CN114672318A - 一种茶多酚纳米粒子稳定的皮克林乳液及其制备方法 - Google Patents
一种茶多酚纳米粒子稳定的皮克林乳液及其制备方法 Download PDFInfo
- Publication number
- CN114672318A CN114672318A CN202011548459.7A CN202011548459A CN114672318A CN 114672318 A CN114672318 A CN 114672318A CN 202011548459 A CN202011548459 A CN 202011548459A CN 114672318 A CN114672318 A CN 114672318A
- Authority
- CN
- China
- Prior art keywords
- emulsion
- pickering emulsion
- preparation
- nanoparticles
- oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000839 emulsion Substances 0.000 title claims abstract description 145
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 36
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 35
- 241001122767 Theaceae Species 0.000 title abstract description 20
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 39
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000003921 oil Substances 0.000 claims abstract description 26
- 235000019198 oils Nutrition 0.000 claims abstract description 22
- 238000010008 shearing Methods 0.000 claims abstract description 15
- 239000003381 stabilizer Substances 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 235000015112 vegetable and seed oil Nutrition 0.000 claims abstract description 5
- 239000008158 vegetable oil Substances 0.000 claims abstract description 5
- 239000012071 phase Substances 0.000 claims description 41
- 238000000034 method Methods 0.000 claims description 20
- WMBWREPUVVBILR-WIYYLYMNSA-N (-)-Epigallocatechin-3-o-gallate Chemical compound O([C@@H]1CC2=C(O)C=C(C=C2O[C@@H]1C=1C=C(O)C(O)=C(O)C=1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-WIYYLYMNSA-N 0.000 claims description 16
- WMBWREPUVVBILR-UHFFFAOYSA-N GCG Natural products C=1C(O)=C(O)C(O)=CC=1C1OC2=CC(O)=CC(O)=C2CC1OC(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-UHFFFAOYSA-N 0.000 claims description 16
- 229940030275 epigallocatechin gallate Drugs 0.000 claims description 16
- 230000001804 emulsifying effect Effects 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 8
- 239000008346 aqueous phase Substances 0.000 claims description 7
- 235000021388 linseed oil Nutrition 0.000 claims description 7
- 239000000944 linseed oil Substances 0.000 claims description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000004945 emulsification Methods 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004006 olive oil Substances 0.000 claims description 2
