CN105166885A - Conjugated linoleic acid embedded microcapsule preparation method - Google Patents
Conjugated linoleic acid embedded microcapsule preparation method Download PDFInfo
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- CN105166885A CN105166885A CN201510484137.3A CN201510484137A CN105166885A CN 105166885 A CN105166885 A CN 105166885A CN 201510484137 A CN201510484137 A CN 201510484137A CN 105166885 A CN105166885 A CN 105166885A
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- cla
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- octenyl succinate
- succinate anhydride
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229940108924 conjugated linoleic acid Drugs 0.000 title abstract 6
- JBYXPOFIGCOSSB-GOJKSUSPSA-N 9-cis,11-trans-octadecadienoic acid Chemical compound CCCCCC\C=C\C=C/CCCCCCCC(O)=O JBYXPOFIGCOSSB-GOJKSUSPSA-N 0.000 title abstract 3
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 title abstract 3
- 229920002472 Starch Polymers 0.000 claims abstract description 57
- 235000019698 starch Nutrition 0.000 claims abstract description 57
- 239000008107 starch Substances 0.000 claims abstract description 57
- 239000000839 emulsion Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000084 colloidal system Substances 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- -1 octenyl succinate anhydride Chemical class 0.000 claims description 36
- 229920001285 xanthan gum Polymers 0.000 claims description 30
- 230000008569 process Effects 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000004567 concrete Substances 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- 229920002907 Guar gum Polymers 0.000 claims description 6
- 235000010417 guar gum Nutrition 0.000 claims description 6
- 239000000665 guar gum Substances 0.000 claims description 6
- 229960002154 guar gum Drugs 0.000 claims description 6
- 238000001246 colloidal dispersion Methods 0.000 claims description 5
- 238000000265 homogenisation Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000010008 shearing Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 2
- 241000206575 Chondrus crispus Species 0.000 claims description 2
- 108010010803 Gelatin Proteins 0.000 claims description 2
- 229920002148 Gellan gum Polymers 0.000 claims description 2
- 229920000161 Locust bean gum Polymers 0.000 claims description 2
- 235000010489 acacia gum Nutrition 0.000 claims description 2
- 239000001785 acacia senegal l. willd gum Substances 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 239000008273 gelatin Substances 0.000 claims description 2
- 229920000159 gelatin Polymers 0.000 claims description 2
- 235000019322 gelatine Nutrition 0.000 claims description 2
- 235000011852 gelatine desserts Nutrition 0.000 claims description 2
- 235000010492 gellan gum Nutrition 0.000 claims description 2
- 239000000216 gellan gum Substances 0.000 claims description 2
- 235000010420 locust bean gum Nutrition 0.000 claims description 2
- 239000000711 locust bean gum Substances 0.000 claims description 2
- 239000001814 pectin Substances 0.000 claims description 2
- 235000010987 pectin Nutrition 0.000 claims description 2
- 229920001277 pectin Polymers 0.000 claims description 2
- 235000010413 sodium alginate Nutrition 0.000 claims description 2
- 239000000661 sodium alginate Substances 0.000 claims description 2
- 229940005550 sodium alginate Drugs 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- 235000010491 tara gum Nutrition 0.000 claims description 2
- 239000000213 tara gum Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 210000000813 small intestine Anatomy 0.000 abstract description 8
- 235000013305 food Nutrition 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 235000016709 nutrition Nutrition 0.000 abstract description 2
- 238000001694 spray drying Methods 0.000 abstract description 2
- FLISWPFVWWWNNP-BQYQJAHWSA-N dihydro-3-(1-octenyl)-2,5-furandione Chemical compound CCCCCC\C=C\C1CC(=O)OC1=O FLISWPFVWWWNNP-BQYQJAHWSA-N 0.000 abstract 3
- 150000002148 esters Chemical class 0.000 abstract 3
- 235000014106 fortified food Nutrition 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 230000001766 physiological effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 241000030538 Thecla Species 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 230000000968 intestinal effect Effects 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- 108090000790 Enzymes Proteins 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229940088598 enzyme Drugs 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 210000004051 gastric juice Anatomy 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000006069 physical mixture Substances 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- ADHNUPOJJCKWRT-JLXBFWJWSA-N (2e,4e)-octadeca-2,4-dienoic acid Chemical class CCCCCCCCCCCCC\C=C\C=C\C(O)=O ADHNUPOJJCKWRT-JLXBFWJWSA-N 0.000 description 1
