CN103284159B - Linoleic acid loaded soy isolate protein/chitosan composite microcapsule and preparation method thereof - Google Patents
Linoleic acid loaded soy isolate protein/chitosan composite microcapsule and preparation method thereof Download PDFInfo
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- CN103284159B CN103284159B CN201310260475.XA CN201310260475A CN103284159B CN 103284159 B CN103284159 B CN 103284159B CN 201310260475 A CN201310260475 A CN 201310260475A CN 103284159 B CN103284159 B CN 103284159B
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 34
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 title claims abstract description 18
- 235000020778 linoleic acid Nutrition 0.000 title claims abstract description 18
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 title claims abstract description 18
- 239000002131 composite material Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 108090000623 proteins and genes Proteins 0.000 title claims abstract description 8
- 102000004169 proteins and genes Human genes 0.000 title claims abstract description 8
- 229920001661 Chitosan Polymers 0.000 title abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 9
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 3
- 108010073771 Soybean Proteins Proteins 0.000 claims description 22
- 235000019710 soybean protein Nutrition 0.000 claims description 22
- 238000013019 agitation Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 239000000839 emulsion Substances 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 7
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 7
- 244000068988 Glycine max Species 0.000 claims description 6
- 235000010469 Glycine max Nutrition 0.000 claims description 6
- 239000002775 capsule Substances 0.000 claims description 5
- 235000011187 glycerol Nutrition 0.000 claims description 5
- 235000018102 proteins Nutrition 0.000 claims description 5
- 238000007711 solidification Methods 0.000 claims description 5
- 230000008023 solidification Effects 0.000 claims description 5
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical group CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 4
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract 2
- 238000003756 stirring Methods 0.000 abstract 2
- 239000000725 suspension Substances 0.000 abstract 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 230000008014 freezing Effects 0.000 abstract 1
- 238000007710 freezing Methods 0.000 abstract 1
- 238000000265 homogenisation Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000012460 protein solution Substances 0.000 abstract 1
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 3
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 2
- 235000012000 cholesterol Nutrition 0.000 description 2
- 235000004626 essential fatty acids Nutrition 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 208000034189 Sclerosis Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 230000003143 atherosclerotic effect Effects 0.000 description 1
- 238000006701 autoxidation reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 201000005577 familial hyperlipidemia Diseases 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000010499 rapseed oil Substances 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002792 vascular Effects 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
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- Manufacturing Of Micro-Capsules (AREA)
- Medicinal Preparation (AREA)
- Peptides Or Proteins (AREA)
Abstract
The invention discloses a linoleic acid loaded soy isolate protein/chitosan composite microcapsule and a preparation method thereof, and belongs to the technical field of microcapsules of agricultural and sideline products. The preparation method comprises the steps of adding linoleic acid and a little of emulsifier to soy isolate protein solution to be mixed with acetum of chitosan, carrying out homogenization on the mixed solution for 10-15 minutes, so as to form uniform lactescence; adjusting the pH of the lactescence to the range of 4.5-4.8; magnetically stirring for 10-15 minutes; primarily forming the suspension solution of the microcapsule; adjusting the pH value of the suspension solution of the microcapsule to 7-7.3; adding a little of glycerol aqueous solution as a curing agent; magnetically stirring and curing for 1-2 hours; layering and extracting after stewing for 1-3 hours; collecting a web bag after washing by distilled water; freezing and drying in vacuum to obtain the linoleic acid loaded soy isolate protein/chitosan composite microcapsule. The embedding efficiency of the obtained microcapsule is over 60%; the embedding yield is over 65%; the composite microcapsule is long in shelf life and convenient to store.
Description
Technical field
The invention belongs to microcapsules technology field, be specifically related to one and carry linoleic soybean protein isolate/shitosan composite micro-capsule and preparation method thereof.
Background technology
Linoleic acid is that human body can not synthesize, or the aliphatic acid that the amount of synthesis far can not be satisfied the demand, and is called essential fatty acid.Linoleic acid is generally acknowledged a kind of essential fatty acid.Because linoleic acid can reduce blood cholesterol levels, prevention of arterial is atherosis and extremely pay attention to.Research finds, after cholesterol must be combined with linoleic acid, could operate normally in vivo and metabolism.If shortage linoleic acid, cholesterol will be combined with some saturated fatty acids, dysbolism occurs, vascular wall deposits, progressively forms atherosclerotic, causes cardiovascular and cerebrovascular disease.Therefore, medically enough attention are caused to linoleic application, be usually used in disease such as treatment Hyperlipemia and artery sclerosis etc.Several vegetable oil linoleic acid content is higher, and if peanut oil is 26%, soya-bean oil is 57.5%, and rape oil is 15.8%.But linoleic acid very easily autoxidation occurs in atmosphere, cause losing its effect, this brings a difficult problem just to linoleic preservation, needs to find a kind of resist technology preferably, promotes its stability.
