WO2017202104A1 - 一种层层自组装固化亚麻籽油及其复配油脂的方法 - Google Patents
一种层层自组装固化亚麻籽油及其复配油脂的方法 Download PDFInfo
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- WO2017202104A1 WO2017202104A1 PCT/CN2017/075835 CN2017075835W WO2017202104A1 WO 2017202104 A1 WO2017202104 A1 WO 2017202104A1 CN 2017075835 W CN2017075835 W CN 2017075835W WO 2017202104 A1 WO2017202104 A1 WO 2017202104A1
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- oil
- sodium alginate
- linseed oil
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
- A23D7/005—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by ingredients other than fatty acid triglycerides
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
- A23D7/02—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by the production or working-up
- A23D7/04—Working-up
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/10—Complex coacervation, i.e. interaction of oppositely charged particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/20—After-treatment of capsule walls, e.g. hardening
- B01J13/206—Hardening; drying
Definitions
- the invention relates to a layer self-assembling curing linseed oil and a method for compounding the same, belonging to the field of oil processing.
- the content of unsaturated fatty acids in linseed oil is over 90%, among which ⁇ -linolenic acid is the highest (more than 54%), and ⁇ -linolenic acid is n-3 essential fatty acid, which can be converted into EPA and in vivo.
- DHA has the functions of promoting fetal and infant brain growth and development, enhancing memory, improving immunity, improving and maintaining vision, preventing cerebral thrombosis and myocardial infarction.
- Studies have shown that the intake of saturated fatty acids is positively correlated with the occurrence of cardiovascular disease. If the intake of essential fatty acids in the n-3 system is insufficient, the animal's learning ability and visual acuity will decrease. At present, there is a lack of n-3 fatty acids in Chinese diet, but saturated fatty acids and n-6 unsaturated fatty acids are ingested more.
- Flaxseed oil is an excellent raw material for n-3 unsaturated fatty acids. Because of its high content of unsaturated fatty acids, linseed oil is easily oxidized, resulting in undesirable flavor and even harmful substances, which affect the shelf life of linseed oil.
- the microcapsule embedding technology can well retard and avoid the oxidation of linseed oil during processing, transportation and consumption.
- the microencapsulation of linseed oil not only facilitates the use, transportation and preservation, but also promotes the development of many convenient foods, such as nutritional fortified milk powder; prevents the oxidation of some unstable food raw materials; reduces or masks bad taste.
- the commonly used embedding methods include spray drying, emulsion diffusion, interfacial polymerization, complex coagulation, etc., wherein spray drying is applied more because of its simple process.
- Spray drying mostly uses corn starch, modified starch, whey powder, vegetable protein, gelatin, gum arabic, etc. as wall material or emulsifying material to embed linseed oil. Under the action of hot air, the water evaporates and the wall material is wrapped. The core material is buried to form a microcapsule product.
- spray drying has problems such as high temperature, multi-adjuvant compounding, sticking, and low embedding rate.
- Spray drying nozzle temperature is 150 ⁇ 190 ° C, high temperature has an impact on product quality.
- the object of the present invention is to provide a layer-by-layer self-assembling and curing linseed oil and a method for compounding the same.
- the invention first prepares microcapsules of oil and fat, and then solidifies with calcium lactate, and finally layers the cured oil gel beads.
- the layer self-assembly that is, the layer embedding of the oil and fat is realized;
- the gel beads prepared by the method of the invention have high oil loading rate and can reach 1700-7000%;
- the embedding rate of the gel beads prepared by the method of the invention is high, Can reach 92 to 99%.
- the method for self-assembling and solidifying oil and fat provided by the invention comprises the following steps:
- step (3) of the self-assembled and cured oil-alkali sodium alginate gel beads repeating the step (3) of the self-assembled and cured oil-alkali sodium alginate gel beads to achieve self-assembly and solidification of the oil and fat layer.
- the oil may be linseed oil, peony seed oil, grape seed oil, camellia oil, peanut oil, germ oil, walnut oil, flax oil, sesame oil, olive oil, deep sea fish oil, garlic oil and ginger oleoresin.
- the mass ratio of the three can be 40 ⁇ 50 parts: 10-20 parts: 10-20 parts, specifically 45 parts: 15 parts: 15 parts.
- the aqueous sodium alginate solution may have a concentration of 1.1 to 1.4%, specifically 1.1% or 1.4%;
- the mass concentration of the chitosan aqueous solution may be 1 to 3%, specifically 1%, 2% or 3%;
- the calcium lactate aqueous solution may have a mass concentration of 1 to 3%, specifically 1%, 2% or 3%.
