CN114096225A - 包含姜二醇的口腔护理组合物及制备该组合物的方法 - Google Patents
包含姜二醇的口腔护理组合物及制备该组合物的方法 Download PDFInfo
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- CN114096225A CN114096225A CN202080027229.8A CN202080027229A CN114096225A CN 114096225 A CN114096225 A CN 114096225A CN 202080027229 A CN202080027229 A CN 202080027229A CN 114096225 A CN114096225 A CN 114096225A
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- Prior art keywords
- zingiberol
- composition
- polyol
- weight
- oral care
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- OMSYGYSPFZQFFP-UHFFFAOYSA-J zinc pyrophosphate Chemical compound [Zn+2].[Zn+2].[O-]P([O-])(=O)OP([O-])([O-])=O OMSYGYSPFZQFFP-UHFFFAOYSA-J 0.000 description 1
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
-
- 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
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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Abstract
产生包含姜二醇的口腔护理组合物的方法，该方法包括以下步骤：i)将姜二醇加入多元醇或多元醇混合物，该多元醇混合物包含小于多元醇混合物的5重量％的水，以形成悬浮液或溶液形式的姜二醇预混物；ii)将所得悬浮液或溶液加入液体基质组合物中。
Description
本发明涉及一种口腔护理组合物，更具体地涉及一种用于施用于局部表面或口腔的组合物。
背景技术
我们消费的许多产品对我们的牙齿和口腔都有负面影响。例如，酸性饮料和糖果可通过侵蚀牙釉质(其是保护牙齿的外涂层)导致牙齿腐蚀。粘性食物会积聚在牙齿之间的间隙中以及牙龈和牙齿之间的区域。没有良好的口腔卫生时，这些会随着时间的推移在口腔细菌的帮助下变硬，形成称为牙菌斑的薄膜。牙龈炎是由牙菌斑和/或细菌积聚引起的牙龈炎症过程。在牙龈炎期间，存在于牙菌斑生物膜及其相应成分中的细菌与牙龈组织相互作用。牙龈炎是牙周病的轻度阶段，并且定义为可逆性炎症。据信良好的口腔卫生习惯如刷牙和使用具有治疗性抗菌和抗炎功效的漱口水产品可能是个人减少牙龈炎的有效方法。慢性牙龈炎会导致刷牙时牙龈轻微出血。当炎症过程扩展到牙周韧带和牙槽骨和/或对健康产生显著的全身影响时，牙龈炎可能发展为更严重的状态(慢性牙周炎)。慢性牙周炎在到牙齿移位、松动或丢失时是无症状的。
KR100835899(Korean Res.Inst of Bioscience，2008)公开了生姜提取物或从中分离出的姜辣素提供为表现出抗菌能力和杀菌能力，从而有效用于预防或治疗牙周病。
WO2018/041544公开了姜二醇和维生素B3的组合作为减轻炎症的活性物，其可用于口腔、头皮/毛发和皮肤护理产品。
然而，产生其中姜二醇均匀分布在整个产品中的口腔护理组合物是困难的。本发明公开了一种姜二醇均匀分布在整个产品中的制造方法。
发明内容
本发明涉及一种产生包含姜二醇的口腔护理组合物的方法，该方法包括以下步骤：
i)将姜二醇加入多元醇或多元醇混合物中，该多元醇混合物包含小于多元醇混合物5重量％的水，以形成悬浮液或溶液形式的姜二醇预混物；
ii)将所得预混物加入液体基质组合物中。
本发明进一步涉及包含姜二醇组合物的口腔护理组合物，其中姜二醇为多晶形式的。
发明详述
根据本发明制备的组合物包含姜二醇。
姜二醇也以化学名称1-(4-羟基-3-甲氧基苯基)癸烷3,5-二醇已知。用于本发明组合物的姜二醇必须在化学反应中合成。合适的化学合成方法包括在0至10℃的温度下将姜辣素加入合适的溶剂和还原剂中；将反应混合物温热至15至25℃以形成姜二醇；以及使用溶剂萃取从混合物分离姜二醇。
本发明的姜二醇具有以下所示化学结构：
