CN101856125A - Spray freeze-drying preparation technology for polyunsaturated fatty acid oil microcapsule - Google Patents
Spray freeze-drying preparation technology for polyunsaturated fatty acid oil microcapsule Download PDFInfo
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Abstract
The invention relates to a spray freeze-drying preparation technology for a polyunsaturated fatty acid oil microcapsule, which comprises the following technological steps: mixing oil containing polyunsaturated fatty acid with emulsifier and water to obtain mixture; homogenizing the mixture to obtain emulsion; atomizing the emulsion into liquid drops which are sprayed into a spray drying device with temperature of negative 60 DEG C to negative 10 DEG C, wherein powder embedding materials are contained at the bottom part of the spray drying device, and blasting low-temperature gas to fully mix the materials in the spray drying device and to keep the temperature in the spray drying device to be the set temperature; and further drying and screening to obtain polyunsaturated fatty acid oil microcapsule products. The invention has the advantages that the drying temperature of the preparation technology is low, the speed is fast and the nutritional ingredients are not apt to be damaged; the technology is simple and convenient and the automatic mass production can be realized; and the oil embedding rate of the obtained independent polyunsaturated fatty acid oil microcapsule particles is high, the embedding performance is good, the product shelf life is long and the stability is good.
Description
Technical field
The present invention relates to a kind of spray freeze-drying preparation technology of polyunsaturated fatty acid grease microcapsules.
Background technology
The polyunsaturated fatty acid that studies show that in recent years is very important to the health of human body, therefore has a large amount of enterprises to develop the product of multiple unrighted acid.
Polyunsaturated fatty acid (Polyunsaturated fatty acids, PUFA) be meant and contain two or more pairs key and carbon chain length is the straight chain fatty acid of 18～22 carbon atoms, mainly comprise linoleic acid (LA), gamma-Linolenic acid (GLA), arachidonic acid (AA), eicosapentaenoic acid (EPA) and DHA (DHA) etc., wherein, n-3 and n-6 series polyunsaturated fatty acid are as human essential fatty acid, in Human Physiology, bringing into play very crucial effect, mainly show: cardiovascular disease, preventing of diseases such as cancer, aspects such as the growth of promotion physiological cells and immunological regulation.Can generate prostaglandin (PGI2) in vivo as gamma-Linolenic acid (GLA), make TXA2 and PGI2 keep relative equilibrium, thus the formation of anti-tampon; DHA and EPA have the good anticancer effect; Polyunsaturated fatty acids such as arachidonic acid, EPA and DHA can influence the difference in functionality of various kinds of cell.Wherein n-3 is that the effect of aliphatic acid is more extensive, and the generation that it can regulate eicosanoid by immune cell especially reduce the generation of proinflammatory factor PGE2 and leukotriene B4; Regulate membrane fluidity; Regulate the cellular signal transduction approach, especially with lipid medium, protein kinase C and Ca
2+Mobilize relevant approach; Regulate with cell factor generating or peroxidating body propagation, fatty acid oxidation lipoprotein is assembled with the expression of correlation gene; Remove this, polyunsaturated fatty acid can also prevent skin aging, delays senility, antianaphylaxis and promote hair growth etc.
Microcapsules technology be meant utilize filmogen with solid, liquid or gas pockets in wherein, form the technology of the small container of tens microns to thousands of microns of diameters, the inner material that loads of microcapsules is called core (or claiming core material), and the wall film of outside packing is called wall material (or claiming coating material).Through the continuous development of decades, microcapsules technology reaches its maturity, and is widely used in industrial circles such as pharmacy, food, agricultural chemicals, spices, feed addictive and household chemicals.Wherein, microcapsules technology especially attracts people's attention in the preparation field of high added value oil and fat product.Behind microencapsulation, the thermal sensitivity of grease and light sensitivity reduce, thereby can prevent that liposoluble constituent is damaged, and improve trophism, flavor stability and the bioavilability of oil product.
At present, the polyunsaturated fatty acid microencapsulation generally all is to adopt the high temperature spray-drying method, and it is with low cost, and technology is simple, is easy to large-scale industrial production, but evaporates temperature required height, the easy inactivation of active component, and the slit is easily arranged on the cyst wall, compactness is poor.Application number is to relate to the technology that a kind of atomizing freeze drying prepares powder in the patent of 200810195187.X, needs strict control baking temperature in dry run, otherwise product can be sticked together after melting, and influences drying effect and final yield.