Microcapsules technology refers to and the solid matter of dispersion, drop or gas is encapsulated in the method forming microcapsules in one deck dense film completely.Usual dense film is made up of macromolecular material that is natural or Prof. Du Yucang.Microcapsules technology has been applied in the industry such as medicine, agricultural, computer, chemicals, food, cosmetics, causes the extensive concern of academia.
Summary of the invention
The object of this invention is to provide a kind of year linoleic soybean protein isolate/shitosan composite micro-capsule, the compound microcapsules obtained are made up of soybean protein isolate, shitosan, linoleic acid and emulsifying agent, the microscapsule powder obtained is fine and smooth, more than 80 orders, and embedding efficiency is more than 60%, embedding productive rate is more than 65%, and its preparation process is as follows:
(1) soybean isolate protein powder of 5 ~ 8g is dissolved in 100mL, 50 ~ 65 DEG C of water, keep temperature-resistant and magnetic agitation 5 ~ 10min, ultrasonic 10 ~ 20min under 50 ~ 65 DEG C of conditions afterwards, by the mixed liquor that obtains centrifugal 20 ~ 30min under 10000 ~ 15000r, the condition of 4 DEG C, collect supernatant, and by supernatant constant volume to 100mL, obtain soybean protein isolate solution;
(2) shitosan of 1 ~ 2g is dissolved in 100mL, volume fraction is in the aqueous acetic acid of 1 ~ 3%, obtain the acetum of shitosan;
(3) 1 ~ 2g linoleic acid and 0.05 ~ 0.1g emulsifying agent are joined in 100mL soybean protein isolate solution prepared by step (1), the acetum of the 100mL shitosan prepared with step (2) mixes, by mixed liquor homogeneous 10 ~ 15min under the high-shear homogenizer of 6000 ~ 8000r, thus form homogeneous emulsion, the scope of emulsion pH to 4.5 ~ 4.8 is regulated with the hydrochloric acid of 1mol/L, magnetic agitation 10 ~ 15min again, forms the aaerosol solution of microcapsules;
(4) regulate the pH value of microcapsules aaerosol solution to 7 ~ 7.3 with the NaoH solution of 1mol/L, then add 10 ~ 20mL, volume fraction is that the glycerine water solution of 50 ~ 60% is as curing agent, magnetic agitation solidification 1 ~ 2h, layering after standing 1 ~ 3h, collect wet capsule after the washing of suction filtration, distilled water, obtain carrying linoleic soybean protein isolate/shitosan composite micro-capsule powder through vacuum freeze drying.
Wherein, described emulsifying agent can be glycerin monostearate, any one in D-sorbite monoglyceride.Described suction filtration, be low speed Filter paper filtering in adopting, collection obtains filter cake and washs through distilled water.Described vacuum freeze drying is that the filter cake obtained by suction filtration is less than the condition of 10Pa, cold sunken temperature-45 ~ 30 DEG C in vacuum under drying is totally.
Detailed description of the invention
Embodiment 1:
The soybean isolate protein powder of 5g is dissolved in the hot water of the 100mL of 50 DEG C, keep temperature-resistant and magnetic agitation 10min, move on to afterwards in ultrasonic device, 50 DEG C of ultrasonic 10min, the mixed liquor obtained is centrifugal 30min under 10000r, the condition of 4 DEG C, collect supernatant, and supernatant is added water constant volume to 100mL, obtain soybean protein isolate solution; The shitosan of 1g being dissolved in 100ml volume fraction is in the aqueous acetic acid of 1%, obtains the acetum of shitosan; 1.2g linoleic acid and 0.05g glycerin monostearate are joined in the above-mentioned 100mL soybean protein isolate solution prepared, mix with the acetum of the above-mentioned 100mL shitosan prepared, by mixed liquor homogeneous 10min under the high-shear homogenizer of 8000r, thus form homogeneous emulsion, regulate emulsion pH to 4.5 with the hydrochloric acid of 1mol/L, magnetic agitation 15min again, begins to take shape the aaerosol solution of microcapsules.Regulate the pH value of microcapsules aaerosol solution to 7 with the NaoH solution of 1mol/L, adding 15mL volume fraction is that the glycerine water solution of 55% is as curing agent, magnetic agitation solidification 2h, layering after standing 2h, low speed filter paper suction filtration in employing, suction filtration gained filter cake collects wet capsule with after distilled water washing, 10Pa is less than in vacuum, under the condition of cold sunken temperature-45 ~ 30 DEG C, vacuum freeze drying totally, obtain carrying linoleic soybean protein isolate/shitosan composite micro-capsule powder 4.795g, wherein containing soybean protein isolate 3.16g, chitosan-containing 0.8g, containing linoleic acid 0.79g, containing emulsifying agent 0.045, powder order number is 80 orders, its embedding efficiency is 61.2%, embedding productive rate 65.8%, and shelf life is long, be convenient to storage.
