CN100506282C - Linseed oil microcapsule powder and preparation method thereof - Google Patents
Linseed oil microcapsule powder and preparation method thereof Download PDFInfo
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- CN100506282C CN100506282C CNB2007100638296A CN200710063829A CN100506282C CN 100506282 C CN100506282 C CN 100506282C CN B2007100638296 A CNB2007100638296 A CN B2007100638296A CN 200710063829 A CN200710063829 A CN 200710063829A CN 100506282 C CN100506282 C CN 100506282C
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- linseed oil
- microcapsule powder
- oil microcapsule
- starch sodium
- octenyl succinate
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 44
- 235000021388 linseed oil Nutrition 0.000 title claims abstract description 43
- 239000000944 linseed oil Substances 0.000 title claims abstract description 43
- 239000000843 powder Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000839 emulsion Substances 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000002775 capsule Substances 0.000 claims abstract description 20
- 238000001694 spray drying Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000004108 freeze drying Methods 0.000 claims abstract description 9
- 239000001334 starch sodium octenyl succinate Substances 0.000 claims description 35
- 235000013826 starch sodium octenyl succinate Nutrition 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 5
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- 235000013305 food Nutrition 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 230000036541 health Effects 0.000 abstract description 3
- 150000004676 glycans Chemical class 0.000 abstract description 2
- 229920001282 polysaccharide Polymers 0.000 abstract description 2
- 239000005017 polysaccharide Substances 0.000 abstract description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical class C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract 2
- 229920002472 Starch Polymers 0.000 abstract 2
- 125000003342 alkenyl group Chemical group 0.000 abstract 2
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 abstract 2
- 239000011734 sodium Chemical class 0.000 abstract 2
- 229910052708 sodium Inorganic materials 0.000 abstract 2
- 235000019698 starch Nutrition 0.000 abstract 2
- 239000008107 starch Substances 0.000 abstract 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 abstract 2
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 24
- 210000003022 colostrum Anatomy 0.000 description 14
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- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 8
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- 239000001785 acacia senegal l. willd gum Substances 0.000 description 4
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 4
- 235000019165 vitamin E Nutrition 0.000 description 4
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- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 2
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- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 2
- 235000014593 oils and fats Nutrition 0.000 description 2
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- 208000004930 Fatty Liver Diseases 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 206010019708 Hepatic steatosis Diseases 0.000 description 1
- 208000035150 Hypercholesterolemia Diseases 0.000 description 1
- 229920002774 Maltodextrin Polymers 0.000 description 1
- 239000005913 Maltodextrin Substances 0.000 description 1
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- 230000002209 hydrophobic effect Effects 0.000 description 1
- -1 linolenic acid Chemical class 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
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- 150000003180 prostaglandins Chemical class 0.000 description 1
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Landscapes
- General Preparation And Processing Of Foods (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Medicinal Preparation (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The present invention is linseed oil microcapsule powder and its preparation, and features that modified polysaccharide, sodium octyl alkenyl succinate starch, is used as capsule wall material for forming microcapsule in preparing linseed oil microcapsule powder. The preparation process includes adding linseed oil into the solution of sodium octyl alkenyl succinate starch, stirring to form homogeneous emulsion, high pressure homogenizing to obtain linseed oil emulsion of granularity smaller than 1000 nm, and final spray drying or freeze drying to obtain white linseed oil microcapsule powder with high stability and high flowability. The linseed oil microcapsule powder has high linseed oil activity, high stability and high bioavailability, and may be applied in food and health product.
Description
Technical field
The present invention relates to food and field of health care products, is specifically related to linseed oil microcapsule powder and preparation method thereof.
Background technology
Oleum lini mainly is that linum mainly is distributed in North China and the Northwest by the linum squeezing, and the oleum lini by the linum squeezing makes mainly contains unsaturated fatty acids such as linolenic acid, wherein contains the alpha-linolenic acid more than 50%.