Summary of the invention
Technical problem to be solved by this invention provides a kind of spray freeze-drying preparation technology of polyunsaturated fatty acid grease microcapsules, and this preparation technology's baking temperature is low, and speed is fast, and nutritional labeling is difficult for being damaged; Technology is easy, can realize automatic mass production; The independently polyunsaturated fatty acid grease microcapsules particle that obtains, grease embedding rate height, embeddability properties is good, and the product shelf life is long, good stability.
For solving the technical problem that the present invention proposes, the technical solution used in the present invention is:
A kind of spray freeze-drying preparation technology of polyunsaturated fatty acid grease microcapsules is characterized in that: grease, emulsifying agent and the water that will contain polyunsaturated fatty acid mix, and obtain mixture; With the mixture homogeneous, obtain emulsion; Emulsion is atomized into drop, and to be injected to temperature be in-60 ℃～-10 ℃ the spray drying device, powder embedding material is equipped with in the spray drying device bottom, by blasting cryogenic gas, making the interior material of spray drying device fully mix and can keep the interior temperature of spray drying device is design temperature simultaneously; Further dry then, screening obtains the polyunsaturated fatty acid grease microcapsules product.
Press such scheme, described mixture also comprises antioxidant, filler; Described mixture by weight percentage, its mixing match is: polyunsaturated fatty acid 10～30%, emulsifying agent 2～30%, antioxidant 0～0.5%, filler 0～30%, water 30～70%.
Press such scheme, described emulsifying agent is one or more the mixing in vegetable protein, casein, casein sodium, converted starch, lactalbumin, the food-grade glue; Described filler is one or more mixing of maltodextrin, glucose, sucrose; Described antioxidant is multiple or a kind of mixing of sodium ascorbate, vitamin E, ascorbyl palmitate, Tea Polyphenols.
Press such scheme, described mixing temperature is preferably 30～80 ℃.
Press such scheme, the atomizing type of described emulsion is pressure type atomizing, centrifugal spraying or air-blast atomization; The atomizing pressure of described pressure type atomizing is 0.5MPa～2MPa; The stream pressure of air-blast atomization is 0.01～0.2MPa.Adopt this atomization condition, the final products particle size range that obtains can be controlled between 50～400 μ m.
Press such scheme, described powder embedding material is one or more the mixing in starch, microcrystalline cellulose, tricalcium phosphate, calcium carbonate, agar powder, the maltodextrin; The weight proportion of described powder embedding material and emulsion is 10: 1～1: 2.
Press such scheme, described powder embedding material joins in the spray drying device when blasting cryogenic gas continuously or off and on.
Press such scheme, described further drying is to change external fluidized bed drying over to or change vacuum drying system over to carry out vacuum freeze drying, and the final temperature of wherein said external fluidized bed drying is no more than 60 ℃; The final temperature of vacuum freeze drying is no more than 60 ℃.
Press such scheme, in the polyunsaturated fatty acid grease microcapsules product that the spray freeze-drying preparation technology of described polyunsaturated fatty acid grease microcapsules obtains, powder embedding material shared percentage by weight in final products is 20～50%.
Beneficial effect of the present invention:
(1) this preparation technology has adopted a kind of new dry technology, promptly in temperature is-60 ℃～-10 ℃ spray drying device, the drop low temperature of atomizing is solidified, by one deck powder embedding material parcel, change fluidized bed drying or vacuum drying system then over to and carry out vacuum drying simultaneously, obtain the polyunsaturated fatty acid grease microcapsules product, its baking temperature is low, rate of drying is fast, and polyunsaturated fatty acid is difficult for oxidation, and nutritional labeling is difficult for being damaged;
(2) the independently polyunsaturated fatty acid grease microcapsules granule interior densification that obtains, tight, grease embedding rate height;
(3) emulsion is being atomized into when drop is injected in the spray drying device, adopt powder embedding material that polyunsaturated fatty acid is carried out the secondary embedding, grease embedding rate and grease embeddability properties have been improved, completely cut off contacting of polyunsaturated fatty acid and air effectively, improve the quality of product, thereby further improved the product shelf life and the stability of this oil product;
(4) use vacuum drying process further dry, product drying speed is faster, thereby effectively cuts down the consumption of energy, and improves the quality of products;
(5) less demanding to temperature controlling, technology is simple, can realize automatic mass production.
