JP7479254B2 - Dentifrice composition and method for inhibiting adsorption of isopropyl methylphenol to a container of a dentifrice composition - Google Patents
Dentifrice composition and method for inhibiting adsorption of isopropyl methylphenol to a container of a dentifrice composition Download PDFInfo
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- JP7479254B2 JP7479254B2 JP2020153850A JP2020153850A JP7479254B2 JP 7479254 B2 JP7479254 B2 JP 7479254B2 JP 2020153850 A JP2020153850 A JP 2020153850A JP 2020153850 A JP2020153850 A JP 2020153850A JP 7479254 B2 JP7479254 B2 JP 7479254B2
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- dentifrice composition
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- adsorption
- isopropyl methylphenol
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- 239000000203 mixture Substances 0.000 title claims description 75
- IJALWSVNUBBQRA-UHFFFAOYSA-N 4-Isopropyl-3-methylphenol Chemical compound CC(C)C1=CC=C(O)C=C1C IJALWSVNUBBQRA-UHFFFAOYSA-N 0.000 title claims description 59
- NFIDBGJMFKNGGQ-UHFFFAOYSA-N isopropylmethylphenol Natural products CC(C)CC1=CC=CC=C1O NFIDBGJMFKNGGQ-UHFFFAOYSA-N 0.000 title claims description 59
- 239000000551 dentifrice Substances 0.000 title claims description 53
- 238000001179 sorption measurement Methods 0.000 title claims description 26
- 238000000034 method Methods 0.000 title claims description 15
- 230000002401 inhibitory effect Effects 0.000 title claims description 10
- -1 polyoxyethylene Polymers 0.000 claims description 35
- 150000002222 fluorine compounds Chemical class 0.000 claims description 16
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 14
- 239000003945 anionic surfactant Substances 0.000 claims description 13
- 229920000092 linear low density polyethylene Polymers 0.000 claims description 12
- 239000004707 linear low-density polyethylene Substances 0.000 claims description 12
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 11
- 229910052731 fluorine Inorganic materials 0.000 claims description 11
- 239000011737 fluorine Substances 0.000 claims description 11
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 9
- 239000004359 castor oil Substances 0.000 claims description 8
- 235000019438 castor oil Nutrition 0.000 claims description 8
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 8
- 239000000606 toothpaste Substances 0.000 claims description 6
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- 239000003795 chemical substances by application Substances 0.000 claims description 3
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- 239000000796 flavoring agent Substances 0.000 description 14
- 235000019634 flavors Nutrition 0.000 description 14
- 230000000844 anti-bacterial effect Effects 0.000 description 13
- 239000002736 nonionic surfactant Substances 0.000 description 12
- 238000009472 formulation Methods 0.000 description 10
- 239000004698 Polyethylene Substances 0.000 description 9
- 229920001684 low density polyethylene Polymers 0.000 description 9
- 239000004702 low-density polyethylene Substances 0.000 description 9
- 229920000573 polyethylene Polymers 0.000 description 9
- 239000003921 oil Substances 0.000 description 8
- 235000019198 oils Nutrition 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 235000014113 dietary fatty acids Nutrition 0.000 description 7
- 239000000194 fatty acid Substances 0.000 description 7
- 229930195729 fatty acid Natural products 0.000 description 7
- 150000005215 alkyl ethers Chemical class 0.000 description 6
- 239000003899 bactericide agent Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000005020 polyethylene terephthalate Substances 0.000 description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 6
- 239000003082 abrasive agent Substances 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- 125000004432 carbon atom Chemical group C* 0.000 description 5
- 239000003205 fragrance Substances 0.000 description 5
- OSWPMRLSEDHDFF-UHFFFAOYSA-N methyl salicylate Chemical compound COC(=O)C1=CC=CC=C1O OSWPMRLSEDHDFF-UHFFFAOYSA-N 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 208000028169 periodontal disease Diseases 0.000 description 5
- NTOPKICPEQUPPH-UHFFFAOYSA-N IPMP Natural products COC1=NC=CN=C1C(C)C NTOPKICPEQUPPH-UHFFFAOYSA-N 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- XGRSAFKZAGGXJV-UHFFFAOYSA-N 3-azaniumyl-3-cyclohexylpropanoate Chemical compound OC(=O)CC(N)C1CCCCC1 XGRSAFKZAGGXJV-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
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- 150000008051 alkyl sulfates Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
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- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000011775 sodium fluoride Substances 0.000 description 3
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- 239000004094 surface-active agent Substances 0.000 description 3
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- XHXUANMFYXWVNG-ADEWGFFLSA-N (-)-Menthyl acetate Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@H]1OC(C)=O XHXUANMFYXWVNG-ADEWGFFLSA-N 0.000 description 2
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 2
- CFAKWWQIUFSQFU-UHFFFAOYSA-N 2-hydroxy-3-methylcyclopent-2-en-1-one Chemical compound CC1=C(O)C(=O)CC1 CFAKWWQIUFSQFU-UHFFFAOYSA-N 0.000 description 2
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
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- 239000004480 active ingredient Substances 0.000 description 2
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- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000001506 calcium phosphate Substances 0.000 description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 description 2
- 235000011010 calcium phosphates Nutrition 0.000 description 2
- ULDHMXUKGWMISQ-UHFFFAOYSA-N carvone Chemical compound CC(=C)C1CC=C(C)C(=O)C1 ULDHMXUKGWMISQ-UHFFFAOYSA-N 0.000 description 2
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- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 description 2
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 description 2
- 239000000417 fungicide Substances 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
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- 229930182470 glycoside Natural products 0.000 description 2
- JARKCYVAAOWBJS-UHFFFAOYSA-N hexanal Chemical compound CCCCCC=O JARKCYVAAOWBJS-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
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- UWKAYLJWKGQEPM-LBPRGKRZSA-N linalyl acetate Chemical compound CC(C)=CCC[C@](C)(C=C)OC(C)=O UWKAYLJWKGQEPM-LBPRGKRZSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001525 mentha piperita l. herb oil Substances 0.000 description 2
- VAMXMNNIEUEQDV-UHFFFAOYSA-N methyl anthranilate Chemical compound COC(=O)C1=CC=CC=C1N VAMXMNNIEUEQDV-UHFFFAOYSA-N 0.000 description 2
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- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical group [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Cosmetics (AREA)
Description
本発明は、イソプロピルメチルフェノールの容器への吸着が抑制され、経時においてイソプロピルメチルフェノールが安定化した、歯周疾患の予防又は抑制用として好適な歯磨組成物及び歯磨組成物における容器へのイソプロピルメチルフェノールの吸着抑制方法に関する。 The present invention relates to a dentifrice composition suitable for preventing or inhibiting periodontal disease, in which the adsorption of isopropyl methylphenol to a container is inhibited and isopropyl methylphenol is stabilized over time, and to a method for inhibiting the adsorption of isopropyl methylphenol to a container in a dentifrice composition.