- 206010003210 Arteriosclerosis Diseases 0.000 description 1
- 240000004859 Gamochaeta purpurea Species 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 208000001132 Osteoporosis Diseases 0.000 description 1
- 108010019160 Pancreatin Proteins 0.000 description 1
- 229920000294 Resistant starch Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 208000011775 arteriosclerosis disease Diseases 0.000 description 1
- 238000006701 autoxidation reaction Methods 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 230000002478 diastatic effect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002496 gastric effect Effects 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000001319 headspace solid-phase micro-extraction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 229940055695 pancreatin Drugs 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000021254 resistant starch Nutrition 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 230000001228 trophic effect Effects 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The present invention discloses a conjugated linoleic acid embedded microcapsule preparation method which uses octenyl succinic anhydride starch esters and hydrophilic colloids as main raw materials and comprises the following specific steps: firstly, the hydrophilic colloids are uniformly dispersed in water to be prepared into a colloidal solution; then the octenyl succinic anhydride starch esters are added into the colloidal solution to prepare a compound solution of the octenyl succinic anhydride starch esters and the hydrophilic colloids; then conjugated linoleic acids are added into the compound solution to prepare an emulsion; and finally the emulsion is subjected to spray drying to prepare the embedded conjugated linoleic acid microcapsules. The method provides a novel embedding wall material, which improves the oxidative stability of the conjugated linoleic acids, and has a slow-release function, and thus solves the problems that the conjugated linoleic acids are easy for auto-oxidation and low in physiological activity before entering into human body small intestines, and the microcapsule can be used as a nutritional fortifier to be added into functionally and nutritionally fortified food and staple food.
Description
Technical field
The present invention relates to functional food additives technical field, especially relate to a kind of compound system embedding CLA adopting starch octenyl succinate anhydride and hydrophilic colloid, and prepare the method for microcapsules.
Background technology
CLA (CLA) is the general name of the isomers of octadecadienoic acid, can play the effect of the diseases such as prevention and control diabetes, osteoporosis, angiocardiopathy, hypertension, arteriosclerosis, cancer, also has trophic function simultaneously; But its poorly water-soluble, the impact being easily subject to the environmental factors such as heat, light, pH are oxidized; its major absorption site is at the small intestine of human body; but be everlasting and just lose before being absorbed by human small intestine or to reduce its physiologically active; therefore, it needs to have anti-oxidant and slowly-releasing or control-release function carrier and embed protection and to be also absorbed and used in carrying to small intestine its due physiological function of competence exertion.
Spray drying process is at present in the most widely used stable state means of field of food, application in the microcapsule embedded technology of field of food is the most general, the existing method utilizing spraying dry to prepare function factor microcapsules in prior art, most character such as embedding rate, dissolubility, rehydration just laying particular emphasis on microcapsule product, rarely have from adapting to the angle of human internal environment to consider the release of function factor in human body, absorbing state, therefore, the release rate of function factor in human small intestine and utilization rate can not really effectively be improved.
Therefore, be necessary to provide a kind of preparation technology's flow process embedding the microcapsules of CLA, realize the effect that it protects and reduces CLA loss in human consumption's process, to solve the low problem of the release rate of CLA in small intestine.