- the volume ratio of the oil and fat to the aqueous sodium alginate solution may be 1:0.5 to 20, specifically 1:2.5;
- the shearing time can be from 1 to 4 minutes, such as 2 minutes.
- the particle size of the sodium alginate microcapsule can be adjusted by a high speed shear or homogenizer control.
- step (2) the oil and fat sodium alginate microcapsules are added to the calcium lactate aqueous solution by using a syringe;
- the particle size of the cured oil alginate gel beads can be adjusted by adjusting the size of the syringe needle
- the stirring time may be 5 to 10 min, specifically 5 min.
- the stirring time may be 5 to 10 min, specifically 5 min;
- the layered assembly of the microcapsules is achieved by electrostatic adsorption of the chitosan and the sodium alginate, and the calcium lactate is used for curing after assembling each layer of the wall.
- the step (3) is repeated at least 1 to 2 times.
- the layer-by-assembly self-assembled and cured oil-alkali sodium gel beads prepared by the present invention may be dried or packaged by low-temperature blast drying for 8 to 10 hours; or after irradiation sterilization, liquid packaging may be carried out.
- the gel beads prepared by the method of the invention have an oil loading rate of up to 1700-7000%, such as 2900-3100%, and the oil loading rate refers to the core material and the wall of the self-assembling fixed grease gel beads.
- the gel beads prepared by the method of the invention have an embedding rate of 92-99%, and the embedding rate refers to the mass percentage of the gel beads embedding grease and the added total fat.
- FIG. 1 is an electron micrograph of a sodium alginate-linseed oil microcapsule prepared in Example 1 of the present invention, wherein FIG. 1(a) to FIG. 1(f) are respectively prepared in the present Example 1)-6) Electron micrograph of linseed oil-sodium alginate microcapsules.
- FIG. 2 is an electron micrograph of a linseed oil alginate gel bead prepared in Example 2 of the present invention, wherein FIG. 2(a) and FIG. 2(b) are electron micrographs after drying and before drying, respectively.
- the linseed oil-sodium alginate microcapsules were prepared according to the following six conditions:
- ALG represents sodium alginate
- Flaxseed Oil represents linseed oil
- the PDI in Table 1 represents the polydispersity index, reflecting the stability of the system.
- the value of PDI should be less than 1, and the smaller the better. It can be seen from the values of PDI in Table 1 that the standard deviation and PDI value of high concentration of sodium alginate are high, indicating that high concentration of sodium alginate makes the system unstable.
- ZP in Table 1 indicates the potential, and since sodium alginate exhibits a negative charge, the larger the absolute value of the potential, the more stable the system.
- Fig. 1 The SEM photograph of the linseed oil-alginate microcapsule prepared in this embodiment is shown in Fig. 1, wherein Fig. 1(a) - Fig. 1(f) are respectively prepared in the present example 1)-6) Electron micrograph of linseed oil-sodium alginate microcapsules.
- the shiny white ball is an unembedded oil droplet, and it can be seen that the linseed oil is almost completely embedded by sodium alginate.
- the particle size and variation trend of the linseed oil-alginate microcapsules are consistent with those in Table 1.
- the linseed oil-sodium alginate microcapsules exhibit an irregular strip or sphere and are shaped in relation to the high speed shear of a high speed homogenizer.
- the concentration of sodium alginate is optimally 1.1 to 1.4%.
- Example 2 layer self-assembly curing of linseed oil
- Example 1 The linseed oil-alginate microcapsules prepared in 3) of Example 1 were subjected to layer-by-layer self-assembly curing.
- the linseed oil-sodium alginate microcapsules were sucked into a 2 wt% aqueous calcium lactate solution by a syringe, and magnetically stirred for 5 minutes to obtain a solidified linseed oil alginate gel beads.
- step b) repeating step a) twice with a layer of self-assembled and cured linseed oil alginate gel beads to achieve layer-by-layer self-assembly and solidification of linseed oil to obtain linseed oil alginate gel beads.
- FIG. 2 An electron micrograph of the linseed oil alginate gel beads prepared in this embodiment is shown in Fig. 2, wherein Fig. 2(a) and Fig. 2(b) are electron micrographs after drying and before drying, respectively. It can be seen that there is no oil slick or grease oozing out on the surface before and after drying.
- the dried gel beads have a particle size of 0.8 to 1.5 mm, and the undried gel beads have a size of 1.5 to 2.5 mm.