う蝕、歯周病の2大口腔疾患の原因は、口腔内バイオフィルム中の各種細菌にあると考えられている。特に歯周病は、ポルフィロモナス・ジンジバリス等の偏性嫌気性グラム陰性桿菌を主とした細菌による感染症であり、殺菌剤の選定基準としてはバイオフィルムへの浸透力が重要となる。
難水溶性の殺菌剤であるイソプロピルメチルフェノールは、口腔バイオフィルム浸透性が高いことから、イソプロピルメチルフェノールを用いた歯磨剤が上市されている。
The two major oral diseases, dental caries and periodontal disease, are believed to be caused by various bacteria in oral biofilms. Periodontal disease in particular is an infectious disease caused mainly by obligate anaerobic gram-negative bacilli such as Porphyromonas gingivalis, and the ability of a bactericide to penetrate into biofilms is an important criterion for selecting a bactericide.
Isopropyl methylphenol, a poorly water-soluble bactericide, has high oral biofilm penetration, and toothpastes containing isopropyl methylphenol are on the market.
しかしながら、イソプロピルメチルフェノールは、難水溶性成分であるため、口腔用組成物に配合してチューブ等の容器に充填すると、特に可溶化状態が不十分な場合、容器素材として使用するポリエチレン等の樹脂に吸着し、安定性が低下するという問題があった。 However, because isopropylmethylphenol is a poorly water-soluble component, when it is mixed into an oral composition and filled into a container such as a tube, there is a problem that it is adsorbed by the resin, such as polyethylene, used as the container material, reducing stability, especially if the solubilization state is insufficient.
このような容器吸着の問題に対して、特許文献1~3には、容器面から難水溶性殺菌剤を安定配合する技術が提案されているが、これらの技術は、容器製造にかかわる新たな課題が生じるという問題があり、このため、容器に充填される内容物の面から難水溶性殺菌剤を安定化することが有効である。 In response to this problem of container adsorption, Patent Documents 1 to 3 propose techniques for stably blending poorly water-soluble fungicides from the container surface, but these techniques have the problem that new issues arise in container manufacturing. For this reason, it is more effective to stabilize the poorly water-soluble fungicide from the perspective of the contents filled into the container.
充填する内容物の面から、容器への吸着を抑制する技術として、特許文献4~7には、難水溶性殺菌剤と共に適切な界面活性剤や硫酸ナトリウム等の塩を歯磨剤組成物に配合することによって難水溶性殺菌剤の経時における残存率を向上する技術が提案されている。特許文献4、5では、ポリオキシエチレンアルキルエーテル、あるいはポリオキシエチレン硬化ヒマシ油及びカチオン性界面活性剤によってイソプロピルメチルフェノールの残存率が改善し、特許文献6では、ポリオキシエチレンアルキルエーテル及び硫酸ナトリウムによってイソプロピルメチルフェノールの保存後の殺菌力が改善することを開示している。 As a technology for suppressing adsorption to the container from the viewpoint of the contents to be filled, Patent Documents 4 to 7 propose a technology for improving the residual rate of a poorly water-soluble bactericide over time by blending an appropriate surfactant or a salt such as sodium sulfate together with the poorly water-soluble bactericide in a dentifrice composition. Patent Documents 4 and 5 disclose that the residual rate of isopropyl methylphenol is improved by polyoxyethylene alkyl ether or polyoxyethylene hydrogenated castor oil and a cationic surfactant, and Patent Document 6 discloses that the bactericidal power of isopropyl methylphenol after storage is improved by polyoxyethylene alkyl ether and sodium sulfate.
しかしながら、ノニオン性界面活性剤や塩の配合量が多くなるほど、イソプロピルメチルフェノールの殺菌力の低下や製剤安定性の低下を引き起こすという問題があり、このため、イソプロピルメチルフェノールの容器への吸着を抑制して安定性を向上する新たな技術の開発が望まれた。 However, there is a problem that the greater the amount of nonionic surfactant or salt used, the lower the bactericidal activity of isopropyl methylphenol and the lower the stability of the formulation. For this reason, there is a need for the development of a new technology that can suppress the adsorption of isopropyl methylphenol to the container and improve stability.
本発明は、上記事情に鑑みなされたもので、イソプロピルメチルフェノールの容器への吸着が抑制され、経時においてイソプロピルメチルフェノールが安定化した歯磨組成物及び歯磨組成物における容器へのイソプロピルメチルフェノールの吸着抑制方法を提供することを目的とする。 The present invention has been made in consideration of the above circumstances, and aims to provide a dentifrice composition in which adsorption of isopropyl methylphenol to a container is suppressed and in which isopropyl methylphenol is stabilized over time, and a method for suppressing adsorption of isopropyl methylphenol to a container in a dentifrice composition.
本発明者らは上記課題を解決すべく検討を重ねた結果、(A)イソプロピルメチルフェノールと共に、(B)アニオン性界面活性剤、(C)ノニオン性界面活性剤を配合し、最内層がポリエチレンからなる容器に充填した歯磨組成物に、(D)フッ素化合物をフッ素として1,100~3,000ppm配合することによって、イソプロピルメチルフェノールの前記容器への吸着が抑制され、経時においてイソプロピルメチルフェノールが安定化すること、また、十分かつ適度な泡立ち、製剤の外観安定性を確保できることを見出し、本発明をなすに至った。 As a result of extensive investigations aimed at solving the above problems, the inventors have discovered that by blending (A) isopropyl methyl phenol with (B) an anionic surfactant and (C) a nonionic surfactant together, and filling a dentifrice composition in a container with an innermost layer made of polyethylene, and blending (D) a fluorine compound at 1,100 to 3,000 ppm in terms of fluorine, the adsorption of isopropyl methyl phenol to the container is suppressed, isopropyl methyl phenol is stabilized over time, sufficient and appropriate foaming is achieved, and the appearance stability of the formulation can be ensured, which has led to the creation of the present invention.