- 235000008390 olive oil Nutrition 0.000 claims description 2
- 244000269722 Thea sinensis Species 0.000 claims 5
- 239000000126 substance Substances 0.000 abstract description 5
- 239000002537 cosmetic Substances 0.000 abstract description 3
- 229940079593 drug Drugs 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 3
- 235000013305 food Nutrition 0.000 abstract description 3
- 230000000975 bioactive effect Effects 0.000 abstract description 2
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 235000006708 antioxidants Nutrition 0.000 description 32
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 25
- 239000004471 Glycine Substances 0.000 description 12
- 238000007254 oxidation reaction Methods 0.000 description 11
- 230000003647 oxidation Effects 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 229920001223 polyethylene glycol Polymers 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 5
- 235000018417 cysteine Nutrition 0.000 description 5
- 238000003860 storage Methods 0.000 description 4
- 231100000331 toxic Toxicity 0.000 description 4
- 230000002588 toxic effect Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 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 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 230000007760 free radical scavenging Effects 0.000 description 1
- 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 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000399 optical microscopy Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- -1 polyphenol compounds Chemical class 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K15/00—Anti-oxidant compositions; Compositions inhibiting chemical change
- C09K15/04—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds
- C09K15/12—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds containing sulfur and oxygen
- C09K15/14—Anti-oxidant compositions; Compositions inhibiting chemical change containing organic compounds containing sulfur and oxygen containing a phenol or quinone moiety
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/03—Organic compounds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/22—Heterocyclic compounds, e.g. ascorbic acid, tocopherol or pyrrolidones