1-(4-羟基-3-甲氧基苯基)癸烷-3,5-二醇；
WO2018/041544中描述了可用于制备姜二醇的各种可能的化学品和工艺条件。
优选的是，如果姜二醇以0.01重量％至5重量％，更优选0.05重量％至2重量％，最优选0.1重量％至1重量％的水平存在于总组合物中。
优选地，预混物中姜二醇与多元醇的重量比为2∶1至1∶15，更优选1∶1至1∶10，最优选1∶2至1∶6。
优选地，在40℃至90℃，更优选50℃至70℃的温度下将姜二醇加入多元醇或多元醇混合物中以形成预混物，如果多元醇是甘油，则这些温度是特别优选的。
基础组合物优选包含水和/或山梨糖醇，或当组合物在非水性甘油中时。
优选的方法包括以下步骤：
i)将姜二醇加入多元醇或多元醇混合物中，该多元醇混合物包含小于多元醇混合物5重量％的水，以形成悬浮液或溶液形式的姜二醇预混物；
ii)形成包含多元醇和颗粒的液体基质组合物；
iii)将姜二醇预混物加入液体基质组合物中；
iv)向所得组合物中加入另外的颗粒。
基础组合物优选包含颗粒材料，优选地颗粒材料包含二氧化硅。优选的是，预处理组合物i)中二氧化硅的水平为组合物中二氧化硅总水平的20至80重量％，更优选30至70重量％，最优选40至60重量％。
如果存在表面活性剂，则优选的是在步骤iv)中将表面活性剂与另外的颗粒一起加入。
在优选的实施方案中，姜二醇预混物的多元醇包含甘油。优选的是如果用于溶解姜二醇以形成预混物的多元醇混合物包含总多元醇混合物的至少95重量％的单一多元醇，优选99重量％。
本发明的组合物为口腔护理组合物，优选的是其用于清洁口腔的表面，并且称为口腔护理组合物。
因此，本发明组合物的优选产品形式是适合刷牙和/或冲洗口腔表面的那些。
本发明的组合物最优选为洁齿剂的形式。术语“洁齿剂”表示用于清洁口腔表面的口腔组合物。这种组合物不出于治疗试剂的全身施用目的而有意吞咽，而是应用于口腔，用于处理口腔，然后漱出。通常，这样的组合物与清洁工具例如牙刷结合使用，通常通过将其施用于牙刷的刷毛，然后刷洗口腔的可及表面。
优选地，洁齿剂/牙膏呈可挤出的半固体形式，例如乳膏、糊剂或凝胶(或其混合物)。
优选地，液体基质包含水，还优选的是如果液体基质包含山梨糖醇。在洁齿剂中，山梨糖醇和水的组合是优选的。
在一些实施方案中，水的水平为总组合物的15至50重量％，在其他实施方案中，水的水平保持在最低限度，此类组合物被称为非水性的。在非水性组合物中，水的水平低于总组合物的0.5重量％。
除了上述指定的成分之外，根据本发明的组合物(例如洁齿剂/牙膏)通常可以包含其他成分以提高性能和/或消费者可接受性。
根据本发明的组合物，特别是牙膏，优选包含颗粒研磨材料，例如二氧化硅、氧化铝、碳酸钙、磷酸二钙、焦磷酸钙、羟基磷灰石、三偏磷酸盐、不溶性六偏磷酸盐等，包括附聚的颗粒研磨材料，按口腔护理组合物的重量计，其量通常在3％和60％之间。
优选地，该组合物，特别是牙膏，包含二氧化硅基磨料。本发明中使用的优选的磨料二氧化硅是具有低折射率的二氧化硅。它可用作唯一的磨料二氧化硅，或与低水平的其他磨料二氧化硅如根据EP236070的那些结合使用。在本发明中用作磨料的低折射率二氧化硅优选是具有在1.41-1.47范围内，优选1.435-1.445范围内的表观折射率(R.I.)，优选具有在5至15mm之间的重均粒度，在10和100m2/g之间的BET(氮)表面积，以及约70-150cm3/100g吸油量的二氧化硅，但也可以使用具有更低表观折射率的磨料二氧化硅。合适的低折射率磨料二氧化硅(例如，具有在1.435和1.445之间的R.I.)的典型实例是购自RhonePoulenc的Tixosil 63和73；购自Degussa的Sident 10；购自Zeofinn的Zeodent 113；购自Huber的Zeodent 124，购自Crosfield Chemicals的Sorbosil AC 77(具有约1.440的R.I.)。这些二氧化硅在组合物中的量通常为5-60重量％，通常为5-20重量％。
依据所选择的材料，该组合物(特别是如果牙膏)优选包含比例为约0.10至约15重量％的无机或天然或合成增稠剂或胶凝剂。本发明的洁齿剂组合物中的增稠剂的这些比例形成可挤出的形状保持产品，该产品可以从管中挤压到牙刷上，并且不会落入牙刷的刷毛之间，而是可以在其上大体上保持其形状。可用于本发明实践的合适增稠剂或胶凝剂包括无机增稠二氧化硅，例如可从Huber Corporation以商品名Zeodent 165获得的无定形二氧化硅、爱尔兰藓、ι-卡拉胶、黄蓍胶和聚乙烯吡咯烷酮。
根据本发明的组合物优选包含聚合物沉积助剂。优选地，该组合物包含酸酐聚合物，特别优选的是马来酸酐与甲基乙烯基醚的共聚物，其中酸酐部分可以是部分或完全水解或醇解的形式。优选的共聚物包括Gantrez(R)聚合物，例如：