一般的に歯磨組成物にはフッ素が添加されるが、一般的にその濃度は1,000ppm以下程度であり、このような1,100ppmに満たないフッ素濃度でフッ素化合物を添加したのでは、(A)成分と共に(B)、(C)成分を組み合わせ上記容器に充填した歯磨組成物において、イソプロピルメチルフェノールの容器吸着を抑制できないにもかかわらず、(D)成分のフッ素化合物をフッ素として1,100ppm以上という高濃度で使用すると、意外にも、(D)成分のフッ素化合物が吸着抑制剤として作用してイソプロピルメチルフェノールの容器吸着が抑制され、上記格別な作用効果を与える。
この場合、歯磨組成物に(A)イソプロピルメチルフェノールを配合し、泡立ち確保のために(B)アニオン性界面活性剤を配合し、かつイソプロピルメチルフェノールを可溶化させるために(C)ノニオン性界面活性剤を配合しても、イソプロピルメチルフェノールが容器に吸着して残存率が経時で低下するという問題が解決できず、ノニオン性界面活性剤の増量は製剤安定性の低下、更にはイソプロピルメチルフェノールの殺菌力低下を招き、また、アニオン性界面活性剤の増量は可溶化バランスの崩れ、それによる容器吸着の増加を招いた。そこで、本発明者らは、製剤安定性等を低下させることなく十分かつ適度な泡立ちを確保してイソプロピルメチルフェノールの容器吸着を抑制するため、更に検討を進めた結果、(A)、(B)、(C)成分の組み合わせにおいて、(D)成分のフッ素化合物が上述したように吸着抑制剤として特異的に作用し、これによって、イソプロピルメチルフェノールが経時において高率で残存する安定性を与え、また、十分かつ適度な泡立ち、60℃で1ヶ月保存しても液分離を抑制できる製剤の外観安定性を与えることもできた。更には、味を良好に保つこともできた。よって、本発明の歯磨組成物によれば、イソプロピルメチルフェノールを効果的に作用させ、その口腔バイオフィルム浸透殺菌力を十分に発現させることが可能となり、歯周疾患の予防又は抑制に好適に使用することができる。
Fluorine is generally added to dentifrice compositions, but the concentration is generally about 1,000 ppm or less. If a fluorine compound is added at a fluorine concentration of less than 1,100 ppm, it will be impossible to suppress adsorption of isopropyl methylphenol to the container in a dentifrice composition in which component (A) is combined with components (B) and (C) and packed in the above-mentioned container. However, when a fluorine compound of component (D) is used at a high concentration of 1,100 ppm or more in terms of fluorine, unexpectedly, the fluorine compound of component (D) acts as an adsorption inhibitor to suppress adsorption of isopropyl methylphenol to the container, thereby providing the above-mentioned special functional effect.
In this case, even if the dentifrice composition contains (A) isopropyl methylphenol, (B) anionic surfactant to ensure foaming, and (C) nonionic surfactant to solubilize isopropyl methylphenol, the problem of isopropyl methylphenol adsorbing to the container and decreasing the remaining rate over time cannot be solved, and an increase in the amount of nonionic surfactant leads to a decrease in the stability of the preparation and further to a decrease in the bactericidal power of isopropyl methylphenol, and an increase in the amount of anionic surfactant leads to a loss of solubilization balance, which leads to an increase in container adsorption. Therefore, the present inventors have further investigated in order to ensure sufficient and appropriate foaming without decreasing the stability of the preparation and to suppress the adsorption of isopropyl methylphenol to the container, and as a result, in the combination of (A), (B), and (C), the fluorine compound of (D) component acts specifically as an adsorption inhibitor as described above, thereby providing stability in which isopropyl methylphenol remains at a high rate over time, and also providing sufficient and appropriate foaming and external appearance stability of the preparation that can suppress liquid separation even when stored at 60°C for one month. Furthermore, the taste was also maintained at a good level. Therefore, according to the dentifrice composition of the present invention, it is possible to effectively use isopropyl methylphenol and fully exhibit its oral biofilm penetrating bactericidal activity, and the composition can be suitably used for preventing or suppressing periodontal disease.
界面活性剤、硫酸ナトリウム等の塩によって難水溶性殺菌剤の容器への吸着を抑制し、残存率を向上した特許文献4~7から、フッ素化合物によってイソプロピルメチルフェノールが安定化することは予測できない。 Based on Patent Documents 4 to 7, which show that the adsorption of poorly water-soluble disinfectants to containers is suppressed and the residual rate is improved by using surfactants and salts such as sodium sulfate, it is not possible to predict that isopropylmethylphenol would be stabilized by fluorine compounds.
従って、本発明は、下記の歯磨組成物及び歯磨組成物における容器へのイソプロピルメチルフェノールの吸着抑制方法を提供する。
請求項1:
(A)イソプロピルメチルフェノール、
(B)アニオン性界面活性剤、
(C)ノニオン性界面活性剤
を配合し、最内層がポリエチレンからなる容器に充填した歯磨組成物に、
(D)フッ素化合物をフッ素として1,100~3,000ppm
配合したことを特徴とする歯磨組成物。
請求項2:
(C)ノニオン性界面活性剤が、エチレンオキサイドの平均付加モル数20~100のポリオキシエチレン硬化ヒマシ油及び/又は炭素数10~18のアルキル基を有する、エチレンオキサイドの平均付加モル数5~40のポリオキシエチレンアルキルエーテルである請求項1記載の歯磨組成物。
請求項3:
(B)アニオン性界面活性剤が、ラウリル硫酸ナトリウムである請求項1又は2記載の歯磨組成物。
請求項4:
(A)成分を0.01~0.3質量%、(B)成分を0.6~2.5質量%、(C)成分を0.5~3質量%配合した請求項1、2又は3記載の歯磨組成物。
請求項5:
(B)/(C)が質量比として0.2~3である請求項1~4のいずれか1項記載の歯磨組成物。
請求項6:
更に、研磨剤を配合した請求項1~5のいずれか1項記載の歯磨組成物。
請求項7:
(A)イソプロピルメチルフェノール、
(B)アニオン性界面活性剤、
(C)ノニオン性界面活性剤
を配合し、最内層がポリエチレンからなる容器に充填した歯磨組成物に、
(D)フッ素化合物をフッ素として1,100~3,000ppm
配合することを特徴とする、前記歯磨組成物における容器へのイソプロピルメチルフェノールの吸着抑制方法。
請求項8:
(B)/(C)が質量比として0.2~3である請求項7記載の歯磨組成物における容器へのイソプロピルメチルフェノールの吸着抑制方法。
Therefore, the present invention provides the following dentifrice composition and method for inhibiting adsorption of isopropylmethylphenol to a container of a dentifrice composition.
Claim 1:
(A) isopropyl methylphenol,
(B) an anionic surfactant,
(C) A dentifrice composition containing a nonionic surfactant and filled in a container having an innermost layer made of polyethylene,
(D) Fluorine compounds: 1,100 to 3,000 ppm as fluorine
A dentifrice composition comprising:
Claim 2:
The dentifrice composition according to claim 1, wherein the nonionic surfactant (C) is polyoxyethylene hydrogenated castor oil having an average added mole number of ethylene oxide of 20 to 100 and/or polyoxyethylene alkyl ether having an average added mole number of ethylene oxide of 5 to 40 and an alkyl group having 10 to 18 carbon atoms.
Claim 3:
3. The dentifrice composition according to claim 1 or 2, wherein the anionic surfactant (B) is sodium lauryl sulfate.
Claim 4:
4. A dentifrice composition according to claim 1, 2 or 3, containing 0.01 to 0.3 mass% of component (A), 0.6 to 2.5 mass% of component (B), and 0.5 to 3 mass% of component (C).
Claim 5:
5. The dentifrice composition according to claim 1, wherein the mass ratio of (B)/(C) is 0.2 to 3.
Claim 6:
The dentifrice composition according to any one of claims 1 to 5, further comprising an abrasive.