Description of drawings
Fig. 1 is the spray freeze-drying preparation technology flow chart of polyunsaturated fatty acid grease microcapsules.
The specific embodiment
In order to understand the present invention better, below in conjunction with accompanying drawing and several embodiment, further illustrate content of the present invention, but content of the present invention not only is confined to the following examples.
Embodiment 1
| Arachidonic acid content | Casein sodium | Lactalbumin | Maltodextrin | Ascorbyl palmitate | Water |
| ??500g | ??30g | ??400g | ??400g | ??10g | ??1000g |
To go up the table batching after 60 ℃ of mixing, adopt the homogenization pressure homogeneous of 40MPa, form uniform emulsion; Use high-pressure pump then, emulsion is sprayed in the spray drying device of having lowered the temperature for drop by the atomizing lance atomizing, the atomizing pressure of wherein said pressure type atomizing is 1MPa, temperature in the spray drying device is-20 ℃, the spray drying device bottom is equipped with the maltodextrin of 2000g in advance, blasting cryogenic gas simultaneously is design temperature-20 ℃ to keep temperature in the spray drying device, make the drop of atomizing in spray drying device, be frozen into solid particle, and coated by maltodextrin, treat that emulsion all is pressed into spray drying device after; All materials are transferred in the vacuum freeze, regulate the interior absolute pressure of vacuum dryer below 50Pa, and along with drying is carried out, progressively heighten baking temperature, guarantee that final temperature is not more than 60 ℃, add up to dry 10h, take out dried material, screening, isolate unnecessary powder embedding material maltodextrin, be about to it and use 60 mesh standard sieves to sieve earlier, then the screenings that obtains (granularity is passed sieve aperture less than the material of sieve aperture becomes screenings) is sieved through 100 mesh standard sieves, the oversize that obtains (granularity then resides in compass screen surface greater than the material of sieve aperture becomes oversize) is the arachidonic acid microcapsule product.
Detect:
| Arachidonic acid content | Yield | Moisture | The grease embedding rate |
| ??10.32％ | ??98％ | ??2.2％ | ??99.88％ |
Embodiment 2
| Arachidonic acid content is 40% grease | Arabic gum | Casein sodium | Converted starch | Maltodextrin | Tea Polyphenols | Vitamin E | Water |
| ??50Kg | ??1Kg | ??3Kg | ??10Kg | ??60Kg | ??0.5Kg | ??0.5Kg | ??150Kg |
The batching of last table after 40 ℃ of mixing, is adopted the homogenization pressure homogeneous of 60MPa, form uniform emulsion; Use high-pressure pump then, emulsion is atomized into drop by atomizing lance to spray in the spray drying device of having lowered the temperature, the atomizing pressure of wherein said pressure type atomizing is 1.5MPa, temperature in the spray drying device is-30 ℃, the starch of 100Kg is housed in the spray drying device in advance, blasting cryogenic gas simultaneously is design temperature-30 ℃ to keep temperature in the spray drying device, makes the drop of atomizing be frozen into solid particle in spray drying device, and is coated by starch; At the same time, the material that will solidify is sent constantly in the external fluid bed, use-30 ℃～-10 ℃ over dry air to carry out fluidized drying, finish until drying, constantly send into 200kg starch in the spray drying device simultaneously, replenish with material and be transferred to starch loss in the fluid-bed process, the finished product that drying is obtained is admitted to screening system and separates, is packaged to be the arachidonic acid microcapsule product.Isolated starch directly returned in the spray drying device recycle.
