CN103919140B - A kind of perilla herb oil microballoon and preparation method thereof - Google Patents
A kind of perilla herb oil microballoon and preparation method thereof Download PDFInfo
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- 235000004347 Perilla Nutrition 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 244000124853 Perilla frutescens Species 0.000 title 1
- 241000229722 Perilla <angiosperm> Species 0.000 claims abstract description 28
- 108010010803 Gelatin Proteins 0.000 claims abstract description 18
- 229920000159 gelatin Polymers 0.000 claims abstract description 18
- 239000008273 gelatin Substances 0.000 claims abstract description 18
- 235000019322 gelatine Nutrition 0.000 claims abstract description 18
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000839 emulsion Substances 0.000 claims abstract description 10
- -1 fatty acid ester Chemical class 0.000 claims abstract description 9
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 6
- 229930195729 fatty acid Natural products 0.000 claims abstract description 6
- 239000000194 fatty acid Substances 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000012456 homogeneous solution Substances 0.000 claims description 4
- ANOBYBYXJXCGBS-UHFFFAOYSA-L stannous fluoride Chemical compound F[Sn]F ANOBYBYXJXCGBS-UHFFFAOYSA-L 0.000 claims 2
- 239000002253 acid Substances 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 239000004005 microsphere Substances 0.000 abstract description 14
- 229920003012 Hydroxypropyl distarch phosphate Polymers 0.000 abstract description 8
- 239000001310 hydroxy propyl distarch phosphate Substances 0.000 abstract description 8
- 235000013825 hydroxy propyl distarch phosphate Nutrition 0.000 abstract description 8
- DVROLKBAWTYHHD-UHFFFAOYSA-N hydroxy propyl distarch phosphate Chemical compound OC1C(O)C(OC)OC(CO)C1OC(O)CCOC1C(OC2C(C(O)C(OC3C(C(OP(O)(=O)OC4C(C(O)C(OC)OC4CO)O)C(C)OC3CO)O)OC2COC2C(C(O)C(OC)C(CO)O2)O)O)OC(CO)C(OC)C1O DVROLKBAWTYHHD-UHFFFAOYSA-N 0.000 abstract description 8
- 150000002500 ions Chemical class 0.000 abstract description 6
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 229920000223 polyglycerol Polymers 0.000 abstract description 4
- 229910019142 PO4 Inorganic materials 0.000 abstract 1
- 239000010452 phosphate Substances 0.000 abstract 1
- 239000011162 core material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- JAZBEHYOTPTENJ-JLNKQSITSA-N all-cis-5,8,11,14,17-icosapentaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O JAZBEHYOTPTENJ-JLNKQSITSA-N 0.000 description 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 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000020673 eicosapentaenoic acid Nutrition 0.000 description 2
- 229960005135 eicosapentaenoic acid Drugs 0.000 description 2
- JAZBEHYOTPTENJ-UHFFFAOYSA-N eicosapentaenoic acid Natural products CCC=CCC=CCC=CCC=CCC=CCCCC(O)=O JAZBEHYOTPTENJ-UHFFFAOYSA-N 0.000 description 2
- 239000003094 microcapsule Substances 0.000 description 2
- DVSZKTAMJJTWFG-SKCDLICFSA-N (2e,4e,6e,8e,10e,12e)-docosa-2,4,6,8,10,12-hexaenoic acid Chemical compound CCCCCCCCC\C=C\C=C\C=C\C=C\C=C\C=C\C(O)=O DVSZKTAMJJTWFG-SKCDLICFSA-N 0.000 description 1
- GZJLLYHBALOKEX-UHFFFAOYSA-N 6-Ketone, O18-Me-Ussuriedine Natural products CC=CCC=CCC=CCC=CCC=CCC=CCCCC(O)=O GZJLLYHBALOKEX-UHFFFAOYSA-N 0.000 description 1