Summary of the invention
For the problems referred to above that prior art exists, the applicant provides a kind of preparation method embedding the microcapsules of CLA.Present approach provides a kind of novel embedding wall material, improve the oxidation stability of CLA, and there is slow control-release function, thus solve the easy autoxidation of CLA and the problem of physiologically active reduction before entering human small intestine, can be used as a kind of nutrition fortifier and add in functional nutrient condensed food and staple food.
Technical scheme of the present invention is as follows:
Embed a preparation method for the microcapsules of CLA, the method is with starch octenyl succinate anhydride and hydrophilic colloid for primary raw material, and concrete steps are as follows:
(1) hydrophilic colloid is dispersed in water, stirs 15min-90min, make colloidal dispersions even, obtained colloidal solution;
(2) take starch octenyl succinate anhydride, add the colloidal solution that step (1) is obtained, stir and make sample mix even, the combination solution of obtained starch octenyl succinate anhydride and hydrophilic colloid;
(3) in the combination solution that step (2) is obtained, add CLA, use high-speed shearing machine high speed shear to obtain coarse emulsion, high-pressure homogeneously obtain emulsion;
(4) emulsion that step (3) is obtained is carried out spraying dry, the microcapsules of obtained described embedding CLA.
In described step (2), the mass ratio of starch octenyl succinate anhydride and hydrophilic colloid is 20:1-180:1.
In the consumption of CLA and combination solution, the ratio of starch octenyl succinate anhydride and hydrophilic colloid quality summation is 1:10-1:3 in described step (3); The solid content of described emulsion is 10-15%.
The speed that described step (3) high speed is sheared is 11000-24000r/min, shear time 2-4min; Described high-pressure homogeneous pressure is 30-70MPa, and homogenization cycles is 3-5 time.
In described step (4), spray-dired process conditions are: EAT 150-190 DEG C, leaving air temp 75-95 DEG C, charging rate 10-20mL/min.
Described hydrophilic colloid is one or more in guar gum, locust bean gum, tara gum, gellan gum, sodium carboxymethylcellulose, xanthans, sodium alginate, carragheen, Arabic gum, gelatin, pectin.
The technique effect that the present invention is useful is:
1, the present invention's starch octenyl succinate anhydride used (OSA starch) is a kind of slow-digestion starch or resistant starch, hydrophilic colloid has excellent emulsion stability, good film-forming property, and not easily corroded by enzyme, in starch octenyl succinate anhydride, add hydrophilic colloid, good synergistic can be reached after proper proportion is composite; Hydrophilic colloid self is not easily by enzyme effect; more easily hydrated gel layer is formed after being combined with starch; starch can be protected from the degradation of acid to the package action of starch; the diastatic erosion of further suppression; thus improve the digestic property of starch; therefore the two combination effectively can be resisted the hydrolysis of hydrochloric acid in gastric juice and enzyme in gastric juice, improve the digestic property of starch, realize the protective effect in enteron aisle of core and CLA and release property.
2, the present invention adopts microcapsule embedded means, the stability of CLA can be improved, by microencapsulation, its stability is improved for oxidizable, function factor volatile, easily affected by environment, the decomposition that active ingredient can be stoped to cause because of illumination, oxygen etc. and evaporation, reduce or avoid the loss of function factor in process.
3, the present invention adopts safe modified starch and natural polymer as the carrier material of CLA; security is high; meet the requirement of the development of food industry of " green processing "; starch octenyl succinate anhydride has hydrophily and hydrophobicity simultaneously; drastically increase the emulsifiability of starch; the hydrophilic colloids such as xanthans have excellent emulsion stability; make it in microencapsulation processes without the need to additionally adding emulsifying agent or other auxiliary ingredients; protection core and emulsification double action can be played; as microcapsule wall material, method of operating is simple.