Embodiment 2:
The soybean isolate protein powder of 6g is dissolved in the hot water of the 100mL of 55 DEG C, keep temperature-resistant and magnetic agitation 12min, move on to afterwards in ultrasonic device, 55 DEG C of ultrasonic 10min, the mixed liquor obtained is centrifugal 25min under 12000r, the condition of 4 DEG C, collect supernatant, and by supernatant constant volume to 100mL; The shitosan of 1.2g being dissolved in 100ml volume fraction is in the acetum of 2%; 1.5g linoleic acid and 0.06g glycerin monostearate are joined in the above-mentioned 100mL soybean protein isolate solution prepared, mix with the acetum of the above-mentioned 100mL shitosan prepared, by mixed liquor homogeneous 15min under the high-shear homogenizer of 6000r, thus form homogeneous emulsion, regulate emulsion pH to 4.5 with the hydrochloric acid of 1mol/L, magnetic agitation 15min again, begins to take shape the aaerosol solution of microcapsules.Regulate the pH value of microcapsules aaerosol solution to 7 with the NaoH solution of 1mol/L, adding 15mL volume fraction is that the glycerine water solution of 60% is as curing agent, magnetic agitation solidification 2h, layering after standing 3h, low speed filter paper suction filtration in employing, filter cake collects wet capsule with after distilled water washing, 10Pa is less than in vacuum, under the condition of cold sunken temperature-45 ~ 30 DEG C, vacuum freeze drying totally, obtain carrying linoleic soybean protein isolate/shitosan composite micro-capsule powder 5.485g, wherein containing soybean protein isolate 3.42g, chitosan-containing 1g, containing linoleic acid 0.99g, containing emulsifying agent 0.048, powder order number is 100 orders, its embedding efficiency is 61.9%, embedding productive rate 66.3%, and shelf life is long, be convenient to storage.
Embodiment 3:
The soybean isolate protein powder of 8g is dissolved in the hot water of the 100mL of 65 DEG C, keep temperature-resistant and magnetic agitation 10min, move on to afterwards in ultrasonic device, 65 DEG C of ultrasonic 15min, the mixed liquor obtained is centrifugal 20min under 15000r, the condition of 4 DEG C, collect supernatant, and by supernatant constant volume to 100mL; The shitosan of 2g being dissolved in 100ml volume fraction is in the aqueous acetic acid of 3%; 2g linoleic acid and 0.1g D-sorbite monoglyceride are joined in the above-mentioned 100mL soybean protein isolate solution prepared, mix with the acetum of the above-mentioned 100mL shitosan prepared, by mixed liquor homogeneous 10min under the high-shear homogenizer of 8000r, thus form homogeneous emulsion, regulate emulsion pH to 4.8 with the hydrochloric acid of 1mol/L, magnetic agitation 15min again, begins to take shape the aaerosol solution of microcapsules.Regulate the pH value of microcapsules aaerosol solution to 7.3 with the NaoH solution of 1mol/L, adding 20mL volume fraction is that the glycerine water solution of 60% is as curing agent, magnetic agitation solidification 2h, layering after standing 2h, low speed filter paper suction filtration in employing, filter cake collects wet capsule with after distilled water washing, 10Pa is less than in vacuum, under the condition of cold sunken temperature-45 ~ 30 DEG C, vacuum freeze drying totally, obtain carrying linoleic soybean protein isolate/shitosan composite micro-capsule powder 7.538g, wherein containing soybean protein isolate 4.76g, chitosan-containing 1.43g, containing linoleic acid 1.3g, containing emulsifying agent 0.048, powder order number is 100 orders, its embedding efficiency is 62.4%, embedding productive rate 65.3%, and shelf life is long, be convenient to storage.