Claim 7:
(A) isopropyl methylphenol,
(B) an anionic surfactant,
(C) A dentifrice composition containing a nonionic surfactant and filled in a container having an innermost layer made of polyethylene,
(D) Fluorine compounds: 1,100 to 3,000 ppm as fluorine
A method for inhibiting adsorption of isopropyl methylphenol to a container of a dentifrice composition, comprising:
Claim 8:
8. A method for inhibiting adsorption of isopropylmethylphenol to a container of a dentifrice composition according to claim 7, wherein the mass ratio of (B)/(C) is 0.2 to 3.
本発明によれば、イソプロピルメチルフェノールの容器吸着が抑制され、イソプロピルメチルフェノールが経時において安定化し、また、十分かつ適度な泡立ち、製剤の外観安定性が良好な歯磨組成物を提供でき、この歯磨組成物は、イソプロピルメチルフェノールを効果的に作用させてその口腔バイオフィルム浸透殺菌力を十分に発現させることが可能であり、歯周疾患の予防又は抑制用として好適に使用し得る。 According to the present invention, it is possible to provide a dentifrice composition in which isopropyl methylphenol is inhibited from being adsorbed to a container, isopropyl methylphenol is stabilized over time, and the composition foams sufficiently and appropriately, and has good stability in the appearance of the formulation. This dentifrice composition is capable of effectively acting on isopropyl methylphenol to fully express its oral biofilm penetrating bactericidal power, and can be suitably used for preventing or suppressing periodontal disease.
以下、本発明につき更に詳述する。本発明の歯磨組成物は、(A)イソプロピルメチルフェノール、(B)アニオン性界面活性剤、(C)ノニオン性界面活性剤、(D)フッ素化合物を含有する。 The present invention will be described in further detail below. The dentifrice composition of the present invention contains (A) isopropylmethylphenol, (B) anionic surfactant, (C) nonionic surfactant, and (D) a fluorine compound.
本発明において、(A)イソプロピルメチルフェノールの含有量は、組成物全体の0.01~0.3%(質量%、以下、同様。)が好ましく、より好ましくは0.02~0.1%である。配合量が多いほど殺菌効果が高まり、0.01%以上であると、十分な殺菌効果が発揮され、イソプロピルメチルフェノールの安定性を十分に確保できる。0.3%以下であることが、味を良好に確保するには好適である。 In the present invention, the content of (A) isopropyl methylphenol is preferably 0.01 to 0.3% (mass%, the same applies below) of the entire composition, and more preferably 0.02 to 0.1%. The greater the amount, the greater the bactericidal effect, and if it is 0.01% or more, a sufficient bactericidal effect is exhibited and the stability of isopropyl methylphenol can be sufficiently ensured. A content of 0.3% or less is preferable to ensure good taste.
(B)アニオン性界面活性剤としては、特に制限はされないが、例えば、ラウリル硫酸ナトリウム等のアルキル硫酸塩、ラウロイルサルコシンナトリウム等のアシルサルコシン酸塩、ラウロイルメチルタウリンナトリウム等のアシルタウリン塩、ラウロイルグルタミン酸ナトリウム等のN-アシルアミノ酸塩、α-オレフィンスルホン酸ナトリウム等のN-アシルスルホン酸塩、グリセリン脂肪酸エステルの硫酸塩などが挙げられる。これらのうち、泡立ちや味の点で、アルキル硫酸塩、アシルサルコシン酸塩、アシルタウリン塩、N-アシルアミノ酸塩、特にアルキル硫酸塩、とりわけラウリル硫酸ナトリウムが好ましい。 (B) Anionic surfactants are not particularly limited, but examples include alkyl sulfates such as sodium lauryl sulfate, acyl sarcosinates such as sodium lauroyl sarcosine, acyltaurates such as sodium lauroyl methyl taurate, N-acyl amino acid salts such as sodium lauroyl glutamate, N-acylsulfonates such as sodium α-olefin sulfonate, sulfates of glycerin fatty acid esters, etc. Among these, in terms of foaming and taste, alkyl sulfates, acyl sarcosinates, acyltaurates, N-acyl amino acid salts, particularly alkyl sulfates, and especially sodium lauryl sulfate are preferred.
(B)アニオン性界面活性剤の含有量は、組成物全体の0.6%以上、特に0.6~2.5%が好ましく、より好ましくは0.8~1.8%である。0.6%以上であると十分な泡立ちを確保できる。2.5%以下であることが、イソプロピルメチルフェノールの安定性、製剤の外観安定性を十分に確保するには好適である。 The content of (B) anionic surfactant is 0.6% or more of the total composition, preferably 0.6 to 2.5%, and more preferably 0.8 to 1.8%. A content of 0.6% or more ensures sufficient foaming. A content of 2.5% or less is suitable for ensuring sufficient stability of isopropyl methylphenol and stability of the appearance of the formulation.
(C)ノニオン性界面活性剤としては、特に制限はされないが、例えば、ポリオキシエチレン硬化ヒマシ油、ポリオキシエチレンアルキルエーテル、ショ糖脂肪酸エステル、アルキルグリコシド、ポリオキシエチレン-ポリオキシプロピレンブロック共重合体、グリセリンエステルのポリオキシエチレンエーテル、脂肪酸アルキロールアミド、グリセリン脂肪酸エステルなどが挙げられる。これらのうち、イソプロピルメチルフェノールの安定性や味の点で、エチレンオキサイドの平均付加モル数が20~100モルであるポリオキシエチレン硬化ヒマシ油、炭素数10~18のアルキル基を有し、エチレンオキサイドの平均付加モル数が5~40モルであるポリオキシエチレンアルキルエーテル、炭素数10~22の脂肪酸を有し、1つの脂肪酸をエステル化したモノエステルの割合が50%以上であるショ糖脂肪酸エステル、炭素数8~16のアルキル基を有するアルキルグリコシドが好ましく、特にエチレンオキサイドの平均付加モル数が20~100モルのポリオキシエチレン硬化ヒマシ油、炭素数10~18のアルキル基を有し、エチレンオキサイドの平均付加モル数が5~40モルのポリオキシエチレンアルキルエーテル、とりわけエチレンオキサイドの平均付加モル数が20~100モルのポリオキシエチレン硬化ヒマシ油が好ましい。 (C) Nonionic surfactants are not particularly limited, but examples include polyoxyethylene hydrogenated castor oil, polyoxyethylene alkyl ethers, sucrose fatty acid esters, alkyl glycosides, polyoxyethylene-polyoxypropylene block copolymers, polyoxyethylene ethers of glycerin esters, fatty acid alkylol amides, and glycerin fatty acid esters. Among these, in terms of the stability and taste of isopropylmethylphenol, polyoxyethylene hydrogenated castor oil with an average number of added moles of ethylene oxide of 20 to 100 moles, polyoxyethylene alkyl ether with an alkyl group having 10 to 18 carbon atoms and an average number of added moles of ethylene oxide of 5 to 40 moles, sucrose fatty acid ester with a fatty acid having 10 to 22 carbon atoms and a ratio of monoester esterified with one fatty acid of 50% or more, and alkyl glycoside with an alkyl group having 8 to 16 carbon atoms are preferred, and in particular, polyoxyethylene hydrogenated castor oil with an average number of added moles of ethylene oxide of 20 to 100 moles, polyoxyethylene alkyl ether with an alkyl group having 10 to 18 carbon atoms and an average number of added moles of ethylene oxide of 5 to 40 moles, and polyoxyethylene hydrogenated castor oil with an average number of added moles of ethylene oxide of 20 to 100 moles are preferred.
