TWI395745B - Catechu acid coloring inhibition method and toothpaste composition - Google Patents
Catechu acid coloring inhibition method and toothpaste composition Download PDFInfo
- Publication number
- TWI395745B TWI395745B TW096126176A TW96126176A TWI395745B TW I395745 B TWI395745 B TW I395745B TW 096126176 A TW096126176 A TW 096126176A TW 96126176 A TW96126176 A TW 96126176A TW I395745 B TWI395745 B TW I395745B
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- Prior art keywords
- catechin
- hydrogel particles
- water
- catechins
- hydrogel
- Prior art date
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Description
本發明係關於一種兒茶酸類著色抑制方法、以及含有兒茶酸類的水不溶性複合物之水凝膠粒子。又關於一種包含兒茶酸類之牙膏組合物。
已知兒茶酸或單寧酸等係茶葉中所含之多酚類。尤其,已知兒茶酸類具有抗氧化作用、抗菌作用、抑制血中膽固醇濃度作用、抑制血壓上升作用、抑制血糖上升作用等各種生理機能,但其本身為強力抗氧化物質,故而存在會於保存期間引起氧化、聚合之問題。進而,由於若兒茶酸類產生氧化及/或聚合則會引起變色之問題,故將兒茶酸類使用於製劑之自由度受到限制。因此,業者正謀求抑制兒茶酸類氧化或聚合之方法。
於JP-A 9-47654中,因若多酚類於製品中過量存在則會損壞商品價值,故其係以去除多酚類為目的,與抑制兒茶酸類的氧化或聚合之方法不同。
於JP-A 8-333380中揭示有一種茶葉皂素之製造方法:將以含水低級醇對茶葉的熱水萃取殘渣進行萃取之萃取液,以水不溶性聚乙烯吡咯烷酮進行處理,而去除該萃取液中存在之兒茶酸類。
於JP-A 1-218550中,揭示有一種包含下列步驟之除單寧酸茶液之製造方法:以溫水等對經厭氧處理的茶葉進行萃取,於經過濾的萃取液中添加不溶性聚乙烯吡咯烷酮後再進行過濾。
已知蛀牙或牙周病係由口腔內細菌引起。因此,為了預防蛀牙或牙周病,一般而言於口腔用組合物中調配殺菌劑,對口腔內細菌進行殺菌或者抑制其活性。特別是近年來追求天然傾向一直在提高,因而作為殺菌劑則避免使用化學合成物質而使用來自天然物的成分。例如,已知綠茶萃取物以及其成分之茶多酚化合物(兒茶酸類等)可有效抑制口腔內細菌的增殖(例如,JP-A 1-90124、JP-A 2-25413、JP-A 3-86814等)。根據該等文獻,記載有因綠茶萃取物等抑制蛀牙病原菌之轉糖鏈球菌(Sterptococcus mutans)或牙周病病原菌之牙齦卟啉單胞菌(Porphyromonas gingivalis)的增殖,故可提供一種有效預防蛀牙、牙周病之口腔用組合物。然而,多酚化合物(兒茶酸類等)因與氧接觸而引起氧化、聚合,而顯著變色,因此無法避免調配多酚化合物之口腔用組合物自身的經時變色。作為抑制該等之變色之方法,例如提出有於含多酚之植物萃取物中調配入碳數4~5的糖醇(例如木糖醇、赤蘚糖醇等)且分裝密封於不透氧性的單個袋中之方法(JP-A 2000-297022)。