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/46—Ingredients of undetermined constitution or reaction products thereof, e.g. skin, bone, milk, cotton fibre, eggshell, oxgall or plant extracts
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4973—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
- A61K8/498—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/10—Dispersions; Emulsions
- A61K9/107—Emulsions ; Emulsion preconcentrates; Micelles
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/52—Stabilizers
- A61K2800/522—Antioxidants; Radical scavengers
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Epidemiology (AREA)
- Engineering & Computer Science (AREA)
- Botany (AREA)
- Pharmacology & Pharmacy (AREA)
- Medicinal Chemistry (AREA)
- Birds (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Microbiology (AREA)
- Nutrition Science (AREA)
- Dispersion Chemistry (AREA)
- Dermatology (AREA)
- Biotechnology (AREA)
- Mycology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Colloid Chemistry (AREA)
Abstract
本发明属于乳液制备技术领域，公开了一种茶多酚纳米粒子稳定的Pickering乳液及其制备方法。具体包括以具有抗氧化功能的茶多酚纳米粒子作为Pickering乳液的稳定剂，将其水溶液作为乳液的水相，植物油或有机溶剂作为乳液的油相，二者混合后经高速剪切得到水包油型的Pickering乳液。本发明采用的稳定剂自身具备显著的抗氧化功能，能够有效的提高油水界面上抗氧化剂的浓度，提高乳液的抗氧化效率。本发明的制备工艺简单高效、易于实现工业化，所制备的乳液稳定性高、抗氧化效率高、作用时间长，在食品、药品、化妆品中生物活性物质的封装与传递领域具有广泛的应用前景。
Description
技术领域
本发明属于Pickering乳液制备及其应用技术领域，特别涉及一种茶多酚纳米粒子稳定的具有显著抗氧化性的Pickering乳液及其制备方法。
背景技术
Pickering乳液是一种用固体颗粒代替表面活性剂来稳定油水界面的乳液，具有稳定性好、毒性低、环保等特点。Pickering乳液常被用做亲脂或化学不稳定的功能性物质封装和传递。但是这些生物活性物质对光、热、pH等十分敏感，即使被封装在Pickering乳液中，仍然容易被氧化，并且氧化产物对乳液的稳定性和质量等影响很大。已有不少研究发现，Pickering乳液中的氧化反应主要发生在油水界面上，因此，赋予Pickering乳液抗氧化功能来解决体系中的脂氧化问题十分重要，尤其是提高油水界面处的抗氧化剂浓度。传统的抗氧化策略是将抗氧化剂封装在乳液的油相或者水相中来赋予Pickering乳液抗氧化功能，这使得抗氧化剂在油水界面上的浓度低，抗氧化效果并不理想。近年来，有不少论文公开了用化学手段将抗氧化剂封装在Pickering稳定剂中或者制备具有抗氧化功能的Pickering稳定剂来赋予Pickering乳液抗氧化功能，但是这些工艺步骤往往存在工艺复杂耗时、反应条件苛刻、抗氧化功能成分含量低、抗氧化效率低，毒副作用大等问题。因此，亟需开发一种简便快捷的工艺来赋予Pickering乳液更高的抗氧化功能成分含量及抗氧化效率，有效的解决Pickering乳液中的氧化问题。
茶多酚是茶叶中多酚化合物的总称，具有抗氧化、抗炎、抗癌、预防心血管疾病、减脂等多种健康有益效应。茶多酚结构中丰富的羟基能够有效的清除自由基，是天然的抗氧化剂。
本发明利用CN201910526442.2专利申请中已公开的制备方法获得的茶多酚纳米粒子作为Pickering乳液的稳定剂，提供了一种简便的制备工艺来赋予Pickering乳液抗氧化功能，有效地提高了抗氧化剂在油水界面的浓度及抗氧化效率。本发明的工艺步骤简便快捷，条件温和，效率高，并且未添加任何表面活性剂或合成抗氧化剂，所获得的乳液绿色安全，毒副作用小，稳定性高，抗氧化功能显著，在食品、药品、化妆品领域有着广泛的应用前景。
发明内容
为了克服上述现有技术的缺点和不足，本发明的首要目的在于提供一种茶多酚纳米粒子稳定的Pickering乳液的制备方法。本发明将具有抗氧化功能的茶多酚纳米粒子作为Pickering乳液的稳定剂，有效地提高了油水界面抗氧化剂的浓度及效率，从而赋予了Pickering乳液良好的稳定性和显著的抗氧化功能。