Accompanying drawing explanation
Fig. 1 is the thermal analysis curve figure of the microcapsules that OSA starch, xanthans, CLA and embodiment 1 obtains;
Fig. 2 is the infrared spectrogram of the obtained microcapsule wall material of the physical mixture of OSA starch and xanthans, xanthans, OSA starch and embodiment 1;
Fig. 3 is the head space oxygen content change curve of the obtained microcapsules of embodiment 2 and comparative example 2 and CLA;
The preparation curve map of microcapsules CLA in SGF system that Fig. 4 (A) obtains for embodiment 1 and comparative example 1;
The preparation curve map of microcapsules CLA in simulated intestinal fluid system that Fig. 4 (B) obtains for embodiment 1 and comparative example 1.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is specifically described.
Embodiment 1
Embed a preparation method for the microcapsules of CLA, the method is with starch octenyl succinate anhydride and xanthans for primary raw material, and concrete steps are as follows:
(1) 0.4455g xanthans is dispersed in 506.25g water, stirs 60min, make colloidal dispersions even, obtained colloidal solution;
(2) take 44.55g starch octenyl succinate anhydride (OSA starch), add the colloidal solution that step (1) is obtained, stir and make sample mix even, the combination solution of obtained starch octenyl succinate anhydride and xanthans; The mass ratio of starch octenyl succinate anhydride and xanthans is 100:1;
(3) in the combination solution that step (2) is obtained, add 11.25g CLA, use high-speed shearing machine high speed shear to obtain coarse emulsion, high-pressure homogeneously obtain emulsion; The speed of described high speed shear is 20000r/min, and shear time is 2min; Described high-pressure homogeneous pressure is 50MPa, and homogenization cycles is 5 times; The solid content of described emulsion is 10%;
(4) emulsion that step (3) is obtained is carried out spraying dry, the microcapsules of obtained described embedding CLA; Described spray-dired process conditions are: EAT 160 DEG C, leaving air temp 75 DEG C, charging rate 20mL/min.
Embodiment 2
A kind of preparation method embedding the microcapsules of CLA, the method with starch octenyl succinate anhydride and xanthans for primary raw material, concrete steps are with embodiment 1, and difference is: the consumption of xanthans is 0.3719g, and the consumption of starch octenyl succinate anhydride is 44.63g; The i.e. mass ratio 120:1 of starch octenyl succinate anhydride and xanthans.
Embodiment 3
Embed a preparation method for the microcapsules of CLA, the method is with starch octenyl succinate anhydride and xanthans for primary raw material, and concrete steps are as follows:
(1) 0.4455g xanthans is dispersed in 506.25g water, stirs 90min, make colloidal dispersions even, obtained colloidal solution;
(2) take 44.55g starch octenyl succinate anhydride, add the colloidal solution that step (1) is obtained, make sample mix even in stirring, the combination solution of obtained starch octenyl succinate anhydride and xanthans; The mass ratio of starch octenyl succinate anhydride and xanthans is 100:1;
(3) in the combination solution that step (2) is obtained, add 11.25g CLA, use high-speed shearing machine high speed shear to obtain coarse emulsion, high-pressure homogeneously obtain emulsion; The speed of described high speed shear is 11000r/min, and shear time is 4min; Described high-pressure homogeneous pressure is 70MPa, and homogenization cycles is 3 times; The solid content of described emulsion is 10%;
(4) emulsion that step (3) is obtained is carried out spraying dry, the microcapsules of obtained described embedding CLA; Described spray-dired process conditions are: EAT 190 DEG C, leaving air temp 80 DEG C, charging rate 20mL/min.