另一方面,作為將各種藥劑、易變性的有效成分等調配入口腔用組合物中之方法,亦提出有將該成分膠囊化或內包於外殼等中而使其穩定化之方法(JP-A 61-225115、JP-A 1-275520等)。
本發明提供一種兒茶酸類著色抑制方法,其係於兒茶酸類中添加與兒茶酸類形成水不溶性複合物之水溶性聚合物(以下稱為聚合物A)。
又,本發明提供一種水凝膠粒子,其含有兒茶酸類與聚合物A所形成之水不溶性複合物。
本發明提供一種牙膏組合物,其含有:含有兒茶酸類以及與兒茶酸類形成水不溶性複合物的水溶性聚合物之水凝膠粒子、黏結劑、以及水。
本發明提供一種與兒茶酸類形成水不溶性複合物的水溶性聚合物之抑制兒茶酸類著色之用途。進而,本發明提供一種含有水凝膠粒子、黏結劑、以及水之組合物之牙膏用途,其中該水凝膠粒子包含兒茶酸類以及與兒茶酸類形成水不溶性複合物之水溶性聚合物。
於JP-A 9-47654中,揭示有一種由使再生纖維素物質的基材中含有不溶性聚乙烯吡咯烷酮的複合材料所構成之多酚吸附劑。
JP-A 8-333380係以去除目標物質皂素以外的無用物質即兒茶酸類等為目的,與抑制兒茶酸類的氧化或聚合之方法不同。
於JP-A1-218550係以去除萃取液中的單寧酸成分為目的,與抑制兒茶酸類的氧化或聚合之方法不同。
於先前技術中,已知有使兒茶酸類吸附於聚乙烯吡咯烷酮上而吸附除去兒茶酸類之技術,但未知抑制兒茶酸類的氧化及/或聚合而防止變色之方法。
本發明提供一種抑制兒茶酸類的著色而防止變色之方法、以及抑制兒茶酸類著色之水凝膠粒子。
本發明者們發現,利用使牙膏組合物中含有將兒茶酸類及與兒茶酸類形成水不溶性複合物的特定聚合物加以內包之水凝膠粒子,而獲得一種可穩定地保持兒茶酸類,並且藉由輕觸而使凝膠狀粒子容易地破壞從而使兒茶酸類有效作用於牙齒或牙齦表面附近,且使用感良好之牙膏組合物。
本發明提供一種使兒茶酸類穩定地保持於組合物中,並且於使用時兒茶酸類有效地作用於牙齒、牙齦,且使用感良好之牙膏組合物。
根據本發明,兒茶酸類與聚合物A形成水不溶性複合物而使兒茶酸類穩定化,藉此可抑制兒茶酸類之著色。
本發明之牙膏劑可穩定地保持兒茶酸類,且有效作用於牙齒或牙齦表面附近,從而可改善牙齒或牙齦的狀態,且使用感良好。
於本發明中,兒茶酸類為非聚合性兒茶酸類,例如可舉出:兒茶酸、沒食子兒茶酸、兒茶酸沒食子酸酯、沒食子兒茶酸沒食子酸酯等非表體兒茶酸類;表兒茶酸、表沒食子兒茶酸、表兒茶酸沒食子酸酯、表沒食子兒茶酸沒食子酸酯等表體兒茶酸類等。兒茶酸類,可藉由將利用熱水或水溶性有機溶劑自茶葉中萃取的綠茶萃取物進行濃縮、純化等而獲得。又,可藉由使用市售之三井農林(股)「多酚,Polyphenone」、伊藤園(股)「泰阿呋蘭,Thea-Flan」、太陽化學(股)「三苯酚,Sunphenone」等綠茶萃取物的濃縮物進行成分調整,而獲得適於本發明目的之綠茶萃取物。
作為本發明所使用之聚合物A,只要可與兒茶酸類形成水不溶性複合物之水溶性聚合物,則無特別限定。
再者,所謂水不溶性複合物,係指將兒茶酸類水溶液與聚合物A的水溶液混合時,作為不溶物自水中析出之物質。水不溶性複合物之析出,可根據混合液的渾濁、或者以雷射繞射/散射式粒度分布測定裝置對混合液進行測定時存在有由水不溶性複合物產生的峰而確認。
至於聚合物A,可舉出:聚乙烯吡咯烷酮、聚乙烯醇、羥乙基纖維素等,較好的是聚乙烯吡咯烷酮(以下亦略記為PVP)。