(C)ノニオン性界面活性剤の含有量は、組成物全体の0.5~3%が好ましく、より好ましくは1.0~2.5%である。0.5%以上であると、イソプロピルメチルフェノールの安定性を十分に確保できる。3%以下であることが、製剤の外観安定性を十分に確保するには好適である。 The content of (C) the nonionic surfactant is preferably 0.5 to 3% of the total composition, more preferably 1.0 to 2.5%. If it is 0.5% or more, the stability of isopropyl methylphenol can be sufficiently ensured. If it is 3% or less, it is suitable for ensuring sufficient stability of the appearance of the formulation.
更に、(B)アニオン性界面活性剤と(C)ノニオン性界面活性剤との配合割合を示す(B)/(C)が、質量比として0.2~3であることが好ましく、より好ましくは0.4~1.5である。(B)/(C)が上記範囲内であると、イソプロピルメチルフェノールの安定性向上にはより好適であり、また、製剤の外観安定性、泡立ちを十分に確保できる。0.2に満たないと泡立ち、味が劣る場合があり、3を超えるとイソプロピルメチルフェノールの安定性が劣る場合がある。 Furthermore, (B)/(C), which indicates the blending ratio of (B) the anionic surfactant and (C) the nonionic surfactant, is preferably 0.2 to 3, more preferably 0.4 to 1.5, as a mass ratio. When (B)/(C) is within the above range, it is more suitable for improving the stability of isopropyl methylphenol, and the appearance stability and foaming of the formulation can be sufficiently ensured. If it is less than 0.2, the foaming and taste may be inferior, and if it exceeds 3, the stability of isopropyl methylphenol may be inferior.
本発明では、(A)、(B)、(C)成分の組み合わせにおいて、(D)フッ素化合物が、イソプロピルメチルフェノールの安定化剤として作用する。
(D)フッ素化合物としては、例えばフッ化ナトリウム、モノフルオロリン酸ナトリウム、フッ化ストロンチウム等が挙げられ、特にフッ化ナトリウム、モノフルオロリン酸ナトリウムが好ましい。
In the present invention, in the combination of components (A), (B) and (C), the fluorine compound (D) acts as a stabilizer for isopropylmethylphenol.
(D) Examples of the fluorine compound include sodium fluoride, sodium monofluorophosphate, and strontium fluoride, with sodium fluoride and sodium monofluorophosphate being particularly preferred.
(D)フッ素化合物の含有量は、組成物全体に対して、フッ素として1,100~3,000ppmであり、好ましくは1,200~3,000ppm、より好ましくは1,400~2,500ppmである。1,100ppmに満たないと、イソプロピルメチルフェノールの安定性が劣り、安定化できない。フッ素濃度の上昇に伴ってイソプロピルメチルフェノールの安定性は向上するが、3,000ppmを超えると、製剤の外観安定性が悪くなる。
なお、上記フッ素としての含有量の範囲内において、具体的に、フッ化ナトリウムの含有量は、好ましくは組成物全体の0.25~0.66%であり、モノフルオルリン酸ナトリウムの含有量は、好ましくは組成物全体の0.84~2.27%である。
The content of the fluorine compound (D) is 1,100 to 3,000 ppm, preferably 1,200 to 3,000 ppm, more preferably 1,400 to 2,500 ppm, in terms of fluorine, relative to the entire composition. If the content is less than 1,100 ppm, the stability of isopropyl methyl phenol is poor and it cannot be stabilized. As the fluorine concentration increases, the stability of isopropyl methyl phenol improves, but if it exceeds 3,000 ppm, the appearance stability of the formulation deteriorates.
In addition, within the above-mentioned range of the fluorine content, specifically, the content of sodium fluoride is preferably 0.25 to 0.66% of the entire composition, and the content of sodium monofluorophosphate is preferably 0.84 to 2.27% of the entire composition.
本発明の歯磨組成物は、練歯磨、液状歯磨等の歯磨剤、特に練歯磨として好適に調製され、剤型に応じて、上記成分に加えてその他の公知成分を本発明の効果を妨げない範囲で配合することができる。具体的には、研磨剤、粘稠剤、粘結剤、サッカリンナトリウム等の甘味剤、パラオキシ安息香酸エステル又はその塩等の防腐剤、酸化チタン等の着色料、香料、有効成分などを配合し得る。
なお、アニオン性界面活性剤、ノニオン性界面活性剤以外の界面活性剤は配合しなくてもよいが、本発明の効果を妨げない範囲内において、カチオン性界面活性剤、両性界面活性剤を添加してもよい。
The dentifrice composition of the present invention is preferably prepared as a dentifrice such as toothpaste or liquid dentifrice, particularly toothpaste, and in addition to the above-mentioned components, other known components may be blended depending on the dosage form within the range that does not impair the effects of the present invention. Specifically, abrasives, thickening agents, binders, sweeteners such as sodium saccharin, preservatives such as paraoxybenzoic acid esters or salts thereof, colorants such as titanium oxide, flavors, active ingredients, etc. may be blended.
It is not necessary to add surfactants other than anionic surfactants and nonionic surfactants, but cationic surfactants and amphoteric surfactants may be added within the range that does not impair the effects of the present invention.
研磨剤としては、例えば、無水ケイ酸、含水ケイ酸等のシリカ系研磨剤、リン酸水素カルシウム等のリン酸カルシウム系研磨剤、炭酸カルシウム、ゼオライト、ピロリン酸カルシウム、水酸化アルミニウム、アルミナ、ハイドロキシアパタイト、炭酸マグネシウム、第3リン酸マグネシウム、ケイ酸ジルコニウム、結晶セルロース等が挙げられる。特に、使用性の点から、シリカ系研磨剤、リン酸カルシウム系研磨剤が好ましく、中でもシリカ系研磨剤の無水ケイ酸が、フッ素化合物による効果を十分に発現させる点から、より好適である。
また、無水ケイ酸として、BET比表面積が好ましくは50~400m2/g、より好ましくは80~250m2/gのものを用いると、研磨性を低減しつつ十分な清掃効果を与えることもできる。なお、上記BET比表面積は、日本工業規格(JIS8830)に基づいて測定した値である。
研磨剤の含有量は、組成物全体の5~40%好ましく、より好ましくは5~20%である。
Examples of the abrasive include silica-based abrasives such as silicic acid anhydride and silicic acid hydrate, calcium phosphate-based abrasives such as calcium hydrogen phosphate, calcium carbonate, zeolite, calcium pyrophosphate, aluminum hydroxide, alumina, hydroxyapatite, magnesium carbonate, magnesium tertiary phosphate, zirconium silicate, crystalline cellulose, etc. In particular, silica-based abrasives and calcium phosphate-based abrasives are preferred from the viewpoint of usability, and among them, silicic acid anhydride, which is a silica-based abrasive, is more suitable from the viewpoint of fully exerting the effect of the fluorine compound.
