CN108420077A - 一种维生素e纳米乳液及其制备方法 - Google Patents
一种维生素e纳米乳液及其制备方法 Download PDFInfo
- Publication number
- CN108420077A CN108420077A CN201810593024.0A CN201810593024A CN108420077A CN 108420077 A CN108420077 A CN 108420077A CN 201810593024 A CN201810593024 A CN 201810593024A CN 108420077 A CN108420077 A CN 108420077A
- Authority
- CN
- China
- Prior art keywords
- vitamin
- lotion
- nano
- tween
- water
- 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
- 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 title claims abstract description 134
- 229930003427 Vitamin E Natural products 0.000 title claims abstract description 67
- 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 title claims abstract description 67
- 235000019165 vitamin E Nutrition 0.000 title claims abstract description 67
- 229940046009 vitamin E Drugs 0.000 title claims abstract description 67
- 239000011709 vitamin E Substances 0.000 title claims abstract description 67
- 239000006210 lotion Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000007908 nanoemulsion Substances 0.000 claims abstract description 12
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims abstract description 11
- 229920000053 polysorbate 80 Polymers 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 3
- 239000012498 ultrapure water Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000013019 agitation Methods 0.000 claims description 10
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 claims description 5
- 239000003643 water by type Substances 0.000 claims description 5
- 239000003995 emulsifying agent Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 235000013339 cereals Nutrition 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 235000020195 rice milk Nutrition 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- ZBCATMYQYDCTIZ-UHFFFAOYSA-N 4-methylcatechol Chemical compound CC1=CC=C(O)C(O)=C1 ZBCATMYQYDCTIZ-UHFFFAOYSA-N 0.000 abstract 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 125000005471 saturated fatty acid group Chemical group 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
Classifications
-
- 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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/15—Vitamins
-
- 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
- A23L29/035—Organic compounds containing oxygen as heteroatom
-
- 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
- A23L29/035—Organic compounds containing oxygen as heteroatom
- A23L29/04—Fatty acids or derivatives
-
- 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