Detect:
| Arachidonic acid content | Yield | Moisture | The grease embedding rate |
| ??11.0％ | ??99％ | ??2.4％ | ??99.9％ |
Embodiment 3
| DHA content is 35% grease | Pea protein | Converted starch | Maltodextrin | Sodium ascorbate | Water |
| ??60Kg | ??25Kg | ??6Kg | ??50Kg | ??1Kg | ??100Kg |
Behind 80 ℃ of mixing and emulsifyings, homogeneous under the homogenization pressure of 80MPa forms uniform emulsion with the batching of last table; Be drop with emulsion by centrifugal atomizing with pump then, enter in the spray drying device of having lowered the temperature, the centrifugal pan rotating speed of wherein said centrifugal spraying is 3000～4500rpm/min, temperature in the spray drying device is-40 ℃, the tricalcium phosphate that adds 150Kg in the spray drying device in advance, blasting cryogenic gas simultaneously is design temperature-40 ℃ to keep temperature in the spray drying device, make the drop of atomizing in spray drying device, be frozen into solid particle, and coated by tricalcium phosphate; At the same time, the material that will solidify is sent constantly into the continous vacuum freeze drying equipment, vacuum freeze drying 10 hours is constantly sent into the 200kg tricalcium phosphate in the spray drying device simultaneously, replenishes the tricalcium phosphate that is transferred in the vacuum freeze process with material and loses; The finished product that drying is obtained is sent into screening system and is separated, is packaged to be the DHA microcapsule product.Isolated tricalcium phosphate returned in the spray drying device recycle.
Detect:
| DHA content | Yield | Moisture | The grease embedding rate |
| ??11.5％ | ??99％ | ??2.2％ | ??99.91％ |
Embodiment 4
Table 4
| DHA content is 35% grease | Lactalbumin | Casein sodium | Converted starch | Maltodextrin | Tea Polyphenols | Water |
| ??60Kg | ??28Kg | ??3Kg | ??3Kg | ??50Kg | ??1Kg | ??90Kg |
With the described batching of table 4 70 ℃ of mixing, homogeneous under the homogenization pressure of 80MPa, form uniform emulsion, by delivery pump feed liquid is sent into atomizing lance, under the stream pressure of 0.05～0.1MPa, is that drop sprays in the spray drying device of having lowered the temperature with pure air with the feed liquid atomizing, wherein the temperature in the spray drying device is-50 ℃, the microcrystalline cellulose that adds 100Kg in the spray drying device in advance, blasting cryogenic gas simultaneously is design temperature-50 ℃ to keep temperature in the spray drying device, make the drop of atomizing in spray drying device, be frozen into solid particle, and coated by microcrystalline cellulose; At the same time, the material that will solidify is sent constantly into the continous vacuum freeze drying equipment, vacuum freeze drying 10 hours is constantly sent into microcrystalline cellulose 300kg in the spray drying device simultaneously, replenishes the microcrystalline cellulose that is transferred in the vacuum freeze process with material and loses; The finished product that drying is obtained is sent into screening system and is separated, is packaged to be the docosahexaenoic acid grease microcapsule product.Isolated microcrystalline cellulose returned in the spray drying device recycle.
Detect:
| DHA content | Yield | Moisture | The grease embedding rate |
| ??11.4％ | ??99％ | ??2.3％ | ??99.85％ |
Embodiment 5
Table 5
| Arachidonic acid content is 40% grease | Lactalbumin | Casein sodium | Sucrose | Vitamin E | Water |
| ??50Kg | ??7Kg | ??7Kg | ??70Kg | ??1Kg | ??110Kg |
With above-mentioned batching 60 ℃ of mixing, homogeneous under the homogenization pressure of 120MPa, form uniform emulsion, use high-pressure pump then, emulsion is sprayed in the spray drying device of having lowered the temperature for drop by the atomizing lance atomizing, the atomizing pressure of wherein said pressure type atomizing is 2MPa, temperature in the spray drying device is-60 ℃, the starch that adds 100Kg in the spray drying device in advance, blasting cryogenic gas simultaneously is design temperature-60 ℃ to keep temperature in the spray drying device, make the drop of atomizing in spray drying device, be frozen into solid particle, and coated by starch, at the same time, the material that will solidify is sent constantly into the continous vacuum freeze drying equipment, and vacuum freeze drying 10 hours is constantly sent into starch 200kg in the spray drying device simultaneously, replenish with material and be transferred to starch loss in the vacuum freeze process, the finished product that drying is obtained is sent into screening system and is separated, be packaged to be the arachidonic acid microcapsule product.Isolated starch returned in the spray drying device recycle.