Human daily life must comprise satisfied fatty acid and monovalence unsaturated fatty acid series by fatty acid, linoleic acid (ω-6 series) and alpha-linolenic acid series (ω-3 series), human body self can synthesizing saturated fatty acid and monovalence unsaturated fatty acid, but can not synthesize linoleic acid and alpha-linolenic acid, can only from food, absorb.Alpha-linolenic acid have suppress anaphylaxis antiinflammatory action, vision protection, nootropics improving memory, suppress old and feeble, blood fat reducing prevents arteriosclerosis, prevent effect such as cardiovascular and cerebrovascular disease.The shortage of alpha-linolenic acid can cause that growth promoter is slow, may cause diseases such as neurodermatitis, hypercholesterolemia, fatty liver, prostaglandin metabolism disorder, visual function disorder when serious, in case long-term lacking might cause the infringement of brain persistence, cause serious consequences such as hypomnesis, senile dementia, mental retardation.Important function and human body based on alpha-linolenic acid generally absorb insufficient situation, the special alpha-linolenic acid that replenishes of FAO of the United Nations in 1993 and WHO suggestion.It is about 50% that oleum lini contains alpha-linolenic acid, can be used as the alpha-linolenic acid supply source.But there are some shortcomings in oleum lini: abnormal smells from the patient is not good; Unsaturated fatty acid content is higher, easily causes oxidative rancidity; Oils and fats as adding in the food is difficult for mixing, and bioavailability is not high.
Microcapsule technology is that a kind of filmogen of using coats the technology that forms fine particle to solid or liquid, and this technology reaches its maturity through the continuous development of decades.In industrial circles such as pharmacy, food, agricultural chemicals, spice, feed additive and household chemicals, be used widely.In recent years, microcapsule technology is one of focus that attracts people's attention in high added value oil and fat product preparation field.Oils and fats by micro encapsulation after, can reduce greasy thermal sensitivity, prevent that the heliosensitivity liposoluble constituent is damaged, thereby improve trophism, flavor stability and the bioavailability of oil product.
Document " research of an oleum lini powdered oil preparation " literary composition has reported that with gelatin, arabic gum be main wall material, adopts the complex coacervation principle, and oleum lini is carried out micro encapsulation.Need to carry out chemosetting in the preparation process and handle, this brings very big influence to product quality.In addition, after this product was placed through the long period, mobile variation was prone to caking in various degree.
The open CN1222278C of Chinese patent has reported that employing arabic gum, maltodextrin and modified starch prepare alpha-linolenic acid microcapsule as the capsule material.In preparation method, the core preparation need add monoglyceride emulsifying alpha-linolenic acid under 60～70 ℃ of conditions, and preparation capsule material is wide in variety.
Parcel capsule material has all adopted multiple materials such as arabic gum in above-mentioned document and the patent, and this is disadvantageous to control of product quality, because high concentration arabic gum solution viscosity is bigger, brings very big inconvenience to spray drying; Patent CN1222278C temperature is too high, causes that easily the alpha-linolenic acid oxidation loses activity, but also adds the monoglyceride emulsifying agent.Therefore need to seek a kind of suitable single material (its high concentration solution's viscosity is low) and under cryogenic conditions, prepare good stability, mobile big high-quality linseed oil microcapsule powder as parcel capsule material.
Summary of the invention
The purpose of this invention is to provide a kind of linseed oil microcapsule powder and preparation method thereof, by single starch sodium octenyl succinate as the capsule material, at a lower temperature oleum lini is carried out micro encapsulation, solution contains the caking of the powder product of oleum lini, the problem of mobile difference, thereby prepares a kind of stability height, good fluidity and can better keep the active linseed oil microcapsule powder of oleum lini.
Technical scheme of the present invention is:
A kind of linseed oil microcapsule powder, it is characterized in that: this linseed oil microcapsule powder is made up of 1 weight portion core and 0.6～9 weight portion capsule material, core is an oleum lini, and the capsule material is a starch sodium octenyl succinate, and the mean diameter that is scattered in the oleum lini in the capsule material is less than 1000nm.