Claims (2)
1. carry a preparation method for linoleic soybean protein isolate/shitosan composite micro-capsule, its step is as follows:
(1) soybean isolate protein powder of 5 ~ 8g is dissolved in 100mL, 50 ~ 65 DEG C of water, keep temperature-resistant and magnetic agitation 5 ~ 10min, ultrasonic 10 ~ 20min under 50 ~ 65 DEG C of conditions afterwards, collected after centrifugation supernatant, and by supernatant constant volume to 100mL, obtain soybean protein isolate solution;
(2) shitosan of 1 ~ 2g is dissolved in 100mL, volume fraction is in the aqueous acetic acid of 1 ~ 3%, obtain the acetum of shitosan;
(3) 1 ~ 2g linoleic acid and 0.05 ~ 0.1g emulsifying agent are joined in 100mL soybean protein isolate solution prepared by step (1), the acetum of the 100mL shitosan prepared with step (2) mixes, by mixed liquor homogeneous 10 ~ 15min under 6000 ~ 8000r/min, thus form homogeneous emulsion, regulate the emulsion pH scope to 4.5 ~ 4.8, magnetic agitation 10 ~ 15min again, forms the aaerosol solution of microcapsules; Emulsifying agent is glycerin monostearate or D-sorbite monoglyceride;
(4) regulate the pH value of microcapsules aaerosol solution to 7 ~ 7.3, then add 10 ~ 20mL, volume fraction is that the glycerine water solution of 50 ~ 60% is as curing agent, magnetic agitation solidification 1 ~ 2h, layering after standing 1 ~ 3h, collect wet capsule after the filter cake distilled water washing obtained by suction filtration, obtain carrying linoleic soybean protein isolate/shitosan composite micro-capsule powder through vacuum freeze drying;
Centrifugal described in step (1) is by the mixed liquor that obtains centrifugal 20 ~ 30min under 10000 ~ 15000r/min, the condition of 4 DEG C; It is the scope regulating emulsion pH to 4.5 ~ 4.8 with the hydrochloric acid of 1mol/L in step (3); Step (4) NaOH solution of 1mol/L regulates the pH value of microcapsules aaerosol solution to 7 ~ 7.3; Suction filtration described in step (4) adopts Medium speed filter paper to filter, and collection obtains filter cake and washs through distilled water; Vacuum freeze drying described in step (4) is that the filter cake obtained by suction filtration is less than the condition of 10Pa, cold sunken temperature-45 ~ 30 DEG C in vacuum under drying is totally.
2. carry linoleic soybean protein isolate/shitosan composite micro-capsule, it is characterized in that: prepared by preparation method according to claim 1.
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| CN106689389A (en) * | 2016-12-05 | 2017-05-24 | 东北农业大学 | Preparation method of modified soy protein-polyphenol composite emulsion |
| CN106721849A (en) * | 2016-12-20 | 2017-05-31 | 青海览进生物科技开发有限公司 | A kind of preparation method of black fruit fructus lycii anthocyanidin Instant Drinks granule |
| CN107712587A (en) * | 2017-10-17 | 2018-02-23 | 广州润虹医药科技股份有限公司 | A kind of anti-oxidant anti-aging nutrient powder and preparation method thereof |
| CN108112954B (en) * | 2017-12-14 | 2021-07-02 | 广州市恒裕香料有限公司 | Microcapsule food sweetening agent and preparation method thereof |
| CN111955598A (en) * | 2020-08-28 | 2020-11-20 | 广州大学 | Method for preparing acid-soluble soybean protein by using homogenization method |
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| CN115226765A (en) * | 2022-01-26 | 2022-10-25 | 四川农业大学 | Preparation method and application of enzyme-sensitive composite membrane |
| CN115252829A (en) * | 2022-08-07 | 2022-11-01 | 山西省人民医院 | Preparation method of ultrasonic contrast agent capable of targeting kidney cancer administration |
| CN116172086B (en) * | 2023-03-27 | 2024-05-10 | 河南工业大学 | Preparation method and application of novel quick-frozen special grease substitute grease |
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| CN1140332C (en) * | 2001-10-24 | 2004-03-03 | 中国科学院新疆化学研究所 | Conjugate linoleic acid or conjugate linoleate microcapsule |
| CN101125133B (en) * | 2007-09-27 | 2011-06-01 | 武汉麦可得生物技术有限公司 | Unsaturated fatty acid microcapsule preparing technology and application |
| CN102293266B (en) * | 2011-08-18 | 2012-10-31 | 中国海洋大学 | Method for preparing antioxidant fish oil microcapsule |
| CN102742810B (en) * | 2012-07-19 | 2013-11-06 | 青岛农业大学 | Garlic oil microcapsule with shell made of soybean protein isolate and chitosan and preparation method and application thereof |
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