- 241000207923 Lamiaceae Species 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- 230000000954 anitussive effect Effects 0.000 description 1
- 230000003266 anti-allergic effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000002785 anti-thrombosis Effects 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 229940124584 antitussives Drugs 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 description 1
- 235000020669 docosahexaenoic acid Nutrition 0.000 description 1
- KAUVQQXNCKESLC-UHFFFAOYSA-N docosahexaenoic acid (DHA) Natural products COC(=O)C(C)NOCC1=CC=CC=C1 KAUVQQXNCKESLC-UHFFFAOYSA-N 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 230000004382 visual function Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings or cooking oils
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
-
- 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
- A23P20/00—Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
- A23P20/10—Coating with edible coatings, e.g. with oils or fats
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Mycology (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
Abstract
本发明提供了一种紫苏油微球及其制备方法,制备的紫苏油微球形状均匀,表面光滑。制备方法为分别用乙酸溶液(1 % v/v)配制pH 4-5的酸法明胶(A型)均匀溶液和pH4-5的羟丙基二淀粉磷酸酯溶液备用;在一定体积的紫苏油中搅拌下加入聚甘油脂肪酸酯搅动30分钟,逐滴加到配好的明胶溶液中,搅动并剪切均匀,得到均一的乳状液;向乳状液中加入配好的羟丙基二淀粉磷酸酯溶液,搅拌然后静置,25℃下10000rpm离心在室温负压下干燥得到紫苏油微球,包裹物为明胶。制备方法条件温和,不使用有机溶剂,且离子浓度低。The invention provides a perilla oil microsphere and a preparation method thereof. The prepared perilla oil microsphere has uniform shape and smooth surface. The preparation method is to use acetic acid solution (1% v/v) to prepare acid-processed gelatin (type A) uniform solution with pH 4-5 and hydroxypropyl distarch phosphate solution with pH 4-5 for standby; Add polyglycerol fatty acid ester to the oil and stir for 30 minutes, add dropwise to the prepared gelatin solution, stir and cut evenly to obtain a uniform emulsion; add prepared hydroxypropyl distarch to the emulsion The phosphate ester solution was stirred and then left to stand, centrifuged at 10,000 rpm at 25°C, and dried under negative pressure at room temperature to obtain perilla oil microspheres, which were wrapped in gelatin. The preparation method has mild conditions, does not use organic solvents, and has low ion concentration.
Description
技术领域 technical field
本发明涉及食品油脂技术领域,具体说是涉及一种油脂微球及其制备方法。 The invention relates to the technical field of food oil, in particular to an oil microsphere and a preparation method thereof.
背景技术 Background technique
紫苏油是唇形科植物紫苏的干燥成熟果实压榨得到的油脂。紫苏油中富含α-亚麻酸(占总脂肪酸的62 - 85%),在人体内代谢后主要以二十碳五烯酸(EPA)和二十二碳六烯酸(DHA)的形式存在。经研究发现,紫苏油具有抗血栓,抗过敏、抗炎作用,降血压、降血脂、降胆固醇作用,抗癌作用,对学习行为活动和视觉功能的促进作用,镇咳、平喘作用,以及抑菌作用。 Perilla oil is the oil obtained by pressing the dried ripe fruit of perilla plant of Labiatae. Perilla oil is rich in α-linolenic acid (accounting for 62 - 85% of total fatty acids), which is mainly in the form of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) after metabolism in the human body exist. It has been found through research that perilla oil has anti-thrombotic, anti-allergic, anti-inflammatory effects, lowering blood pressure, lowering blood lipids, lowering cholesterol, anti-cancer effects, promoting effects on learning behavior activities and visual functions, antitussive and asthma-relieving effects, and antibacterial effect.