Technical characterictic of the present invention also is: the oleum lini mean diameter that is scattered in the capsule material starch sodium octenyl succinate is 100～500nm.
In order further to improve the oxidation resistance of product itself, prevent that the unsaturated fatty acid in the oleum lini is oxidized, increase the stability of oleum lini, the present invention also can add 0.1～0.5 weight portion vitamin E as required in core.
The present invention also provides a kind of preparation method of described linseed oil microcapsule powder, it is characterized in that this method carries out as follows:
1) takes by weighing 0.6～9 weight portion starch sodium octenyl succinate and add in the entry, under 70～80 ℃ of conditions, be stirred to starch sodium octenyl succinate and dissolve fully, form 30%～60% starch sodium octenyl succinate aqueous solution;
2) with 1) in the starch sodium octenyl succinate aqueous solution that forms be cooled to 30～40 ℃, in this solution, add 1 weight portion oleum lini then, stir and form homogenous emulsion;
3) with 2) through high pressure homogenizer homogenizing circulation 3～8 times, formation oleum lini mean diameter is less than the emulsion of 1000nm under 500～1500bar pressure for the middle emulsion that forms;
4) with 3) in the emulsion that forms carry out spray-drying process, promptly obtain linseed oil microcapsule powder; Perhaps with 3) in the emulsion that forms carry out lyophilization, then with lyophilisation product through pulverizing pelletization treatment, promptly obtain linseed oil microcapsule powder.
Linseed oil microcapsule powder of the present invention adopts single capsule material successfully to prepare oleum lini droplet particle diameter less than the 1000nm linseed oil microcapsule 30～40 ℃ of conditions, this capsule material is selected a kind of modification of polysaccharides---starch sodium octenyl succinate that is applied to food by whole world approval for use, this class polysaccharide molecular weight is big, forms the very big thin film of one deck intensity at the oil-water interfaces place.The linseed oil microcapsule powder of preparing by the present invention has prevented the unsaturated fatty acid oxidative rancidity in the oleum lini effectively, increased the stability of oleum lini, keep the activity of oleum lini, covered oleum lini abnormal smells from the patient offensively, improved the oleum lini bioavailability; Store convenient transportation, and be easy to add in food and the health product.
The specific embodiment
Linseed oil microcapsule powder provided by the present invention is made up of 1 weight portion core and 0.6～9 weight portion capsule material, and core is an oleum lini, and the capsule material is a starch sodium octenyl succinate.Core is that tunica material starch sodium octenyl succinate is wrapped in, and insert in the core oleum lini hydrophobic end of starch sodium octenyl succinate, and the direction of water-wet side directed in opposite.Be scattered in oleum lini mean diameter in the capsule material less than 1000nm.
By ratio optimization to core and capsule material, and optimization of preparation, the oleum lini mean diameter that is scattered in this linseed oil microcapsule in the capsule material is 100～500nm.
Linseed oil microcapsule powder of the present invention can add 0.1～0.5 weight portion vitamin E as required in core, and the one, the oxidation resistance of raising product itself, the 2nd, prevent that further the unsaturated fatty acid in the oleum lini is oxidized, increase the stability of oleum lini.
The preparation method of linseed oil microcapsule powder of the present invention is characterized in that: preparation method is made up of following steps:
1) takes by weighing 0.6～9 weight portion starch sodium octenyl succinate and add in the entry, under 70～80 ℃ of conditions, be stirred to starch sodium octenyl succinate and dissolve fully, form 30%～60% starch sodium octenyl succinate aqueous solution.
2) with 1) in the starch sodium octenyl succinate aqueous solution that forms be cooled to 30～40 ℃, in this solution, add 1 weight portion oleum lini then, stir and form homogenous emulsion.
3) with 2) through high pressure homogenizer homogenizing circulation 3～8 times, formation oleum lini mean diameter is less than the emulsion of 1000nm under 500～1500bar pressure for the middle emulsion that forms.