Furthermore, when a silicic anhydride having a BET specific surface area of preferably 50 to 400 m2 /g, more preferably 80 to 250 m2 /g is used, it is possible to obtain a sufficient cleaning effect while reducing abrasiveness. The BET specific surface area is a value measured based on the Japanese Industrial Standard (JIS 8830).
The content of the abrasive is preferably 5 to 40%, more preferably 5 to 20%, of the entire composition.
粘稠剤としては、ソルビット等の糖アルコール、プロピレングリコール等が挙げられる。粘稠剤の配合量は、通常、5~50%、特に20~45%である。 Thickening agents include sugar alcohols such as sorbitol, propylene glycol, etc. The amount of thickening agent is usually 5 to 50%, and particularly 20 to 45%.
粘結剤としては、ポリアクリル酸ナトリウム、アルギン酸ナトリウム等のアルギン酸誘導体、カルボキシメチルセルロースナトリウム等のセルロース系誘導体、キサンタンガム等のガム類などの有機粘結剤、無機粘結剤が挙げられる。粘結剤の配合量は、通常、0.1~5%である。 Examples of binders include organic binders such as sodium polyacrylate, alginic acid derivatives such as sodium alginate, cellulose derivatives such as sodium carboxymethylcellulose, and gums such as xanthan gum, as well as inorganic binders. The amount of binder used is usually 0.1 to 5%.
香料としては、ペパーミント油、スペアミント油、アニス油、ユーカリ油、ウィンターグリーン油、カシア油、クローブ油、タイム油、セージ油、レモン油、オレンジ油、ハッカ油、カルダモン油、コリアンダー油、マンダリン油、ライム油、ラベンダー油、ローズマリー油、ローレル油、カモミル油、キャラウェイ油、マジョラム油、ベイ油、レモングラス油、オリガナム油、パインニードル油、ネロリ油、ローズ油、ジャスミン油、グレープフルーツ油、スウィーティー油、柚油、イリスコンクリート、アブソリュートペパーミント、アブソリュートローズ、オレンジフラワー等の天然香料や、これら天然香料の加工処理(前溜部カット、後溜部カット、分留、液液抽出、エッセンス化、粉末香料化等)した香料、及び、メントール、カルボン、アネトール、シネオール、サリチル酸メチル、シンナミックアルデヒド、オイゲノール、3-l-メントキシプロパン-1,2-ジオール、チモール、リナロール、リナリールアセテート、リモネン、メントン、メンチルアセテート、N-置換-パラメンタン-3-カルボキサミド、ピネン、オクチルアルデヒド、シトラール、プレゴン、カルビールアセテート、アニスアルデヒド、エチルアセテート、エチルブチレート、アリルシクロヘキサンプロピオネート、メチルアンスラニレート、エチルメチルフェニルグリシデート、バニリン、ウンデカラクトン、ヘキサナール、ブタノール、イソアミルアルコール、ヘキセノール、ジメチルサルファイド、シクロテン、フルフラール、トリメチルピラジン、エチルラクテート、エチルチオアセテート等の単品香料、更に、ストロベリーフレーバー、アップルフレーバー、バナナフレーバー、パイナップルフレーバー、グレープフレーバー、マンゴーフレーバー、バターフレーバー、ミルクフレーバー、フルーツミックスフレーバー、トロピカルフルーツフレーバー等の調合香料等、口腔用組成物に用いられる公知の香料素材を組み合わせて使用することができるが、実施例記載の香料に限定されるものではない。
上記の香料素材は、製剤組成中に0.000001~1%使用するのが好ましく、また、上記香料素材を使用した賦香用香料は、製剤組成中に0.1~2%使用するのが好ましい。
Fragrances include peppermint oil, spearmint oil, anise oil, eucalyptus oil, wintergreen oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, lime oil, lavender oil, rosemary oil, laurel oil, chamomile oil, caraway oil, marjoram oil, bay oil, lemongrass oil, origanum oil, pine needle oil, neroli oil, rose oil, jasmine oil, grapefruit oil, and sweet ginger oil. Natural fragrances such as yuzu oil, iris concrete, absolute peppermint, absolute rose, orange flower, and processed fragrances (front distillation, back distillation, liquid-liquid extraction, essences, powdered fragrances, etc.) of these natural fragrances, as well as menthol, carvone, anethole, cineole, methyl salicylate, cinnamic aldehyde, eugenol, 3-l-menthoxypropane-1,2-diol, thymol, linalool, linalyl acetate, limonene, menthoxypropane-1,2-diol, methyl salicylate, ethyl ... [0043] The flavoring materials may be used in combination with known flavoring materials used in oral compositions, such as single flavorings such as tallow, menthyl acetate, N-substituted-paramenthan-3-carboxamide, pinene, octylaldehyde, citral, pulegone, carbyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, allyl cyclohexane propionate, methyl anthranilate, ethyl methylphenyl glycidate, vanillin, undecalactone, hexanal, butanol, isoamyl alcohol, hexenol, dimethyl sulfide, cyclotene, furfural, trimethylpyrazine, ethyl lactate, and ethyl thioacetate, as well as blended flavors such as strawberry flavor, apple flavor, banana flavor, pineapple flavor, grape flavor, mango flavor, butter flavor, milk flavor, fruit mix flavor, and tropical fruit flavor, but are not limited to the flavors described in the examples.
The above-mentioned flavor materials are preferably used in an amount of 0.000001 to 1% in the formulation, and flavorings using the above-mentioned flavor materials are preferably used in an amount of 0.1 to 2% in the formulation.
有効成分としては、イソプロピルメチルフェノール、フッ素化合物以外の口腔用として公知の薬効成分、具体的にはカチオン性殺菌剤、抗炎症剤、酵素、植物抽出物、歯石防止剤、歯垢防止剤などを、本発明の効果を妨げない範囲で有効量配合することができる。 Active ingredients include isopropylmethylphenol, fluorine compounds, and other known oral medicinal ingredients, specifically cationic bactericides, anti-inflammatory agents, enzymes, plant extracts, anti-tartar agents, and anti-plaque agents, which can be blended in effective amounts within a range that does not interfere with the effects of the present invention.