Embodiment 4
Embed a preparation method for the microcapsules of CLA, the method is with starch octenyl succinate anhydride and guar gum for primary raw material, and concrete steps are as follows:
(1) 0.2486g guar gum is dispersed in 506.25 water, stirs 60min, make colloidal dispersions even, obtained colloidal solution;
(2) take 44.75g starch octenyl succinate anhydride, add the colloidal solution that step (1) is obtained, stir and make sample mix even, the combination solution of obtained starch octenyl succinate anhydride and guar gum; The mass ratio of starch octenyl succinate anhydride and guar gum is 180:1;
(3) in the combination solution that step (2) is obtained, add 11.25g CLA, use high-speed shearing machine high speed shear to obtain coarse emulsion, high-pressure homogeneously obtain emulsion; The speed of described high speed shear is 24000r/min, and shear time is 2min; Described high-pressure homogeneous pressure is 30MPa, and homogenization cycles is 5 times; The solid content of described emulsion is 10%;
(4) emulsion that step (3) is obtained is carried out spraying dry, the microcapsules of obtained described embedding CLA; Described spray-dired process conditions are: EAT 180 DEG C, leaving air temp 90 DEG C, charging rate 15mL/min.
Comparative example 1
Embed a preparation method for the microcapsules of CLA, concrete steps are with embodiment 1, and difference is: the consumption of xanthans is 0g; The i.e. mass ratio 100:0 of wherein starch octenyl succinate anhydride and xanthans.
Comparative example 2
Embed a preparation method for the microcapsules of CLA, concrete steps are with embodiment 1, and difference is: the consumption of xanthans is 0g, and the consumption of starch octenyl succinate anhydride is 44.63g; The i.e. mass ratio 120:0 of starch octenyl succinate anhydride and xanthans.
Test case
1, TAS (TGA) is adopted to assess the heat endurance (get 1.0 ~ 2.0mg sample microcapsules and be placed in crucible, scan 500 DEG C with the speed of 10 DEG C/min from 50 DEG C) of microencapsulation CLA the microcapsules obtained by embodiment 1 and raw material starch octenyl succinate anhydride, xanthans and CLA.Test result TGA collection of illustrative plates as shown in Figure 1.
The reacting initial temperature of microcapsules and raw material starch octenyl succinate anhydride, xanthans and CLA is 243.5 DEG C, 226.3 DEG C, 222.2 DEG C, 156.0 DEG C respectively as shown in Figure 1.
2, the wall material of microcapsules obtained after embodiment 1 spraying dry and the physical mixture of raw material starch octenyl succinate anhydride, xanthans and starch octenyl succinate anhydride and xanthans are carried out infrared spectrum detection, test result infrared spectrogram as shown in Figure 2.Wall material absworption peak as seen from Figure 2 after spraying dry moves to low ripple, and this illustrates and defines hydrogen bond between OSA starch and xanthans.
3, the microcapsules that embodiment 2 and comparative example 2 obtain are preserved 0 respectively respectively at 50 DEG C, 4,21,28,45 and 70h after, use Headspace-solid phase microextraction and gas Chromatographic Determination head space oxygen content, obtain microcapsules as shown in Figure 3 under 50 DEG C of conditions, the head space oxygen content of different resting period changes.
Can find that from figure the mass ratio of OSA starch and xanthans in wall material is the oxidation stability that the microcapsules of 120:1 significantly improve CLA; Wherein, after 70h, the head space oxygen content of the CLA consumption embedded through OSA starch and the composite carrier of xanthans is 0.3011O
2/ mol, the head space oxygen content through the CLA consumption of OSA starch embedding is 0.3834O
2/ mol, the head space oxygen content without the CLA consumption of embedding protection is 0.6858O
2/ mol.
4, the microcapsules that embodiment 1 and comparative example 1 obtain are about 2g and are scattered in 900mL, pH is 1.2, in the SGF that temperature is 37 DEG C, turns basket rotating speed 50rpm, simulation gastric environment 2h, respectively 0,15,30,60,90 and 120min time take out 1mL sample, determine the content at 233nm place CLA with ultraviolet specrophotometer after going out CLA with n-hexane extraction, obtain the preparation curve map of CLA in SGF as shown in Fig. 4 (A).Can find that from figure OSA starch and xanthans mass ratio in wall material are that the preparation of the CLA of microcapsules in SGF after 2h of 100:1 and 100:0 is respectively 6.14%, 5.26%.