4) with 3) in the emulsion that forms carry out spray-drying process, promptly obtain linseed oil microcapsule powder; Perhaps with 3) in the emulsion that forms carry out lyophilization, then with lyophilisation product through pulverizing pelletization treatment, promptly obtain linseed oil microcapsule powder.
Preparation method step 4) spray drying condition is as follows: 180～230 ℃ of inlet temperature, 40～80 ℃ of leaving air temps; The lyophilization temperature is-40～-80 ℃.
Below enumerate seven embodiment to being described further in the claim scope of the present invention:
Embodiment 1 takes by weighing 0.6 weight portion starch sodium octenyl succinate and adds in 2 weight parts waters, stirs to form the starch sodium octenyl succinate aqueous solution under 70 ℃ of conditions; This solution is cooled to 40 ℃, in this solution, adds 1 weight portion oleum lini then, continue to be stirred to formation oleum lini colostrum; Again this colostrum high pressure homogenize under the 1500bar pressure condition is formed milky emulsion 3 times; At last this milky emulsion is obtained white linseed oil microcapsule powder by spray drying, inlet temperature is 190 ℃, and leaving air temp is 50 ℃.Measuring this milky emulsion mean diameter by laser particle analyzer is 718nm.
Embodiment 2 takes by weighing 1 weight portion starch sodium octenyl succinate and adds in 3 weight parts waters, stirs to form the starch sodium octenyl succinate aqueous solution under 75 ℃ of conditions; This solution is cooled to 35 ℃, in this solution, adds 1 weight portion oleum lini then, continue to be stirred to formation oleum lini colostrum; Again this colostrum high pressure homogenize under the 800bar pressure condition is formed milky emulsion 4 times; At last this milky emulsion is obtained white linseed oil microcapsule powder by spray drying, inlet temperature is 190 ℃, and leaving air temp is 40 ℃.Measuring this milky emulsion mean diameter by laser particle analyzer is 602nm.
Embodiment 3 takes by weighing 4 weight portion starch sodium octenyl succinate and adds in 10 weight parts waters, stirs to form the starch sodium octenyl succinate aqueous solution under 80 ℃ of conditions; This solution is cooled to 30 ℃, in this solution, adds 1 weight portion oleum lini and 0.1 weight portion vitamin E then, continue to be stirred to formation oleum lini colostrum; Again this colostrum high pressure homogenize under the 1000bar pressure condition is formed milky emulsion 4 times; At last this milky emulsion is obtained white linseed oil microcapsule powder by spray drying, inlet temperature is 200 ℃, and leaving air temp is 60 ℃.Measuring this milky emulsion mean diameter by laser particle analyzer is 448nm.
Embodiment 4 takes by weighing 6 weight portion starch sodium octenyl succinate and adds in 10 weight parts waters, stirs to form the starch sodium octenyl succinate aqueous solution under 80 ℃ of conditions; This solution is cooled to 35 ℃, in this solution, adds 1 weight portion oleum lini and 0.5 weight portion vitamin E then, continue to be stirred to formation oleum lini colostrum; Again this colostrum high pressure homogenize under the 800bar pressure condition is formed milky emulsion 6 times; At last this milky emulsion is obtained white linseed oil microcapsule powder by spray drying, inlet temperature is 210 ℃, and leaving air temp is 60 ℃.Measuring this milky emulsion mean diameter by laser particle analyzer is 332nm.
Embodiment 5 takes by weighing 9 weight portion starch sodium octenyl succinate and adds in 20 weight parts waters, stirs to form the starch sodium octenyl succinate aqueous solution under 75 ℃ of conditions; This solution is cooled to 35 ℃, in this solution, adds 1 weight portion oleum lini then, continue to be stirred to formation oleum lini colostrum; Again this colostrum high pressure homogenize under the 500bar pressure condition is formed milky emulsion 8 times; At last this milky emulsion is obtained white linseed oil microcapsule powder by spray drying, inlet temperature is 230 ℃, and leaving air temp is 80 ℃.Measuring this milky emulsion mean diameter by laser particle analyzer is 204nm.