本発明の歯磨組成物は、最内層がポリエチレンからなるチューブ容器に好適に充填される。
かかる容器としては、例えば、外層から低密度ポリエチレン/エチレン・アクリル酸共重合体樹脂/アルミニウム/エチレン・アクリル酸共重合体樹脂/直鎖状低密度ポリエチレン(最内層)、低密度ポリエチレン/エチレン・ビニルアルコールの共重合体/低密度ポリエチレン/エチレン・ビニルアルコールの共重合体/直鎖状低密度ポリエチレン(最内層)、及び低密度ポリエチレン/ポリエチレンテレフタレート/低密度ポリエチレン/ガラス蒸着ポリエチレンテレフタレート/エチレン・メタクリル酸共重合体樹脂/直鎖状低密度ポリエチレン(最内層)などからなるラミネート層構造を有するものが挙げられるが、最内層がポリエチレンであれば他の層構成はいずれでも良く、特に最内層が直鎖状低密度ポリエチレンであるものが好ましい。
The dentifrice composition of the present invention is suitably packed in a tube container whose innermost layer is made of polyethylene.
Examples of such containers include those having a laminate layer structure consisting of, from the outer layer, low-density polyethylene/ethylene-acrylic acid copolymer resin/aluminum/ethylene-acrylic acid copolymer resin/linear low-density polyethylene (innermost layer), low-density polyethylene/ethylene-vinyl alcohol copolymer/low-density polyethylene/ethylene-vinyl alcohol copolymer/linear low-density polyethylene (innermost layer), and low-density polyethylene/polyethylene terephthalate/low-density polyethylene/glass-deposited polyethylene terephthalate/ethylene-methacrylic acid copolymer resin/linear low-density polyethylene (innermost layer). As long as the innermost layer is polyethylene, the other layer configurations may be any, and it is particularly preferable that the innermost layer is linear low-density polyethylene.
なお、直鎖状低密度ポリエチレンはリニア低密度ポリエチレンともいい、製法としては、高密度ポリエチレン製造工程において、直鎖状ポリマーにα-オレフィン(例えば、ブテン-1、ヘキセン-1、4-メチルペンテン、オクテン-1)を共重合させ、短鎖分岐を導入して低密度化したものであり、押出コーティング用の直鎖状低密度ポリエチレンは、密度0.915~0.938g/cm3のものが一般的に使用される。
最内層のポリエチレンの厚さとしては、特に規定されないが、通常30~100μm程度の厚さを有し、ラミネート層全体では200~450μmの厚さのものが通常用いられる。
上記チューブ容器では、特に内容物吐出口、胴部をつなぐ肩部、とりわけ肩部に、内容物中の配合成分が吸着し易いが、本発明においては、上記各部の最内層がポリエチレンであっても、イソプロピルメチルフェノールの吸着が抑制され安定性が優れる。
Linear low-density polyethylene is also called linear low-density polyethylene, and is produced by copolymerizing an α-olefin (e.g., butene-1, hexene-1, 4-methylpentene, octene-1) with a linear polymer in the high-density polyethylene production process to introduce short chain branches and reduce the density. Linear low-density polyethylene for extrusion coating generally has a density of 0.915 to 0.938 g/ cm3 .
The thickness of the innermost polyethylene layer is not particularly limited, but is usually about 30 to 100 μm, and the total thickness of the laminate layer is usually 200 to 450 μm.
In the above-mentioned tube container, the ingredients in the contents are easily adsorbed, particularly to the contents discharge port and the shoulder connecting the body, especially to the shoulder. However, in the present invention, even if the innermost layer of each of the above-mentioned parts is polyethylene, adsorption of isopropyl methylphenol is suppressed, and the stability is excellent.
このような最内層がポリエチレンからなるチューブ容器は、市販のものを使用でき、例えば、歯磨チューブとして大日本印刷(株)、凸版印刷(株)などの容器包材メーカーから入手することができる。 Such tube containers with an innermost layer made of polyethylene can be commercially available. For example, toothpaste tubes can be obtained from container and packaging manufacturers such as Dai Nippon Printing Co., Ltd. and Toppan Printing Co., Ltd.
以下、実施例及び比較例を示し、本発明を具体的に説明するが、本発明は下記の実施例に制限されるものではない。なお、下記において、%は特に断らない限りいずれも質量%を示す。実施例5及び10は参考例である。 The present invention will be specifically described below with reference to examples and comparative examples, but the present invention is not limited to the following examples. In the following, % means mass % unless otherwise specified. Examples 5 and 10 are reference examples.
[実施例、比較例]
表1~3に示す組成の歯磨組成物を常法によって調製し、下記に示すようにチューブ容器に充填し、これを試験歯磨組成物として、下記方法で評価した。結果を表1~3に併記した。
[Examples and Comparative Examples]
Dentifrice compositions having the compositions shown in Tables 1 to 3 were prepared by a conventional method and filled into tube containers as described below. These test dentifrice compositions were evaluated by the following methods. The results are shown in Tables 1 to 3.
試験歯磨組成物の調製
歯磨組成物を、最内層が直鎖状低密度ポリエチレンからなる直径26mmのラミネートチューブ(LDPE55/PET12/LDPE20/白LDPE60/EMAA20/AL10/EMAA30/LDPE20/LLDPE30,厚み257μm(大日本印刷(株)製))に60g充填した。
なお、使用したラミネートチューブの層構成における略号と名称は以下の通りであり、略号に続く数字は各層の厚み(μm)を示したものである。
LDPE:低密度ポリエチレン
白LDPE:白色低密度ポリエチレン
LLDPE:直鎖状低密度ポリエチレン
AL:アルミニウム
EAA:エチレン・アクリル酸の共重合体樹脂
PET:ポリエチレンテレフタレート
EMAA:エチレン・メタクリル酸の共重合体樹脂
SiOx-PET:ガラス蒸着ポリエチレンテレフタレート
Preparation of test dentifrice compositions 60 g of each dentifrice composition was packed into a laminate tube having a diameter of 26 mm and an innermost layer made of linear low-density polyethylene (LDPE55/PET12/LDPE20/white LDPE60/EMAA20/AL10/EMAA30/LDPE20/LLDPE30, thickness 257 μm (manufactured by Dai Nippon Printing Co., Ltd.)).
The abbreviations and names of the layer structures of the laminate tubes used are as follows, and the numbers following the abbreviations indicate the thickness (μm) of each layer.