另一方面,由于紫苏油中不饱和脂肪酸含量高,紫苏油存在容易被氧化,而且口感不好的不足之处。人们尝试了微胶囊包埋和充氮保护等方法,取得了一定的成果,但存在一些局限之处。随着微胶囊制备技术的发展,出现了制作粒径更小、操作条件温和的纳米微球技术。但是经查阅文献,目前国内尚未紫苏油微球的相关报道。本发明利用在pH4 -5条件下酸法明胶(A型)与羟丙基二淀粉磷酸酯带相反电荷,且均为分子聚合物的特点,通过离子凝聚作用、空间位阻作用及脱水作用,形成微球。该方法制备方法条件温和,不使用有机溶剂,且离子浓度低。 On the other hand, due to the high content of unsaturated fatty acids in perilla oil, perilla oil has the disadvantages of being easily oxidized and having a bad mouthfeel. People have tried methods such as microcapsule embedding and nitrogen filling protection, and have achieved certain results, but there are some limitations. With the development of microcapsule preparation technology, nano-microsphere technology with smaller particle size and mild operating conditions has emerged. However, after reviewing the literature, there is no relevant report on perilla oil microspheres in China. The present invention utilizes the characteristics of acid-processed gelatin (type A) and hydroxypropyl distarch phosphate having opposite charges under the condition of pH 4-5, and both are molecular polymers, through ion coagulation, steric hindrance and dehydration, Form microspheres. The preparation method of the method has mild conditions, does not use organic solvents, and has low ion concentration.
发明内容 Contents of the invention
本发明的目的提供一种紫苏油微球及其制备方法,该法制备的紫苏油微球提高了紫苏油的稳定性,增加紫苏油的生物利用率。采用该方法制备的紫苏油微球粒径细微,表面光滑,包埋良好。 The object of the present invention is to provide a perilla oil microsphere and a preparation method thereof, the perilla oil microsphere prepared by the method improves the stability of the perilla oil and increases the bioavailability of the perilla oil. The perilla oil microspheres prepared by this method have fine particle size, smooth surface and good embedding.
一种紫苏油微球及其制备方法,其特征在于,在室温下分别用乙酸溶液(1 % v/v)配制pH 4-5的酸法明胶(A型)均匀溶液(0.05 %– 0.50 % ),和pH4-5的羟丙基二淀粉磷酸酯溶液(0.2 %– 1.5 %)备用;在一定体积的紫苏油中搅拌下加入聚甘油脂肪酸酯(0.025 %– 0.225 %),50℃水浴中搅动30分钟,逐滴加到配好的明胶溶液中(紫苏油与明胶的比例为3:1 -1:5, v/w),搅动30分钟并在1000 – 2000 r/min 转速下剪切均匀,得到均一的乳状液;向乳状液中加入配好的羟丙基二淀粉磷酸酯溶液溶液,搅拌20分钟,然后静置3-8小时,25℃下10000 rpm离心10min,收集形成的粒子,得到的湿粒子分散于蒸馏水中。然后在室温负压下干燥,在25℃干燥条件下保存。该微球的芯材为紫苏油,包裹物为明胶。制备方法条件温和,不使用有机溶剂,且离子浓度低。 A kind of perilla oil microsphere and its preparation method, it is characterized in that, the homogeneous solution (0.05%-0.50% % ), and pH 4-5 hydroxypropyl distarch phosphate solution (0.2%–1.5%) for later use; add polyglycerol fatty acid ester (0.025%–0.225%) to a certain volume of perilla oil while stirring, 50 Stir in a water bath at ℃ for 30 minutes, add dropwise to the prepared gelatin solution (the ratio of perilla oil to gelatin is 3:1 -1:5, v/w), stir for 30 minutes and keep stirring at 1000 – 2000 r/min Cut evenly at a rotating speed to obtain a uniform emulsion; add the prepared hydroxypropyl distarch phosphate solution to the emulsion, stir for 20 minutes, then stand for 3-8 hours, and centrifuge at 10,000 rpm for 10 minutes at 25°C. The particles formed were collected and the resulting wet particles were dispersed in distilled water. Then dry at room temperature under negative pressure, and store under dry conditions at 25°C. The core material of the microsphere is perilla oil, and the wrapper is gelatin. The preparation method has mild conditions, does not use organic solvents, and has low ion concentration.