本发明的另一目的在于提供上述方法制备的具有显著抗氧化性的Pickering乳液。
本发明的目的通过下述技术方案实现：
一种茶多酚纳米粒子稳定的Pickering乳液的制备方法，包括以下具体步骤:
(1)水相的制备：将具有抗氧化功能的多酚纳米粒子作为Pickering乳液的稳定剂，将其用去离子水配制成溶液作为Pickering乳液的水相；
(2)Pickering乳液的制备：将油相与步骤(1)中配制的水相混合，剪切乳化，获得Pickering乳液；
(3)凝胶状Pickering乳液的制备：向步骤(2)获得的乳液中加入PEG水溶液，再剪切乳化，获得凝胶状的Pickering乳液；
(4)高内相Pickering乳液的制备：向步骤(2)获得的乳液中继续添加油相，剪切乳化，得到高内相的Pickering乳液。
步骤(1)中所述的多酚纳米粒子包括表没食子儿茶素没食子酸酯(EGCG)纳米粒子、茶多酚纳米粒子中的至少一种。
步骤(1)中所述的多酚纳米粒子溶液的质量浓度为0.5%-4%。
步骤(2)中所述的油相为植物油或有机溶剂；植物油为亚麻籽油、橄榄油中的至少一种；有机溶剂为正己烷、乙酸乙酯、二氯甲烷中的至少一种。
步骤(2)中所述的水相与油相的体积比为2:3-1:3。
步骤(2)中所述的剪切乳化的转速为8000-12000 rpm，时间为30 s-180 s。
步骤(3)中所述的PEG水溶液包括分子量为800、4000、10000、20000的PEG中的至少一种；质量浓度为1%-5%；乳液与PEG水溶液的体积比为9:1-3:1。
所述的多酚纳米粒子稳定的Pickering 乳液通过上述方法制备得到。
本发明相对于现有技术，具有如下的优点和有益效果:
（1）利用天然植物基抗氧化剂作为Pickering乳液稳定剂的基材，原料绿色环保、天然可再生，容易获得；
（2）将具有高抗氧化功能成分含量的茶多酚纳米粒子作为乳液的稳定剂，能够有效地提高油水界面抗氧化剂的浓度及抗氧化效率，显著的提高乳液的氧化稳定性；
（3）整个乳液的工艺步骤具有操作简单快捷，可重复性好，成本低，易于工业化生产的优点，在未引入任何额外/合成抗氧化剂的情况下实现了乳液的抗氧化功能，并且抗氧化效率和有效作用时间得到了显著延长；
（4）由于在体系中引入了聚乙二醇，乳液的稳定得到了明显的增强，并且抗氧化剂的用量也得到了降低，在有效节约成本的同时，减少了对人体可能存在的毒副作用；
（5）由于对含油量进行调节，可以获得膏状的高内相乳液；
（6）茶多酚纳米粒子稳定的Pickering乳液具有显著的抗氧化性和长期稳定性，有利于亲脂或化学不稳定的功能性物质的封装和传递，可通过口服、经皮等形式广泛的应用于食品、药品、化妆品等领域。
附图说明
图1展示了贮存时间对实例1制备得到的乳液的稳定性的影响。
图2展示了对比例1制备得到的乳液液滴的光学显微镜图片。
图3展示了贮存时间对对比例1制备得到的乳液的稳定性的影响。
图4展示了对比例1制备得到的乳液再室温下储存一个月以后的抗氧化/清除自由基的效率。
图5展示了贮存时间对实例2制备得到的乳液的稳定性的影响。
图6展示了实例3制备得到的凝胶状乳液的倒置外观图。
图7展示了实例4制备得到的高内相Pickering乳液的倒置外观图。
图8展示了实例1-4及对比例1制备得到的Pickeirng乳液在水和油中的分散情况。
具体实施方式
下面将详细地用以下实例对本发明进行进一步说明，使本发明能够更加完整、透彻的被本领域的技术人员所理解，但本发明并不是被这些实例所限制。
实例1：
一种半胱氨酸茶多酚纳米粒子稳定的Pickering乳液的制备，具体包括以下步骤：
(1)水相的制备：将半胱氨酸EGCG纳米粒子作为Pickering乳液的稳定剂，将其用去离子水配制成质量浓度为0.5%-4%的溶液作为Pickering乳液的水相；
(2)Pickering乳液的制备：将亚麻籽油与步骤(1)中配制的水相混合(水油比：1:1)，剪切乳化(10000 rpm，60 s)，获得Pickering乳液；
本实例对步骤(1)中的半胱氨酸EGCG纳米粒子的质量浓度进行了梯度试验，质量浓度分别为0.5%、1%、2%、3%、4%，得到了不同半胱氨酸EGCG纳米粒子稳定的Pickering乳液(分别记为0.5-0.5ETP-1、1-0.5ETP-1、2-0.5ETP-1、3-0.5ETP-1、4-0.5ETP-1)。乳液的乳化层高度受纳米粒子浓度的影响，较高浓度的纳米粒子稳定的乳液具有较厚的乳化层。并监测乳液在制备1天、7天、14天后的外观，乳液没有发生进一步分层(如图1所示)。
对比例1：
一种甘氨酸茶多酚纳米粒子稳定的Pickering乳液的制备
同实例1，区别在于所选用的氨基酸为甘氨酸；
本对比例对步骤(1)中的甘氨酸EGCG纳米粒子的质量浓度进行了梯度试验，质量浓度分别为0.5%、1%、2%、3%、4%，得到了不同甘氨酸EGCG纳米粒子稳定的Pickering乳液(分别记为0.5-0.5ETP-2、1-0.5ETP-2、2-0.5ETP-2、3-0.5ETP-2、4-0.5ETP-2)。乳液的乳化层高度同样受纳米粒子浓度的影响，较高浓度的纳米粒子稳定的乳液具有较厚的乳化层。在乳液新制时用光学显微镜观察了乳液的液滴形貌，液滴呈球形，但液滴尺寸也受甘氨酸EGCG纳米粒子浓度的影响，浓度越高，液滴尺寸越小(如图2所示)。监测乳液在制备1天、7天、14天后的外观，乳液没有发生进一步分层，稳定性良好(如图3所示)。对比例1中的甘氨酸EGCG纳米粒子的乳化性能较实例1中的半胱氨酸EGCG纳米粒子的乳化性能更好，其稳定的Pickering乳液比实例1中的Pickering乳液的稳定性更好，可见纳米粒子的性质对乳液的稳定性也有影响。并且在室温下储存1个月后，对比例1的乳液仍具有较强的抗氧化性，抗氧化当量为水溶性维生素E的18.5倍(如图4所示)。