- A23L29/10—Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Mycology (AREA)
- Cosmetics (AREA)
Abstract
本发明公开了一种维生素E纳米乳液及其制备方法，其主要成分为维生素E，MCT，无水乙醇，Tween‑80，和超纯水。本发明的方法操作简单，且制备的纳米乳液分散性好，粒径均匀，稳定性好。
Description
技术领域
本发明属于纳米乳液制备领域，具体涉及一种维生素E纳米乳液及其制备方法。
背景技术
维生素E是一种淡黄色、粘稠的脂溶性维生素，对酸、碱和高温不敏感，但是在有氧和光照的情况下极易被破坏，故常置于密闭棕色瓶中贮藏。维生素E有良好的抗氧化效果，能清除肌体中的自由基和活性氧，因而能抗衰老，调节免疫能力、预防和治疗一些疾病。此外，维生素E还能提高皮肤抵御紫外线损伤的能力，淡化细纹，降低色素沉积，被广泛添加于化妆品中。但是，维生素E水溶性低，且易被氧化，故应用范围受到很大程度的限制。而将维生素E制成纳米乳液，能提高它的水溶性、生物利用度和稳定性。MCT是一种由饱和脂肪酸组成的无色粘稠度低的液体，有良好的氧化稳定性和热稳定性。MCT是一种很好的油相载体，将其与维生素E混合，能显著降低维生素E的粘度，进而减小纳米乳液的粒径；同时还有保护维生素E的功效。
将维生素E制成纳米乳液，具有以下优点：（1）维生素E在水中的溶解度和分散性得到提高；（2）包埋物维生素E得到保护，提高它的稳定性；（3）MCT为油相载体，制得的维生素E纳米乳液容易吸收，生物利用度高。
发明内容
本发明的目的在于针对现有技术的不足，提供了一种维生素E纳米乳液及其制备方法。本发明制备工艺简单，且制备的纳米乳液分散性好，粒径均匀，贮藏稳定性好。
为实现上述目的，本发明采用如下技术方案：
一种维生素E纳米乳液主要由以下原料制成：维生素E，中链甘油三酯（MCT），无水乙醇，Tween-80，和超纯水。
所述的维生素E纳米乳液以MCT为油相载体，Tween-80为乳化剂。
制备如上所述的维生素E纳米乳液的方法包括以下步骤：
（1）称量400~800mg的维生素E，200~600mg的MCT，用涡旋混匀器充分混合，随后放入水浴超声器中超声混匀30min，得维生素E与MCT的混合油相；
（2）称量20mg的维生素E与MCT混合油相，0.1g的无水乙醇以及0.1g的Tween-80于25mL的烧杯中，磁力搅拌研磨2min，使其充分混匀；
（3）将10mL超纯水加入到步骤（2）得到的混合液中，磁力搅拌12h，使得维生素E均匀分散于水相中，得到水包油型的维生素E粗乳液；
（4）将维生素E粗乳液置于水浴超声器中，超声40min，设置超声功率为200W，即得维生素E纳米乳液。
所制得的维生素E纳米乳液的粒径在14~40nm，PDI为0.1~0.3，Zeta电位-13.8~-11.0mV。
本发明的显著优点在于：
（1）维生素E纳米乳液制备过程中以无毒无害的MCT为油相载体，因而安全性更高。
（2）乳化剂Tween-80的质量浓度仅为1%，制得的乳液可以被用于食品工业领域。
（3）无水乙醇为助乳化剂，可以降低油水界面张力，从而降低纳米乳液的粒径和PDI。
（4）乳液的粒径小，分散性好，贮藏稳定性高；用本发明提供的组分和方法制备的维生素E纳米乳液的粒径分布在14-40nm范围内，PDI小于0.3。
（5）乳液的制备工艺条件简单，很容易应用于工业化生产。
具体实施方式
为进一步公开而不是限制本发明，以下结合实例对本发明作进一步的详细说明。
实施例1
一种维生素E纳米乳液的制备方法，具体步骤为：
（1）称量600mg的维生素E，400mg的MCT（两者质量比为3:2），用涡旋混匀器充分混合，随后放入水浴超声器中超声混匀30min，得维生素E与MCT的混合油相；
（2）称量20mg的维生素E与MCT混合油相，0.1g的无水乙醇以及0.1g的Tween-80于25mL的烧杯中，磁力搅拌研磨2min，使其充分混匀；
（3）将10mL超纯水加入到步骤（2）得到的混合液中，磁力搅拌12h，使得维生素E均匀分散于水相中，得到水包油型的维生素E粗乳液；
（4）将维生素E粗乳液置于水浴超声器中，超声40min，设置超声功率为200W，即得维生素E纳米乳液。
测得的维生素E纳米乳液平均粒径为14.68nm，PDI为0.195，电位-13.8mV。
实施例2
一种维生素E纳米乳液的制备方法，具体步骤为：
（1）称量400mg的维生素E，600mg的MCT（两者质量比为2:3），用涡旋混匀器充分混合，随后放入水浴超声器中超声混匀30min，得维生素E与MCT的混合油相；
（2）称量20mg的维生素E与MCT混合油相，0.1g的无水乙醇以及0.1g的Tween-80于25mL的烧杯中，磁力搅拌研磨2min，使其充分混匀；
（3）将10mL超纯水加入到步骤（2）得到的混合液中，磁力搅拌12h，使得维生素E均匀分散于水相中，得到水包油型的维生素E粗乳液；
（4）将维生素E粗乳液置于水浴超声器中，超声40min，设置超声功率为200W，即得维生素E纳米乳液。
测得的维生素E纳米乳液平均粒径为15.28nm，PDI为0.198，电位-12.5mV。
实施例3
一种维生素E纳米乳液的制备方法，具体步骤为：
（1）称量800mg的维生素E，200mg的MCT（两者质量比为4:1），用涡旋混匀器充分混合，随后放入水浴超声器中超声混匀30min，得维生素E与MCT的混合油相；
（2）称量20mg的维生素E与MCT混合油相，0.1g的无水乙醇以及0.1g的Tween-80于25mL的烧杯中，磁力搅拌研磨2min，使其充分混匀；
（3）将10mL超纯水加入到步骤（2）得到的混合液中，磁力搅拌12h，使得维生素E均匀分散于水相中，得到水包油型的维生素E粗乳液；
（4）将制得的维生素E粗乳液置于水浴超声器中，超声40min，设置超声功率为200W，即得维生素E纳米乳液。