Embodiment 6 takes by weighing 9 weight portion starch sodium octenyl succinate and adds in 20 weight parts waters, stirs to form the starch sodium octenyl succinate aqueous solution under 75 ℃ of conditions; This solution is cooled to 35 ℃, in this solution, adds 1 weight portion oleum lini then, continue to be stirred to formation oleum lini colostrum; Again this colostrum high pressure homogenize under the 800bar pressure condition is formed milky emulsion 6 times; At last this milky emulsion is obtained block linseed oil microcapsule at-80 ℃ of lyophilization 8h, at last should the bulk linseed oil microcapsule pulverize and obtain linseed oil microcapsule powder through mortar.Measuring this milky emulsion mean diameter by laser particle analyzer is 138nm.
Embodiment 7 takes by weighing 4 weight portion starch sodium octenyl succinate and adds in 10 weight parts waters, stirs to form the starch sodium octenyl succinate aqueous solution under 80 ℃ of conditions; This solution is cooled to 35 ℃, in this solution, adds 1 weight portion oleum lini then, continue to be stirred to formation oleum lini colostrum; Again this colostrum high pressure homogenize under the 1000bar pressure condition is formed milky emulsion 6 times; At last this milky emulsion is obtained block linseed oil microcapsule at-40 ℃ of lyophilization 18h, at last should the bulk linseed oil microcapsule pulverize and obtain linseed oil microcapsule powder through ball mill.Measuring this milky emulsion mean diameter by laser particle analyzer is 221nm.
Claims (2)
1. linseed oil microcapsule powder, it is characterized in that: this linseed oil microcapsule powder is made up of 1 weight portion core and 0.6～9 weight portion capsule material, core is an oleum lini, the capsule material is a starch sodium octenyl succinate, and the oleum lini mean diameter that is scattered in the capsule material starch sodium octenyl succinate is 100～500nm.
2. linseed oil microcapsule powder preparation method as claimed in claim 1 is characterized in that this method carries out as follows:
1) starch sodium octenyl succinate with 0.6～9 weight portion adds in the entry, is stirred to starch sodium octenyl succinate and dissolves fully under 70～80 ℃ of conditions, forms 30%～60% starch sodium octenyl succinate aqueous solution;
2) with 1) in the starch sodium octenyl succinate aqueous solution that forms be cooled to 30～40 ℃, in this solution, add the oleum lini of 1 weight portion then, stir the back and form homogenous emulsion;
3) with 2) through high pressure homogenizer homogenizing circulation 3～8 times, form the oleum lini mean diameter is the emulsion of 100～500nm to the middle emulsion that forms under 500～1500bar pressure;
4) with 3) in the emulsion that forms carry out spray-drying process, promptly obtain linseed oil microcapsule powder; Perhaps with 3) in the emulsion that forms carry out lyophilization, then with cryodesiccated product through pulverizing pelletization treatment, promptly obtain linseed oil microcapsule powder.
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| CNB2007100638296A CN100506282C (en) | 2007-02-12 | 2007-02-12 | Linseed oil microcapsule powder and preparation method thereof |
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| CNB2007100638296A CN100506282C (en) | 2007-02-12 | 2007-02-12 | Linseed oil microcapsule powder and preparation method thereof |
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| CN100506282C true CN100506282C (en) | 2009-07-01 |
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| MX2012010555A (en) * | 2010-03-29 | 2012-10-05 | Firmenich & Cie | Spray-dried crystalline active ingredient. |
| CN101919454B (en) * | 2010-08-16 | 2013-05-01 | 苏州市佳禾食品工业有限公司 | Acid-resistant non-dairy creamer and preparation method thereof |
| CN102048159B (en) * | 2010-11-15 | 2013-02-13 | 清华大学 | Camellia oil microcapsule powder and preparation method thereof |
| CN102177980A (en) * | 2011-04-08 | 2011-09-14 | 清华大学 | Maize germ oil microcapsule powder and preparation method thereof |
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