5, the microcapsules that embodiment 1 and comparative example 1 obtain are about 2g and are scattered in 900mL, pH is 6.8, in the simulated intestinal fluid (PBS containing 450mg pancreatin) that temperature is 37 DEG C, turn basket rotating speed 50rpm, simulation small intestine condition 2h, respectively 0,15,30,60,90 and 120min time take out 1mL sample, determine the content at 233nm place CLA with ultraviolet specrophotometer after going out CLA with n-hexane extraction, obtain the preparation curve map of CLA in simulated intestinal fluid as shown in Fig. 4 (B).Can find that from figure OSA starch and xanthans mass ratio in wall material are that the preparation of the CLA of microcapsules in simulated intestinal fluid after 2h of 100:1 and 100:0 is respectively 76.81%, 45.23%.
Claims (6)
1. embed a preparation method for the microcapsules of CLA, the method for primary raw material, is characterized in that concrete steps are as follows with starch octenyl succinate anhydride and hydrophilic colloid:
(1) hydrophilic colloid is dispersed in water, stirs 15min-90min, make colloidal dispersions even, obtained colloidal solution;
(2) take starch octenyl succinate anhydride, add the colloidal solution that step (1) is obtained, stir and make sample mix even, the combination solution of obtained starch octenyl succinate anhydride and hydrophilic colloid;
(3) in the combination solution that step (2) is obtained, add CLA, use high-speed shearing machine high speed shear to obtain coarse emulsion, high-pressure homogeneously obtain emulsion;
(4) emulsion that step (3) is obtained is carried out spraying dry, the microcapsules of obtained described embedding CLA.
2. preparation method according to claim 1, is characterized in that the mass ratio of starch octenyl succinate anhydride and hydrophilic colloid in described step (2) is 20:1-180:1.
3. preparation method according to claim 1, is characterized in that the ratio of starch octenyl succinate anhydride and hydrophilic colloid quality summation in the consumption of CLA in described step (3) and combination solution is 1:10-1:3; The solid content of described emulsion is 10-15%.
4. preparation method according to claim 1, is characterized in that the speed that described step (3) high speed is sheared is 11000-24000r/min, shear time 2-4min; Described high-pressure homogeneous pressure is 30-70MPa, and homogenization cycles is 3-5 time.
5. preparation method according to claim 1, is characterized in that in described step (4), spray-dired process conditions are: EAT 150-190 DEG C, leaving air temp 75-95 DEG C, charging rate 10-20mL/min.
6. preparation method according to claim 1, is characterized in that described hydrophilic colloid is one or more in guar gum, locust bean gum, tara gum, gellan gum, sodium carboxymethylcellulose, xanthans, sodium alginate, carragheen, Arabic gum, gelatin, pectin.