实例2：
一种甘氨酸茶多酚纳米粒子稳定的Pickering乳液的制备，具体包括以下步骤：
(1)水相的制备：将甘氨酸EGCG纳米粒子作为Pickering乳液的稳定剂，将其用去离子水配制成质量浓度为4%的溶液作为Pickering乳液的水相；
(2)Pickering乳液的制备：将亚麻籽油与步骤(1)中配制的水相混合(水油比：2:3-3:7)，剪切乳化(10000 rpm，60 s)，获得Pickering乳液；
本实例对步骤(2)中的油相体积分数进行了梯度试验，亚麻籽油对总体系的体积分数分别为：40%、50%、60%、70%，得到含有不同油相体积分数的Pickering乳液(分别记为4-0.4ETP-2、4-0.5ETP-2、4-0.6ETP-2、4-0.7ETP-2)。乳液的乳化层高度受油相体积分数的影响，油相体积分数越大，乳化层高度越高，含油量达到70%后，乳液在制备完成的初期就成了凝胶状，未发生分层现象。监测乳液在制备1天、7天、14天后的外观，乳液没有发生进一步分层(如图5所示)。
实例3 ：
一种凝胶状的甘氨酸茶多酚纳米粒子稳定的Pickering乳液的制备，具体包括以下步骤：
(1)水相的制备：将甘氨酸EGCG纳米粒子作为Pickering乳液的稳定剂，将其用去离子水配制成质量浓度为0.5%的溶液作为Pickering乳液的水相；
(2)Pickering乳液的制备：将亚麻籽油与步骤(1)中配制的水相混合(水油比：2:3-3:7)，剪切乳化(10000 rpm，60 s)，获得Pickering乳液；
(3)凝胶状Pickering乳液的制备：向步骤(2)获得的乳液中加入质量浓度为2%的PEG水溶液(乳液与PEG水溶液的体积比为9:1)，再剪切乳化(10000 rpm，30 s)，获得凝胶状的Pickering乳液；
本实例通过向所获得的低浓度、具有流动性的Pickering乳液中简单的添加PEG水溶液，获得了在低纳米粒子浓度下的凝胶状乳液，并且乳液不随瓶子的倒置而发生流动，倒置后仍然停留在瓶子的底部(如图6所示)。较实例2获得的乳液，粘度有了大幅度的提升，同时减少了纳米粒子的用量，降低成本的同时较小了可能的毒副作用。
实例4：
一种甘氨酸茶多酚纳米粒子稳定的高内相Pickering乳液的制备，具体包括以下步骤：
(1)水相的制备：将甘氨酸EGCG纳米粒子作为Pickering乳液的稳定剂，将其用去离子水配制成质量浓度为4%的溶液作为Pickering乳液的水相；
(2)Pickering乳液的制备：将亚麻籽油与步骤(1)中配制的水相混合(水油比： 3:7)，剪切乳化(10000 rpm，60 s)，获得Pickering乳液；
(3)高内相Pickering乳液的制备：向步骤(2)获得的乳液中继续添加油相直至油相体积分数为75%，剪切乳化(10000 rpm，30 s)，得到高内相的Pickering乳液；
本实例在实例2 的基础上进一步提升了油相体积分数，得到了高内相Pickering乳液，并在新制备时进行了倒置实验，甘氨酸EGCG高内相Pickering乳液在倒置前后均未流动，始终停留在瓶子底部。
上述所有实例中的乳液的类型是通过观察乳液液滴在水和油中的分散情况来判断的。将获得的乳液滴到水中，乳液迅速分散开来，而滴到油中则不分散，维持液滴的形状，说明所有获得的乳液时水包油型的(如图8所示)。
最后，需要说明的是，以上优选实例仅为本发明的几个具体实例，本发明不只限于以上实例，还可以有许多的变形。从本发明公开的内容直接或间接得来的所有变形，均应认为是本发明的保护范围。
Claims (8)
1.一种茶多酚纳米粒子稳定的Pickering乳液的制备方法，其特征在于：包括以下具体步骤：
(1) 水相的制备：将具有抗氧化功能的茶多酚纳米粒子作为Pickering乳液的稳定剂，将其用去离子水配制成溶液作为Pickering乳液的水相；
(2) Pickering乳液的制备：将油相与步骤(1)中配制的水相混合，剪切乳化，获得Pickering乳液；
(3) 凝胶状Pickering乳液的制备：向步骤(2)获得的乳液中加入PEG水溶液，再剪切乳化，获得凝胶状的Pickering乳液；
(4) 高内相Pickering乳液的制备：向步骤(2)获得的乳液中继续添加油相，剪切乳化，得到高内相的Pickering乳液。
2.根据权利要求1所述的茶多酚纳米粒子稳定的Pickering乳液的制备方法，其特征在于：茶多酚纳米粒子包括表没食子儿茶素没食子酸酯(EGCG)纳米粒子、茶多酚纳米粒子中的至少一种。
3.根据权利要求1所述的多酚纳米粒子稳定的Pickering乳液的制备方法，其特征在于：步骤(1)中所述的多酚纳米粒子溶液的质量浓度为0.5%-4%。
4.根据权利要求1所述的多酚纳米粒子稳定的Pickering乳液的制备方法，其特征在于：步骤(2)中所述的油相为植物油或有机溶剂；植物油为亚麻籽油、橄榄油中的至少一种；有机溶剂为正己烷、乙酸乙酯、二氯甲烷中的至少一种。
5.根据权利要求1所述的多酚纳米粒子稳定的Pickering乳液的制备方法，其特征在于：步骤(2)中所述的水相与油相的体积比为2:3-1:3。