Gantrez S-95：分子量216,000；游离酸；
Gantrez S-96：分子量700,000；游离酸；
Gantrez S-97：分子量1,500,000；游离酸；和
Gantrez MS-955：分子量1,060,000；钙/钠盐。
特别优选的马来酸和甲基乙烯基醚的共聚物具有1,000,000或更大的分子量，并且尤其优选的材料是Gantrez S-97。
根据本发明的组合物可包含牙齿增白剂。增白剂优选包含绿色和/或蓝色颜料。在本发明的上下文中，颜料通常理解为在相关温度下不溶于相关介质的遮盖物/材料。这与可溶的染料形成对比。在本发明的上下文中，“相关介质”是人唾液，在刷牙期间在口腔温度，即至多37℃下使用组合物的液体介质。作为合理的近似，相关介质可视为是水，相关温度为25℃。
优选地，蓝色颜料是颜料蓝15，更优选颜料蓝15:1、15:2、15:3、15:4、15:5或15:6，最优选15:1。优选的颜料是蓝色颜料，其是酞菁蓝颜料、CI第74160号、Covarine蓝。
优选的绿色颜料是酞菁绿，优选酞菁绿CI-74260。
优选地，组合物中颜料的总水平为0.01重量％至3重量％，更优选0.02重量％至2重量％。
如果组合物是牙膏，则它可以是双相糊剂，其中增白颜料存在于一个相中。
根据本发明的组合物可包含水溶性或水微溶性锌离子源，例如氯化锌、乙酸锌、葡萄糖酸锌、硫酸锌、氟化锌、柠檬酸锌、乳酸锌、氧化锌、单甘油锌、酒石酸锌、焦磷酸锌和马来酸锌；
根据本发明的组合物可以包含口腔护理酶体系，例如产生过氧化氢的酶体系(例如氧化还原酶葡萄糖氧化酶)、淀粉转葡糖苷酶、葡聚糖酶和/或非水溶性葡聚糖酶(任选在提供锌离子的化合物和/或8-羟基喹啉衍生物的存在下)、乳过氧化物酶、乳铁蛋白、溶菌酶及其混合物；
本发明的组合物可包含氟化物源，例如氟化钠、氟化亚锡、焦磷酸亚锡、单氟磷酸钠、氟化锌铵、氟化锡铵、氟化钙、氟化钴铵及其混合物；
在一个实施方案中，包含在本发明组合物中的一类优选口腔护理活性物包括用于牙齿再矿化的试剂。本发明上下文中的术语“再矿化”是指在牙齿上原位生成羟基磷灰石。
用于牙齿再矿化的合适试剂的具体实例是钙源和磷酸盐源的混合物，其在递送至牙齿时导致在牙齿上原位生成羟基磷灰石。
可在本上下文中使用的钙源类型(下文称为“再矿化钙源”)的说明性实例包括例如磷酸钙、葡萄糖酸钙、氧化钙、乳酸钙、甘油磷酸钙、碳酸钙、氢氧化钙、硫酸钙、羧甲基纤维素钙、藻酸钙、柠檬酸的钙盐、硅酸钙及其混合物。优选地，再矿化钙源是硅酸钙。
基于口腔护理组合物的总重量，本发明的组合物中的再矿化钙源(例如硅酸钙)的量通常为1％至30％，优选5％至20％(按总重量计)的再矿化钙源。
可在本上下文中使用的磷酸盐源类型(下文称为“再矿化磷酸盐源”)的说明性实例包括例如磷酸二氢钠、磷酸氢二钠、焦磷酸钠、焦磷酸四钠、三聚磷酸钠、六偏磷酸钠、磷酸二氢钾、磷酸三钠、磷酸三钾及其混合物。优选地，再矿化磷酸盐源是磷酸三钠和磷酸二氢钠的混合物。
基于口腔护理组合物的总重量，本发明的组合物中的再矿化磷酸盐源(例如磷酸三钠和磷酸二氢钠)的量通常为2至15％，优选4至10％(按总重量计)的再矿化磷酸盐源。
也可以使用任何上述材料的混合物。
根据本发明的组合物可以包含本领域常见的其他成分，例如：
抗菌剂，例如氯己定、血根碱提取物、甲硝唑、季铵化合物例如氯化十六烷基吡啶；双胍类，例如氯己定二葡糖酸盐、海克替啶、奥替尼啶、阿来西定；和卤化双酚化合物，例如2,2'亚甲基双-(4-氯-6-溴苯酚)；
抗炎剂，例如布洛芬、氟比洛芬、阿司匹林、吲哚美辛等；
防龋齿剂，例如氟化钠和氟化亚锡、氟化胺、单氟磷酸钠、三偏磷酸钠和酪蛋白；
菌斑缓冲剂，例如尿素、乳酸钙、甘油磷酸钙和聚丙烯酸锶；
维生素，例如维生素A、C和E；
植物提取物；
植物来源的抗氧化剂，例如类黄酮、儿茶酸、多酚和单宁化合物及其混合物；
脱敏剂，例如柠檬酸钾、氯化钾、酒石酸钾、碳酸氢钾、草酸钾、硝酸钾和锶盐；
抗牙结石剂，例如碱金属焦磷酸盐、含次磷酸盐的聚合物、有机膦酸盐和磷酰柠檬酸等；
生物分子，例如细菌素、抗体、酶等；
香味剂，例如薄荷和留兰香油；
蛋白质材料，例如胶原；
防腐剂；
遮光剂；
氨基酸，例如精氨酸
着色剂；
pH调节剂；
甜味剂；
药学上可接受的载体，例如淀粉、蔗糖、水或水/酒精体系等；
表面活性剂，例如阴离子、非离子、阳离子和两性离子或两性表面活性剂；
保湿剂，例如甘油、山梨糖醇、丙二醇、木糖醇、乳糖醇等；
粘合剂和增稠剂，例如羧甲基纤维素钠、羟乙基纤维素
黄原胶、阿拉伯树胶等，以及合成聚合物，例如聚丙烯酸盐和羧基乙烯基聚合物例如
还可以包括可以增强活性成分例如抗抗菌剂的递送的聚合物化合物；
用以缓冲口腔护理组合物的pH和离子强度的缓冲剂和盐；并且