- the linseed oil alginate gel beads prepared in this example had an oil loading rate of 3010% and an embedding rate of 92%.
- Example 3 layer self-assembly curing of linseed oil
- Example 1 The linseed oil-alginate microcapsules prepared in 3) of Example 1 were subjected to layer-by-layer self-assembly curing.
- the linseed oil-sodium alginate microcapsules were aspirated with a syringe and added to a 1 wt% aqueous solution of calcium lactate, and magnetically stirred for 5 minutes to obtain a solidified linseed oil alginate gel beads.
- step b) repeating step a) once a layer of self-assembled and solidified linseed oil alginate gel beads to achieve layer-by-layer self-assembly and solidification of linseed oil to obtain linseed oil alginate gel beads.
- the linseed oil alginate gel beads prepared in this example had an oil loading rate of 3100% and an embedding rate of 97%.
- Example 4 layer self-assembly curing of linseed oil
- Example 1 The linseed oil-alginate microcapsules prepared in 3) of Example 1 were subjected to layer-by-layer self-assembly.
- the linseed oil-sodium alginate microcapsules were sucked into a 3 wt% aqueous calcium lactate solution by a syringe, and magnetically stirred for 5 minutes to obtain a solidified linseed oil alginate gel beads.
- step b) repeating step a) twice with a layer of self-assembled and cured linseed oil alginate gel beads to achieve layer-by-layer self-assembly and solidification of linseed oil to obtain linseed oil alginate gel beads.
- the linseed oil alginate gel beads prepared in this example had an oil loading rate of 3000% and an embedding rate of 95%.
- Example 1 The linseed oil-alginate microcapsules prepared in 4) of Example 1 were subjected to layer-by-layer self-assembly.
- the linseed oil-sodium alginate microcapsules were sucked into a 2 wt% aqueous calcium lactate solution by a syringe, and magnetically stirred for 5 minutes to obtain a solidified linseed oil alginate gel beads.
- the cured linseed oil pellet prepared in the step (1) is placed in a 2 wt% aqueous solution of chitosan Medium magnetic stirring for 5 min. After taking out, it was placed in a 1.4 wt% sodium alginate solution and magnetically stirred for 10 min. Finally, the pellet was placed in a 2 wt% calcium lactate aqueous solution and magnetically stirred for 5 min to obtain a self-assembled and solidified linseed oil alginate gel bead.
- step b) repeating step a) once a layer of self-assembled and solidified linseed oil alginate gel beads to achieve layer-by-layer self-assembly and solidification of linseed oil to obtain linseed oil alginate gel beads.
- the oil loading rate of the linseed oil alginate gel beads prepared in this example was 2910%.
- Example 6 layer self-assembly curing of linseed oil
- Example 1 The linseed oil-alginate microcapsules prepared in 4) of Example 1 were subjected to layer-by-layer self-assembly.
- the linseed oil-sodium alginate microcapsules were aspirated with a syringe and added to a 1 wt% aqueous solution of calcium lactate, and magnetically stirred for 5 minutes to obtain a solidified linseed oil alginate gel beads.
- the solidified linseed oil pellet prepared in the step (1) was placed in a 1 wt% aqueous solution of chitosan and magnetically stirred for 5 min. After taking out, it was placed in a 1.4 wt% sodium alginate solution and magnetically stirred for 10 min. Finally, the pellet was placed in a 1 wt% calcium lactate aqueous solution and magnetically stirred for 5 min to obtain a self-assembled and solidified linseed oil alginate gel bead.
- step b) repeating step a) twice with a layer of self-assembled and cured linseed oil alginate gel beads to achieve layer-by-layer self-assembly and solidification of linseed oil to obtain linseed oil alginate gel beads.
- the oil loading rate of the linseed oil alginate gel beads prepared in this example was 2890%, and the embedding rate was 94%.
- Example 1 The linseed oil-alginate microcapsules prepared in 4) of Example 1 were subjected to layer-by-layer self-assembly.
- the linseed oil-sodium alginate microcapsules were sucked into a 3 wt% aqueous calcium lactate solution by a syringe, and magnetically stirred for 5 minutes to obtain a solidified linseed oil alginate gel beads.
- the solidified linseed oil pellet prepared in the step (1) was placed in a 3 wt% aqueous solution of chitosan and magnetically stirred for 5 min. After taking out, it was placed in a 1.4 wt% sodium alginate solution and magnetically stirred for 10 min. Finally, the pellet was placed in a 3 wt% calcium lactate aqueous solution and magnetically stirred for 5 min to obtain a self-assembled and solidified linseed oil alginate gel bead.