测得的维生素E纳米乳液平均粒径为37.91nm，PDI为0.239，电位-11.0mV。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (4)
1.一种维生素E纳米乳液，其特征在于：主要由以下原料制成：维生素E，中链甘油三酯，无水乙醇，Tween-80和超纯水。
2.根据权利要求1所述的维生素E纳米乳液，其特征在于：所述维生素E乳液以中链甘油三酯为油相载体，Tween-80为乳化剂。
3.一种制备如权利要求1所述的维生素E纳米乳液的方法，其特征在于：包括以下步骤：
（1）称量400~800mg的维生素E，200~600mg的中链甘油三酯，用涡旋混匀器充分混合，随后放入水浴超声器中超声混匀30min，得维生素E与中链甘油三酯的混合油相；
（2）称量20mg的混合油相，0.1g的无水乙醇以及0.1g的Tween-80于25mL的烧杯中，磁力搅拌研磨2min，使其充分混匀；
（3）将10mL超纯水加入到步骤（2）得到的混合液中，磁力搅拌12h，使得维生素E均匀分散于水相中，得到水包油型的维生素E粗乳液；
（4）将维生素E粗乳液置于水浴超声器中，超声40min，设置超声功率为200W，即得维生素E纳米乳液。
4.一种如权利要求3所述的制备方法制得的维生素E纳米乳液，其特征在于：维生素E纳米乳液的粒径在14~40nm，PDI为0.1~0.3，Zeta电位-13.8~-11.0mV。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810593024.0A CN108420077A (zh) | 2018-06-11 | 2018-06-11 | 一种维生素e纳米乳液及其制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810593024.0A CN108420077A (zh) | 2018-06-11 | 2018-06-11 | 一种维生素e纳米乳液及其制备方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108420077A true CN108420077A (zh) | 2018-08-21 |
Family
ID=63164823
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810593024.0A Pending CN108420077A (zh) | 2018-06-11 | 2018-06-11 | 一种维生素e纳米乳液及其制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108420077A (zh) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546016A (zh) * | 2003-12-04 | 2004-11-17 | 东南大学 | 天然维生素e纳米制剂及其制备方法 |
| KR20090132357A (ko) * | 2008-06-20 | 2009-12-30 | 한국식품연구원 | 레스베라트롤을 함유하는 나노에멀젼, 나노입자 및 그제조방법 |
| CN103191670A (zh) * | 2013-04-15 | 2013-07-10 | 山东大学 | 一种聚合物稳定的纳米乳液的制备方法 |
| CN103520103A (zh) * | 2013-10-14 | 2014-01-22 | 陕西科技大学 | 一种维生素e纳米乳及其制备方法 |
| CN103859015A (zh) * | 2014-03-04 | 2014-06-18 | 浙江大学 | 月桂精油微乳液樱桃番茄保鲜剂及其制备方法 |
| CN106947594A (zh) * | 2017-05-10 | 2017-07-14 | 仲恺农业工程学院 | 一种延缓饲用油氧化的微乳液及其制备方法 |
| CN107496196A (zh) * | 2017-09-08 | 2017-12-22 | 苏州大学 | 超声纳米喷雾液体制剂及其制备方法 |
-
2018
- 2018-06-11 CN CN201810593024.0A patent/CN108420077A/zh active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546016A (zh) * | 2003-12-04 | 2004-11-17 | 东南大学 | 天然维生素e纳米制剂及其制备方法 |
| KR20090132357A (ko) * | 2008-06-20 | 2009-12-30 | 한국식품연구원 | 레스베라트롤을 함유하는 나노에멀젼, 나노입자 및 그제조방법 |
| CN103191670A (zh) * | 2013-04-15 | 2013-07-10 | 山东大学 | 一种聚合物稳定的纳米乳液的制备方法 |
| CN103520103A (zh) * | 2013-10-14 | 2014-01-22 | 陕西科技大学 | 一种维生素e纳米乳及其制备方法 |
| CN103859015A (zh) * | 2014-03-04 | 2014-06-18 | 浙江大学 | 月桂精油微乳液樱桃番茄保鲜剂及其制备方法 |
| CN106947594A (zh) * | 2017-05-10 | 2017-07-14 | 仲恺农业工程学院 | 一种延缓饲用油氧化的微乳液及其制备方法 |
| CN107496196A (zh) * | 2017-09-08 | 2017-12-22 | 苏州大学 | 超声纳米喷雾液体制剂及其制备方法 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Qiu et al. | Construction, stability, and enhanced antioxidant activity of pectin-decorated selenium nanoparticles | |