具体实施方式 实施例1: The specific implementation method Embodiment 1:
在室温下分别用乙酸溶液(1 % v/v)配制pH 4的酸法明胶(A型)均匀溶液(0.05 % ),和pH 4的羟丙基二淀粉磷酸酯溶液(0. 5 %)备用;在一定体积的紫苏油中搅拌下加入聚甘油脂肪酸酯(0.025 %),50℃水浴中搅动30分钟,逐滴加到配好的明胶溶液中(紫苏油与明胶的比例为1:1, v/w),搅动30分钟并在1500 r/min 转速下剪切均匀,得到均一的乳状液;向乳状液中加入配好的羟丙基二淀粉磷酸酯溶液,搅拌20分钟,然后静置4小时,25℃下10000 rpm离心10min,收集形成的粒子,得到的湿粒子分散于蒸馏水中。然后在室温负压下干燥,在25℃干燥条件下保存。该微球的芯材为紫苏油,包裹物为明胶。制备方法条件温和,不使用有机溶剂,且离子浓度低。 Prepare pH 4 acid-processed gelatin (Type A) homogeneous solution (0.05%) and pH 4 hydroxypropyl distarch phosphate solution (0.5%) with acetic acid solution (1% v/v) at room temperature Standby; add polyglycerol fatty acid ester (0.025%) to a certain volume of perilla oil while stirring, stir in a water bath at 50°C for 30 minutes, and add dropwise to the prepared gelatin solution (the ratio of perilla oil to gelatin is 1:1, v/w), stir for 30 minutes and shear evenly at 1500 r/min to obtain a uniform emulsion; add the prepared hydroxypropyl distarch phosphate solution to the emulsion, and stir for 20 minutes , and then left to stand for 4 hours, centrifuged at 10,000 rpm for 10 minutes at 25°C to collect the formed particles, and the obtained wet particles were dispersed in distilled water. Then dry at room temperature under negative pressure, and store under dry conditions at 25°C. The core material of the microsphere is perilla oil, and the wrapper is gelatin. The preparation method has mild conditions, does not use organic solvents, and has low ion concentration.
实施例2: Example 2:
在室温下分别用乙酸溶液(1 % v/v)配制pH 5的酸法明胶(A型)均匀溶液0.09 %),和pH 5的羟丙基二淀粉磷酸酯溶液(0.8 %)备用;在一定体积的紫苏油中搅拌下加入聚甘油脂肪酸酯(0.05 %),50℃水浴中搅动30分钟,逐滴加到配好的明胶溶液中(紫苏油与明胶的比例为1:3,v/w),搅动30分钟并在 2000 r/min 转速下剪切均匀,得到均一的乳状液;向乳状液中加入配好的羟丙基二淀粉磷酸酯溶液,搅拌20分钟,然后静置6小时,25℃下10000 rpm离心10min,收集形成的粒子,得到的湿粒子分散于蒸馏水中。然后在室温负压下干燥,在25℃干燥条件下保存。该微球的芯材为紫苏油,包裹物为明胶。制备方法条件温和,不使用有机溶剂,且离子浓度低。 At room temperature, use acetic acid solution (1% v/v) to prepare acid-process gelatin (type A) homogeneous solution of pH 5 (0.09%), and hydroxypropyl distarch phosphate solution (0.8%) of pH 5 for later use; Add polyglycerol fatty acid ester (0.05%) to a certain volume of perilla oil with stirring, stir in a water bath at 50°C for 30 minutes, and add dropwise to the prepared gelatin solution (the ratio of perilla oil to gelatin is 1:3 , v/w), stirred for 30 minutes and sheared evenly at 2000 r/min to obtain a uniform emulsion; added the prepared hydroxypropyl distarch phosphate solution to the emulsion, stirred for 20 minutes, and then statically Place for 6 hours, centrifuge at 10,000 rpm for 10 minutes at 25°C, collect the formed particles, and disperse the obtained wet particles in distilled water. Then dry at room temperature under negative pressure, and store under dry conditions at 25°C. The core material of the microsphere is perilla oil, and the wrapper is gelatin. The preparation method has mild conditions, does not use organic solvents, and has low ion concentration.
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