hydroxide, sodium bicarbonate, yellow soda ash, potassium hydroxide or the salt of wormwood; Or the concentration corresponding with above-mentioned solid alkali is the alkali lye of 0.1 ~ 0.2mol/L.
6. the preparation method of composite aminoacid chelating zinc according to claim 1 is characterized in that: after the reaction solution described in the d step is cooled to normal temperature, can directly carry out centrifugally to reaction solution, drying is pulverized, and makes composite aminoacid chelating zinc; Or add methyl alcohol, ethanol or acetone organic solvent and precipitate extraction, centrifugation, washing, drying is pulverized and is obtained product.
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| CN106831091A (en) * | 2016-12-16 | 2017-06-13 | 三门峡龙飞生物工程有限公司 | A kind of geobiont repair |
| CN109548986A (en) * | 2019-01-09 | 2019-04-02 | 武汉轻工大学 | A kind of preparation method of chelates of composite amino acid |
| CN111072755A (en) * | 2020-01-06 | 2020-04-28 | 湖北泓肽生物科技有限公司 | Lipeptide complex, pharmaceutical composition thereof, preparation method and application thereof |
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| CN111072755A (en) * | 2020-01-06 | 2020-04-28 | 湖北泓肽生物科技有限公司 | Lipeptide complex, pharmaceutical composition thereof, preparation method and application thereof |
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Application publication date: 20130828 |