可以包含的其他任选成分是例如漂白剂，例如过氧化合物，例如过氧化二磷酸钾，泡腾体系如碳酸氢钠/柠檬酸体系和变色体系。
现在将通过以下非限制性实施例举例说明本发明。
具体实施方式
实施例
通过将水+山梨糖醇混合，然后将TiO2、糖精和PEG 1500以及氟化钠加入到混合物中来制备基础组合物。接着加入二氧化硅和羧甲基纤维素钠。
在单独的容器中将姜二醇添加到表1中列出的多元醇中。将混合物加热至65℃并搅拌混合物。将所得姜二醇预混物加入基础组合物中。
最后，加入二氧化硅、表面活性剂和其他微量成分。
实施例的配方如表1所示：
表1
*与姜二醇作为预混物而添加。
**在配制中
配制的容易度如表2所示。
表2
| 实施例 | 结果 |
| 1 | 姜二醇在牙膏中均匀分散 |
| 3 | 姜二醇在牙膏中不那么均匀的分散 |
| 2 | 姜二醇在牙膏配制物中均匀分散 |
| A | 难以配制，不分散 |
表2的结果表明，与对比例相比，根据本发明的实施例更容易配制组合物。
Claims (14)
1.一种产生包含姜二醇的口腔护理组合物的方法，所述方法包括以下步骤：
i)将姜二醇加入多元醇或多元醇混合物以形成悬浮液或溶液形式的姜二醇预混物，该多元醇混合物包含小于所述多元醇混合物的5重量％的水；
ii)将所得悬浮液或溶液加入液体基质组合物中。
2.根据权利要求1所述的方法，其中所述多元醇或多元醇混合物包含甘油。
3.根据权利要求1或2所述的方法，其中在加入所述姜二醇时或加入所述姜二醇之后，所述多元醇或多元醇混合物处于50℃至90℃的温度。
4.根据前述权利要求中任一项所述的方法，其中所述多元醇混合物包含基于所述多元醇混合物总量的至少95重量％的单一多元醇。
5.根据前述权利要求中任一项所述的方法，其中所述姜二醇存在于所述组合物总量中的水平为0.01重量％至5重量％，优选0.05重量％至2重量％，更优选0.1重量％至1重量％。
6.根据前述权利要求中任一项所述的方法，其中所述预混物中姜二醇与多元醇的重量比为2∶1至1∶15，优选1∶1至1∶10，更优选1∶2至1∶6。
7.根据前述权利要求中任一项所述的方法，其中所述液体基质组合物包含水和山梨糖醇。
8.根据权利要求7所述的方法，其中所述总组合物中水的水平为所述组合物总量的15重量％至50重量％。
9.根据前述权利要求中任一项所述的方法，其中所述组合物包含颗粒。
10.根据前述权利要求中任一项所述的方法，其中所述液体基质组合物包含颗粒。
11.根据前述权利要求中任一项所述的方法，其中所述颗粒包含二氧化硅。
12.根据权利要求9至11中任一项所述的方法，其中在加入所述姜二醇之后将所述颗粒的一部分加入所述液体基质组合物中。
13.根据前述权利要求中任一项所述的方法，其中所述口腔护理组合物是洁齿剂。
14.根据前述权利要求中任一项的口腔护理组合物，其中所述姜二醇为多晶形式。
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
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| EP19167838.2 | 2019-04-08 | ||
| EP19167838 | 2019-04-08 | ||
| PCT/EP2020/051635 WO2020207633A1 (en) | 2019-04-08 | 2020-01-23 | Oral care composition comprising gingerdiol and process for producing the composition |
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| CN114096225A true CN114096225A (zh) | 2022-02-25 |
| CN114096225B CN114096225B (zh) | 2023-11-14 |
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| EP (1) | EP3952829B1 (zh) |
| CN (1) | CN114096225B (zh) |
| BR (1) | BR112021016929A2 (zh) |
| CL (1) | CL2021002535A1 (zh) |
| WO (1) | WO2020207633A1 (zh) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102639189A (zh) * | 2009-12-04 | 2012-08-15 | 高露洁-棕榄公司 | 含有姜提取物的口腔组合物及相关方法 |