Detect:
| Arachidonic acid content | Yield | Moisture | The grease embedding rate |
| ??12.3％ | ??99％ | ??2.4％ | ??99.88％ |
Powder embedding material starch described in embodiment 2 and the embodiment 5 is the two starch of cornstarch or acetylation adipic acid.In the polyunsaturated fatty acid grease microcapsules product that the foregoing description 1～5 obtains: arachidonic acid or DHA content are the percetage by weight of arachidonic acid or DHA in the polyunsaturated fatty acid grease microcapsules product; Contain the weight that contains the grease of polyunsaturated fatty acid in the weight/raw material of grease of polyunsaturated fatty acid in yield=polyunsaturated fatty acid grease microcapsules product; Moisture is the percetage by weight of water in the polyunsaturated fatty acid grease microcapsules product; The grease embedding rate is a percetage by weight.
Claims (10)
1. the spray freeze-drying preparation technology of a polyunsaturated fatty acid grease microcapsules is characterized in that: will contain grease, emulsifying agent and the water of polyunsaturated fatty acid, and obtain mixture; With the mixture homogeneous, obtain emulsion; Emulsion is atomized into drop, and to be injected to temperature be in-60 ℃～-10 ℃ the spray drying device, powder embedding material is equipped with in the spray drying device bottom, by blasting cryogenic gas, making the interior material of spray drying device fully mix and can keep the interior temperature of spray drying device is design temperature simultaneously; Further dry then, screening obtains the polyunsaturated fatty acid grease microcapsules product.
2. the spray freeze-drying preparation technology of polyunsaturated fatty acid grease microcapsules according to claim 1 is characterized in that: described emulsifying agent is one or more the mixing in vegetable protein, casein, casein sodium, converted starch, lactalbumin, the food-grade glue.
3. the spray freeze-drying preparation technology of polyunsaturated fatty acid grease microcapsules according to claim 1, it is characterized in that: described mixture also comprises antioxidant, filler; Described mixture by weight percentage, its mixing match is: the grease 10～30%, emulsifying agent 2～30%, antioxidant 0～0.5%, filler 0～30%, the water 30～70% that contain polyunsaturated fatty acid.
4. the spray freeze-drying preparation technology of polyunsaturated fatty acid grease microcapsules according to claim 3 is characterized in that: described filler is one or more mixing of maltodextrin, glucose, sucrose; Described antioxidant is multiple or a kind of mixing of sodium ascorbate, vitamin E, ascorbyl palmitate, Tea Polyphenols.
5. the spray freeze-drying preparation technology of polyunsaturated fatty acid grease microcapsules according to claim 1, it is characterized in that: described mixing temperature is 30～80 ℃.
6. the spray freeze-drying preparation technology of polyunsaturated fatty acid grease microcapsules according to claim 1, it is characterized in that: the atomizing type of described emulsion is pressure type atomizing, centrifugal spraying or air-blast atomization; The atomizing pressure of described pressure type atomizing is 0.5MPa～2MPa; The stream pressure of air-blast atomization is 0.01～0.2MPa.
7. the spray freeze-drying preparation technology of polyunsaturated fatty acid grease microcapsules according to claim 1 is characterized in that: described powder embedding material is one or more the mixing in starch, microcrystalline cellulose, tricalcium phosphate, calcium carbonate, agar powder, the maltodextrin; The weight proportion of described powder embedding material and emulsion is 10: 1～1: 2.
8. the spray freeze-drying preparation technology of polyunsaturated fatty acid grease microcapsules according to claim 1, it is characterized in that: described powder embedding material joins in the spray drying device when blasting cryogenic gas continuously or off and on.
9. the spray freeze-drying preparation technology of polyunsaturated fatty acid grease microcapsules according to claim 1, it is characterized in that: described further drying is to change external fluidized bed drying over to or change vacuum drying system over to carry out vacuum freeze drying, and the final temperature of wherein said external fluidized bed drying is no more than 60 ℃; The final temperature of vacuum freeze drying is no more than 60 ℃.
10. the spray freeze-drying preparation technology of polyunsaturated fatty acid grease microcapsules according to claim 1, it is characterized in that: in the polyunsaturated fatty acid grease microcapsules product that the spray freeze-drying preparation technology of described polyunsaturated fatty acid grease microcapsules obtains, powder embedding material shared percentage by weight in final products is 20～50%.
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| CN102860506A (en) * | 2012-08-08 | 2013-01-09 | 辽宁省大连海洋渔业集团公司 | Krill oil microcapsual powder and its preparation method |
| CN102987382A (en) * | 2012-08-08 | 2013-03-27 | 辽宁省大连海洋渔业集团公司 | Krill oil microcapsule powder and preparation method thereof |
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