6.根据权利要求1所述的多酚纳米粒子稳定的Pickering乳液的制备方法，其特征在于：步骤(2)中所述的剪切乳化的转速为8000-12000 rpm，时间为30 s-180 s。
7.根据权利要求1所述的多酚纳米粒子稳定的Pickering乳液的制备方法，其特征在于：步骤(3)中所述的PEG水溶液包括分子量为800、4000、10000、20000的PEG中的至少一种；质量浓度为1%-5%；乳液与PEG水溶液的体积比为9:1-3:1。
8.权利要求1-7任一权利要求所述方法制备得到的Pickering乳液。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011548459.7A CN114672318A (zh) | 2020-12-24 | 2020-12-24 | 一种茶多酚纳米粒子稳定的皮克林乳液及其制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011548459.7A CN114672318A (zh) | 2020-12-24 | 2020-12-24 | 一种茶多酚纳米粒子稳定的皮克林乳液及其制备方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114672318A true CN114672318A (zh) | 2022-06-28 |
Family
ID=82071187
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011548459.7A Pending CN114672318A (zh) | 2020-12-24 | 2020-12-24 | 一种茶多酚纳米粒子稳定的皮克林乳液及其制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114672318A (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115886204A (zh) * | 2022-12-20 | 2023-04-04 | 大连工业大学 | 一种用于饺子馅料添加剂的Pickering高内相乳液的制备方法 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105817152A (zh) * | 2016-03-18 | 2016-08-03 | 东华大学 | 一种具有生物相容性和生物可降解性的Pickering乳液及其制备方法 |
| US20180141015A1 (en) * | 2015-07-28 | 2018-05-24 | Korea Advanced Institute Of Science And Technology | Pickering emulsion and method of preparing the same |
| CN110623937A (zh) * | 2018-06-21 | 2019-12-31 | 四川大学 | 茶多酚基多功能纳米复合物及其制备方法与应用 |
| CN111534110A (zh) * | 2020-05-29 | 2020-08-14 | 华南农业大学 | 一种醇溶蛋白-酚型抗氧化剂纳米粒子及其制备的皮克林乳液 |
-
2020
- 2020-12-24 CN CN202011548459.7A patent/CN114672318A/zh active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180141015A1 (en) * | 2015-07-28 | 2018-05-24 | Korea Advanced Institute Of Science And Technology | Pickering emulsion and method of preparing the same |
| CN105817152A (zh) * | 2016-03-18 | 2016-08-03 | 东华大学 | 一种具有生物相容性和生物可降解性的Pickering乳液及其制备方法 |
| CN110623937A (zh) * | 2018-06-21 | 2019-12-31 | 四川大学 | 茶多酚基多功能纳米复合物及其制备方法与应用 |
| CN111534110A (zh) * | 2020-05-29 | 2020-08-14 | 华南农业大学 | 一种醇溶蛋白-酚型抗氧化剂纳米粒子及其制备的皮克林乳液 |
Non-Patent Citations (1)
| Title |
|---|
| 薛万波: "用于稳定Pickering 乳液的氨基化明胶纳米颗粒的制备", 《精细化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115886204A (zh) * | 2022-12-20 | 2023-04-04 | 大连工业大学 | 一种用于饺子馅料添加剂的Pickering高内相乳液的制备方法 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110917137B (zh) | 一种醇溶蛋白纳米颗粒和淀粉纳米颗粒协同稳定的皮克林乳液的制备方法 | |