| CN104414869A (zh) * | 2013-09-02 | 2015-03-18 | 西姆莱斯股份公司 | 一种皮肤和/或毛发美白混合物 |
| US20180021231A1 (en) * | 2014-10-30 | 2018-01-25 | Conopco, Inc., D/B/A Unilever | Method of controlling sweat production |
| WO2018041544A1 (en) * | 2016-08-30 | 2018-03-08 | Unilever N.V. | A personal care composition |
| CN107847413A (zh) * | 2015-05-28 | 2018-03-27 | 西姆莱斯股份公司 | 含有姜根提取物的化妆品组合物 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB8604985D0 (en) | 1986-02-28 | 1986-04-09 | Unilever Plc | Precipitated silicas |
| US5037633A (en) * | 1990-08-16 | 1991-08-06 | Chesebrough-Pond's Usa Co., Division Of Conopco, Inc. | Microbiologically stabilized phase for bicarbonate toothpaste manufacture |
| KR100835899B1 (ko) | 2006-12-12 | 2008-06-09 | 한국생명공학연구원 | 생강 추출물 또는 이로부터 분리된 진저롤을 포함하는치주질환의 예방 또는 치료용 조성물 |
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2020
- 2020-01-23 EP EP20703158.4A patent/EP3952829B1/en active Active
- 2020-01-23 WO PCT/EP2020/051635 patent/WO2020207633A1/en active Search and Examination
- 2020-01-23 CN CN202080027229.8A patent/CN114096225B/zh active Active
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102639189A (zh) * | 2009-12-04 | 2012-08-15 | 高露洁-棕榄公司 | 含有姜提取物的口腔组合物及相关方法 |
| CN104414869A (zh) * | 2013-09-02 | 2015-03-18 | 西姆莱斯股份公司 | 一种皮肤和/或毛发美白混合物 |
| US20180021231A1 (en) * | 2014-10-30 | 2018-01-25 | Conopco, Inc., D/B/A Unilever | Method of controlling sweat production |
| CN107847413A (zh) * | 2015-05-28 | 2018-03-27 | 西姆莱斯股份公司 | 含有姜根提取物的化妆品组合物 |
| WO2018041544A1 (en) * | 2016-08-30 | 2018-03-08 | Unilever N.V. | A personal care composition |
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| Publication number | Publication date |
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| CL2021002535A1 (es) | 2022-04-29 |
| WO2020207633A1 (en) | 2020-10-15 |
| CN114096225B (zh) | 2023-11-14 |
| BR112021016929A2 (pt) | 2021-11-03 |
| EP3952829A1 (en) | 2022-02-16 |
| EP3952829B1 (en) | 2022-11-02 |
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