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| CN201510484137.3A CN105166885A (en) | 2015-08-07 | 2015-08-07 | Conjugated linoleic acid embedded microcapsule preparation method |
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Cited By (11)
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| CN106578141A (en) * | 2016-12-20 | 2017-04-26 | 乌鲁木齐上善元生物科技有限公司 | Conjugated linoleic acid microcapsule and preparation method thereof |
| CN107162719A (en) * | 2017-05-15 | 2017-09-15 | 天长市翔净蔬菜种植发展有限公司 | One kind promotes the growing mixed fertile preparation method of asparagus lettuce |
| CN108642105A (en) * | 2018-04-18 | 2018-10-12 | 江南大学 | A kind of method of enzyme process inclusion tributyrin |
| CN109452621A (en) * | 2018-11-01 | 2019-03-12 | 江南大学 | A kind of pH responsive type starch base microcapsules and preparation method thereof |
| CN110583801A (en) * | 2019-10-17 | 2019-12-20 | 东北农业大学 | Method for preparing powdered oil by compounding octenyl succinic anhydride modified starch and xanthan gum |
| CN110693003A (en) * | 2019-10-23 | 2020-01-17 | 华南理工大学 | Emulsion gel embedded with fat-soluble vitamins and production method thereof based on pulsed electric field |
| CN111196757A (en) * | 2020-01-16 | 2020-05-26 | 中国农业大学 | Antioxidant covalently bound linoleic acid and preparation method and application thereof |
| CN113598376A (en) * | 2021-08-11 | 2021-11-05 | 郑州瑞普生物工程有限公司 | Preparation method of folic acid micro-capsule powder applied to copper ion-containing tablet product |
| WO2023056805A1 (en) * | 2021-10-08 | 2023-04-13 | 天津科技大学 | Preparation method for modified starch-lipid binary complex |
| CN116508760A (en) * | 2023-02-23 | 2023-08-01 | 河北兴柏农业科技股份有限公司 | Spinosad microcapsule powder and preparation method thereof |
| CN116869934A (en) * | 2023-09-06 | 2023-10-13 | 成都自然素生物科技有限公司 | Supermolecule nano colloid of polyphenol substance and preparation method thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106578141A (en) * | 2016-12-20 | 2017-04-26 | 乌鲁木齐上善元生物科技有限公司 | Conjugated linoleic acid microcapsule and preparation method thereof |
| CN107162719A (en) * | 2017-05-15 | 2017-09-15 | 天长市翔净蔬菜种植发展有限公司 | One kind promotes the growing mixed fertile preparation method of asparagus lettuce |
| CN108642105A (en) * | 2018-04-18 | 2018-10-12 | 江南大学 | A kind of method of enzyme process inclusion tributyrin |
| CN109452621B (en) * | 2018-11-01 | 2022-04-15 | 江南大学 | pH-sensitive starch-based microcapsule and preparation method thereof |
| CN109452621A (en) * | 2018-11-01 | 2019-03-12 | 江南大学 | A kind of pH responsive type starch base microcapsules and preparation method thereof |
| CN110583801A (en) * | 2019-10-17 | 2019-12-20 | 东北农业大学 | Method for preparing powdered oil by compounding octenyl succinic anhydride modified starch and xanthan gum |
| CN110693003A (en) * | 2019-10-23 | 2020-01-17 | 华南理工大学 | Emulsion gel embedded with fat-soluble vitamins and production method thereof based on pulsed electric field |
| CN111196757A (en) * | 2020-01-16 | 2020-05-26 | 中国农业大学 | Antioxidant covalently bound linoleic acid and preparation method and application thereof |
| CN113598376A (en) * | 2021-08-11 | 2021-11-05 | 郑州瑞普生物工程有限公司 | Preparation method of folic acid micro-capsule powder applied to copper ion-containing tablet product |
| CN113598376B (en) * | 2021-08-11 | 2023-11-21 | 郑州瑞普生物工程有限公司 | Preparation method of folic acid microcapsule powder applied to copper ion-containing tablet products |
| WO2023056805A1 (en) * | 2021-10-08 | 2023-04-13 | 天津科技大学 | Preparation method for modified starch-lipid binary complex |
| CN116508760A (en) * | 2023-02-23 | 2023-08-01 | 河北兴柏农业科技股份有限公司 | Spinosad microcapsule powder and preparation method thereof |
| CN116508760B (en) * | 2023-02-23 | 2024-03-29 | 河北兴柏农业科技股份有限公司 | Spinosad microcapsule powder and preparation method thereof |
| CN116869934A (en) * | 2023-09-06 | 2023-10-13 | 成都自然素生物科技有限公司 | Supermolecule nano colloid of polyphenol substance and preparation method thereof |
| CN116869934B (en) * | 2023-09-06 | 2023-11-10 | 成都自然素生物科技有限公司 | Supermolecule nano colloid of polyphenol substance and preparation method thereof |
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