- step b) repeating step a) twice with a layer of self-assembled and cured linseed oil alginate gel beads to achieve layer-by-layer self-assembly and solidification of linseed oil to obtain linseed oil alginate gel beads.
- the linseed oil alginate gel beads prepared in this example had an oil loading rate of 2900% and an embedding rate of 95%.
- Example 8 layer self-assembly curing of linseed oil compound grease
- composition of the linseed oil compound fat is: linseed oil, peony seed oil and grape seed oil, the mass ratio of the three is 45 parts: 15 parts: 15 parts.
- the linseed oil compounded fat sodium alginate microcapsules were added by syringe to the 3 wt% calcium lactate aqueous solution, and magnetically stirred for 5 min to obtain a cured linseed oil compounded fat sodium alginate gel beads.
- step b) repeating step a) twice with a layer of self-assembled and cured linseed oil compounded with sodium alginate gel beads to achieve layer-by-layer self-assembly and solidification of linseed oil, and obtaining linseed oil compounding fat alginic acid Sodium gel beads.
- the oil loading rate of the linseed oil compounded fat sodium alginate gel beads prepared in this example was 3100%, and the embedding rate was 99%.
- the embedding material used in the method of the invention comprises sodium alginate, chitosan and calcium lactate, and does not contain emulsifiers such as Tween and Span which are commonly used in the prior art, and they are all additives for safety comparison, and the utilization degree is utilized. high.
- the oil-bearing rate of the gel beads prepared by the invention is high, and the oil loading rate of the microcapsules of the invention is as high as 1700-7000% according to the mass ratio of the core materials to the wall materials.
- the embedding rate of the gel beads prepared by the invention is high, and the embedding rate of the microcapsules of the invention is as high as 92 to 99% according to the mass ratio of the entrapped oil to the total fat added.
- the method of the present invention can be carried out at room temperature, and the temperature is lower than that of the spray drying method, thereby saving costs.
- the method of the invention can not only embed linseed oil, but also embed other oils or compound embedding.
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Abstract
Description
Claims (10)
- 一种层层自组装固化亚麻籽油及其复配油脂的方法,包括如下步骤:(1)将油脂分散于海藻酸钠水溶液中,经剪切或均质得到油脂海藻酸钠微胶囊;(2)将所述油脂海藻酸钠微胶囊加入至乳酸钙水溶液中,经搅拌,得到固化的油脂海藻酸钠凝胶珠;(3)将所述固化的油脂海藻酸钠凝胶珠依次加入至壳聚糖水溶液、所述海藻酸钠水溶液和所述乳酸钙水溶液中,并经依次搅拌,得到一层自组装固化的油脂海藻酸钠凝胶珠;(4)将所述一层自组装固化的油脂海藻酸钠凝胶珠重复步骤(3),即实现对油脂的层层自组装固化。
- 根据权利要求1所述的方法,其特征在于:所述油脂为亚麻籽油、牡丹籽油、葡萄籽油、山茶油、花生油、胚芽油、核桃油、胡麻油、芝麻油、橄榄油、深海鱼油、大蒜精油和姜油树脂中至少一种。
- 根据权利要求1或2所述的方法,其特征在于:所述海藻酸钠水溶液的质量浓度为1.1~1.4%;所述壳聚糖水溶液的质量浓度为1~3%;所述乳酸钙水溶液的质量浓度为1~3%。
- 根据权利要求1-3中任一项所述的方法,其特征在于:步骤(1)中,所述油脂与所述海藻酸钠水溶液的体积比为1:0.5~20;所述剪切的时间为1~4min。
- 根据权利要求1-4中任一项所述的方法,其特征在于:步骤(2)中,采用注射器将所述油脂海藻酸钠微胶囊加入至所述乳酸钙水溶液中;所述搅拌的时间为5~10min。
- 根据权利要求1-5中任一项所述的方法,其特征在于:步骤(3)中,所述搅拌的时间为5~10min。
- 根据权利要求1-6中任一项所述的方法,其特征在于:步骤(4)中,重复步骤(3)至少1~2次。
- 权利要求1-7中任一项所述方法制备的凝胶珠。
- 根据权利要求8所述的凝胶珠,其特征在于:所述凝胶珠的载油率为1700~7000%,所述载油率指的是所述凝胶珠的芯材与壁材的质量百分比。
- 根据权利要求8所述的凝胶珠,其特征在于:所述凝胶珠的包埋率为92~99%,所述包埋率指的是被所述凝胶珠包埋的油脂与加入的总油脂的质量百分比。
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