| Walia et al. | Fish oil based vitamin D nanoencapsulation by ultrasonication and bioaccessibility analysis in simulated gastro-intestinal tract | |
| Soleimanian et al. | Formulation and characterization of novel nanostructured lipid carriers made from beeswax, propolis wax and pomegranate seed oil | |
| EP2726104A1 (en) | Method of forming encapsulated compositions with enhanced solubility and stability | |
| Xie et al. | Encapsulation of astaxanthin-enriched camelina oil extract in ovalbumin/gum arabic stabilized emulsion with/without crosslinking by tannic acid | |
| CN102552058A (zh) | 复合维生素脂质纳米粒及其制备方法 | |
| Wei et al. | Fabrication and characterization of emulsions stabilized by tannic acid-wheat starch complexes | |
| KR100951706B1 (ko) | 레스베라트롤을 함유하는 나노에멀젼, 나노입자 및 그제조방법 | |
| Zhang et al. | The influence of maltodextrin on the physicochemical properties and stabilization of beta-carotene emulsions | |
| CN114672318A (zh) | 一种茶多酚纳米粒子稳定的皮克林乳液及其制备方法 | |
| CN112544982B (zh) | 一种纳米硒皮克林乳液及其制备方法与应用 | |
| CN113426389B (zh) | 一种醇溶蛋白微胶囊的制备方法和产品 | |
| Ma et al. | Encapsulation of emulsions by a novel delivery system of fluid core–hard shell biopolymer particles to retard lipid oxidation | |
| CN112602875A (zh) | 一种制备包覆光敏剂的食品级纳米乳液的方法 | |
| CN114795998B (zh) | 一种西红花苷双层包裹微囊的制备方法 | |
| Kumar et al. | Effect of self nanoemulsifying drug delivery system (SNEDDS) on intestinal permeation and anti-diabetic activity of Berberis aristata extract: in-vitro and ex-vivo studies | |
| de Castro Reis et al. | Evaluation of Nanostructured Lipid Carriers Produced with Interesterified Buriti Oil | |
| CN113116820A (zh) | 一种虾青素皮克林乳液及其制备方法 | |
| Reis et al. | A modified premix method for the emulsification of spearmint essential oil (Mentha spicata) by ceramic membranes | |
| CN114126587B (zh) | 用于制备微型乳剂的组合物、微型乳剂、它们的制造方法、以及微型乳剂的应用 | |
| CN110583972A (zh) | 一种蛋白-多酚复合体及其制备方法和应用 | |
| CN114452227A (zh) | 一种反溶剂重结晶法制备水包油包醇多重皮克林乳液的方法 | |
| Ge et al. | Storage stability and in vitro digestion of apigenin encapsulated in Pickering emulsions stabilized by whey protein isolate–chitosan complexes | |
| CN107233260B (zh) | 一种复方茶多酚纳米乳及其制备方法和应用 | |
| CN113367323A (zh) | 一种食品级多功能木质素/二氧化硅纳米颗粒乳化剂的绿色制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220628 |
|
| RJ01 | Rejection of invention patent application after publication |