LDPE: White low-density polyethylene LDPE: White low-density polyethylene LLDPE: Linear low-density polyethylene AL: Aluminum EAA: Ethylene-acrylic acid copolymer resin PET: Polyethylene terephthalate EMAA: Ethylene-methacrylic acid copolymer resin SiOx-PET: Glass-deposited polyethylene terephthalate
(1)イソプロピルメチルフェノールの安定性の評価方法
60℃で1ヶ月保存後の歯磨組成物について、下記試験条件に従いHPLCを用いてイソプロピルメチルフェノール量を測定した。各サンプルの製造直後のイソプロピルメチルフェノール量を100%とした際の残存率を算出し、下記の判定基準に従ってイソプロピルメチルフェノールの安定性を判定し、IPMP安定性として表に示した。
試験条件;
・検出器:紫外吸光光度計(測定波長:285nm)
・カラム:YMC-Pack ODS-A A-303(4.6mmφ×250mm)
・カラム温度:45℃
・移動相:アセトニトリル/水/酢酸混液(60:40:1)
使用機器;
・ポンプ:日本分光(株)、PU-980
・試料導入部:日本分光(株)、AS-950
・検出器:日本分光(株)、UV-970
・カラム恒温槽:日本分光(株)、CO-960
・流量:1mL/min
判定基準;
◎:97%以上100%以下
○:94%以上97%未満
△:90%以上94%未満
×:90%未満
(1) Method for evaluating the stability of isopropyl methylphenol The amount of isopropyl methylphenol in the dentifrice composition after storage at 60° C. for one month was measured using HPLC under the following test conditions. The remaining rate was calculated when the amount of isopropyl methylphenol immediately after the preparation of each sample was taken as 100%, and the stability of isopropyl methylphenol was evaluated according to the following evaluation criteria, and shown in the table as IPMP stability.
Test condition;
Detector: ultraviolet spectrophotometer (measurement wavelength: 285 nm)
Column: YMC-Pack ODS-A A-303 (4.6 mmφ×250 mm)
Column temperature: 45°C
Mobile phase: Acetonitrile/water/acetic acid mixture (60:40:1)
Used equipment;
Pump: JASCO Corporation, PU-980
Sample introduction section: JASCO Corporation, AS-950
Detector: JASCO Corporation, UV-970
Column thermostat: JASCO Corporation, CO-960
Flow rate: 1 mL/min
Judgment criteria;
◎: 97% or more and 100% or less ○: 94% or more and less than 97% △: 90% or more and less than 94% ×: Less than 90%
(2)製剤の外観安定性の評価方法
60℃で1ヶ月保存後の歯磨組成物をわら半紙上に約15cm吐出させた。わら半紙の裏に染み込んだ水分の長さから、下記の判定基準に従って液分離安定性を評価した。
判定基準
◎:0.2cm未満
○:0.2cm以上0.5cm未満
×:0.5cm以上
(2) Evaluation method for appearance stability of preparations Dentifrice compositions stored at 60° C. for one month were ejected onto a piece of straw paper to a depth of about 15 cm. Liquid separation stability was evaluated based on the length of water that had soaked into the back of the straw paper, according to the following criteria.
Criteria: ◎: Less than 0.2 cm ○: 0.2 cm or more but less than 0.5 cm ×: 0.5 cm or more
(3)泡立ちの評価方法
歯磨組成物を歯ブラシに載せ、口腔内を洗浄した際の泡立ちを、5名の被験者が下記の評点基準によって評価した。5名の評価点を平均し、下記の判定基準に従って泡立ちを評価した。
評点基準;
5点:泡立ちが良い
4点:やや泡立ちが良い
3点:どちらともいえない
2点:やや泡立ちが悪い
1点:泡立ちが悪い
判定基準;
◎:平均点4.0点以上
○:平均点3.0点以上4.0点未満
△:平均点2.0点以上3.0点未満
×:平均点2.0点未満
(3) Method for evaluating foaming The dentifrice composition was applied to a toothbrush and the foaming generated when the oral cavity was cleaned was evaluated by five subjects according to the following rating scale. The scores of the five subjects were averaged and the foaming was evaluated according to the following judging scale.
Scoring criteria:
5 points: good foaming; 4 points: some foaming; 3 points: neither good nor bad; 2 points: some poor foaming; 1 point: poor foaming. Evaluation criteria:
◎: Average score of 4.0 points or more ○: Average score of 3.0 points or more and less than 4.0 points △: Average score of 2.0 points or more and less than 3.0 points ×: Average score of less than 2.0 points
表1~3の結果から明らかなように、比較例に示すように(A)成分と共に(B)、(C)成分を配合すると、IPMP安定性が悪くなり、(D)成分を添加してもその配合量又は(B)/(C)比が不適切であるとIPMP安定性が劣るが、(A)、(B)、(C)成分に(D)成分を適切量かつ適切な(B)/(C)比の範囲内で組み合わせて配合した本発明の歯磨組成物(実施例)は、IPMP安定性、製剤の外観安定性及び泡立ちが優れた。また、歯磨き後の味も良好であった。 As is clear from the results in Tables 1 to 3, when component (A) is mixed with components (B) and (C), as shown in the comparative examples, IPMP stability is poor, and even if component (D) is added, the IPMP stability is poor if the amount of component (D) or the (B)/(C) ratio is inappropriate. However, the dentifrice composition of the present invention (Example) in which component (A), (B), and (C) are combined with component (D) in an appropriate amount and within an appropriate (B)/(C) ratio range, exhibited excellent IPMP stability, formulation appearance stability, and foaming. In addition, the taste after brushing was also good.
Claims (11)
(B)アニオン性界面活性剤、
(C)エチレンオキサイドの平均付加モル数20~100のポリオキシエチレン硬化ヒマシ油を配合し、(B)/(C)が質量比として0.4~1.3であり、最内層が直鎖状低密度ポリエチレンからなる容器に充填した歯磨組成物に、
(D)フッ素化合物をフッ素として1,400~2,500ppm
配合したことを特徴とする歯磨組成物。 (A) isopropyl methylphenol,
(B) an anionic surfactant,
(C) polyoxyethylene hydrogenated castor oil having an average added mole number of ethylene oxide of 20 to 100 is blended, (B)/(C) is a mass ratio of 0.4 to 1.3, and the dentifrice composition is filled in a container having an innermost layer made of linear low-density polyethylene,
(D) Fluorine compounds: 1,400 to 2,500 ppm as fluorine
A dentifrice composition comprising:
(B)アニオン性界面活性剤、
(C)エチレンオキサイドの平均付加モル数20~100のポリオキシエチレン硬化ヒマシ油
を配合し、(B)/(C)が質量比として0.4~1.3であり、最内層が直鎖状低密度ポリエチレンからなる容器に充填した歯磨組成物に、
(D)フッ素化合物をフッ素として1,400~2,500ppm
配合することを特徴とする、前記歯磨組成物における容器へのイソプロピルメチルフェノールの吸着抑制方法。 (A) isopropyl methylphenol,
(B) an anionic surfactant,
(C) polyoxyethylene hydrogenated castor oil having an average added mole number of ethylene oxide of 20 to 100 is blended, (B)/(C) is a mass ratio of 0.4 to 1.3, and the dentifrice composition is filled in a container having an innermost layer made of linear low-density polyethylene,
(D) Fluorine compounds: 1,400 to 2,500 ppm as fluorine
A method for inhibiting adsorption of isopropyl methylphenol to a container of a dentifrice composition, comprising:
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