| Hosseinnia et al. | Optimization of Ziziphora clinopodiodes essential oil microencapsulation by whey protein isolate and pectin: A comparative study | |
| CN107550764B (zh) | 一种高稳定性的美藤果油水润q弹珠的制备方法 | |
| Mahdi et al. | Enhancement of antioxidant activity, antifungal activity, and oxidation stability of Citrus reticulata essential oil nanocapsules by clove and cinnamon essential oils | |
| TWI652107B (zh) | 分散液及水凝膠之形成方法 | |
| CN102300549B (zh) | 油包水型乳化防晒化妆品 | |
| Zhu et al. | Preparation of spray-dried soybean oil body microcapsules using maltodextrin: Effects of dextrose equivalence | |
| Choi et al. | Microencapsulation of gallic acid through the complex of whey protein concentrate-pectic polysaccharide extracted from Ulmus davidiana | |
| JP2011051972A (ja) | 有機無機複合粒子並びにその製造方法、該粒子を含む分散液および該粒子を配合した化粧料 | |
| CN105851057A (zh) | 表面处理氧化锌粉体、抗菌剂和抗菌性组合物 | |
| Silva et al. | Coupling of high-intensity ultrasound and mechanical stirring for producing food emulsions at low-energy densities | |
| Gallegos-Infante et al. | Physicochemical properties and antioxidant capacity of oak (Quercus resinosa) leaf infusions encapsulated by spray-drying | |
| Wang et al. | Waxy maize starch nanoparticles incorporated tea polyphenols to stabilize Pickering emulsion and inhibit oil oxidation | |
| Zhao et al. | Physical and oxidative stability of astaxanthin microcapsules prepared with liposomes | |
| Manne et al. | Pterocarpus marsupium Roxb. heartwood extract synthesized chitosan nanoparticles and its biomedical applications | |
| Nasri et al. | Sardinelle protein isolate as a novel material for oil microencapsulation: Novel alternative for fish by-products valorisation | |
| CN108420077A (zh) | 一种维生素e纳米乳液及其制备方法 | |
| CN103202780A (zh) | 一种化妆品用纳米精华液及其制备方法 | |
| Lan et al. | Rational design of food-grade polyelectrolyte complex coacervate for encapsulation and enhanced oral delivery of oenothein B | |
| Sharif et al. | Preparation, characterization and rheological properties of vitamin E enriched nanoemulsion. | |
| KR20180003902A (ko) | 리그닌-탄수화물 복합체 및 이의 제조방법 | |
| CN107661280A (zh) | 固态粉末化妆材料的制造方法和固态粉末化妆材料 | |
| CN113995137A (zh) | 一种由燕麦蛋白虫胶稳定的亚麻籽油皮克林乳液的制备方法 | |
| CN113304702B (zh) | 一种砂仁精油微胶囊的制备方法 | |
| Liu et al. | Preparation of low density TiO2/poly (methyl methacrylate) composite particles by emulsifier-free emulsion polymerization |
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: 20180821 |
|
| RJ01 | Rejection of invention patent application after publication |