就有效抑制兒茶酸類著色之觀點而言,聚合物A之重量平均分子量,較好的是6000以上,更好的是60000以上,更好的是400000以上,尤其好的是1300000以上。又,就抑制水不溶性複合物成為塊狀凝集物且獲得微細的水不溶性複合物之觀點而言,較好的是3000000以下,更好的是2000000以下。
於本發明中,聚合物A之重量平均分子量,係利用一般的重量平均分子量測定法即光散射法等所測定之值。
於本發明之方法中,就有效抑制兒茶酸類著色之觀點而言,聚合物A之添加量,較好的是相對於兒茶酸類為1~4倍重量,更好的是1~3倍重量,更好的是1.2~2.2倍重量。
於本發明中,可藉由於兒茶酸類水溶液等中添加聚合物A的水溶液等,以攪拌機等進行混合,而形成水不溶性複合物,從而抑制兒茶酸類著色。
本發明之水凝膠粒子含有兒茶酸類與聚合物A所形成之水不溶性複合物。
本說明書中所謂「水凝膠」,係指以水為溶劑而形成之不溶於水的高分子(凝膠形成劑)含水膨潤體。至於凝膠形成劑,較好的是天然系高分子化合物,例如可舉出:瓊脂、-角叉菜膠、ι-角叉菜膠、λ-角叉菜膠、角叉藻膠(furcellaran)、海藻酸鹽、海藻酸丙二醇酯等海藻萃取物;瓜爾豆膠、刺槐豆膠、羅望子種子多糖類、塔拉膠(tara gum)、苦木膠等植物種子黏性物質;果膠、阿拉伯半乳糖等植物果實黏性物質;三仙膠、硬葡聚糖(scleroglucan)、普魯蘭多糖、葡聚糖(dextran)、結蘭膠(gellan gum)、卡特蘭多糖(curdlan)等微生物產生黏性物質;明膠、白蛋白、酪蛋白等動物蛋白質;大豆蛋白質、小麥蛋白質等植物蛋白質;羧甲基纖維素、甲基纖維素、微結晶纖維素等纖維素及其衍生物;澱粉、澱粉磷酸酯、澱粉乙醇酸酯等澱粉及其衍生物,該等可單獨使用或將2種以上混合使用。作為形成易物理性崩解的脆凝膠粒子之高分子,較好的是-角叉菜膠、瓊脂、結蘭膠。
再者,瓊脂溶解於水之溫度,一般為75℃以上,主要為75~90℃,將瓊脂溶解於水後進行冷卻時之凝膠化溫度為30~45℃。
於本發明之水凝膠粒子中,將兒茶酸類與聚合物A形成之水不溶性複合物分散內包於包含凝膠形成劑及水之連續相中。就有效抑制兒茶酸類著色之觀點而言,水不溶性複合物中聚合物A相對於兒茶酸類之比例,較好的是1~4倍重量,更好的是1~3倍重量,更好的是1.2~2.2倍重量。
就抑制水不溶性複合物形成塊狀凝集物且獲得微細的水不溶性複合物之觀點而言,本發明之水凝膠粒子中兒茶酸類與聚合物A形成之水不溶性複合物的含量,較好的是12重量%以下,更好的是8重量%以下,更好的是6重量%以下。
就防止水凝膠粒子調配於其他劑中時產生破壞之觀點而言,本發明之水凝膠粒子中凝膠形成劑之含量,較好的是0.25~5.0重量%,更好的是0.5~4.0重量%,更好的是1.0~3.0重量%。
本發明之水凝膠粒子,除本發明之水不溶性複合物、凝膠形成劑及水以外,亦可含有糖類、多元醇等水溶性有機化合物,或者著色劑、防腐劑、水溶性香料等成分。
至於糖類,可舉出:葡萄糖、半乳糖、果糖、甘露糖、甘露醇、蔗糖、麥芽糖、乳糖等。
至於多元醇,可舉出:丙三醇、山梨糖醇、乙二醇、聚乙二醇、丙二醇、聚丙二醇、寡糖等。
就外觀及生產性之觀點而言,本發明之水凝膠粒子之平均粒徑,較好的是5~10000 μm,更好的是100~10000 μm,尤其好的是200~5000 μm。水凝膠粒子之平均粒徑,係使用各種篩孔的篩,將100 g粒子於水中進行濕式分級,再以濾紙去除多餘的水分,然後測定重量且以重量平均粒徑來表示(篩法)。
又,對本發明之水凝膠粒子之形狀並無特別限定,較好的是具有以曲面而構成之旋轉體形狀。此處,所謂「以曲面而構成之旋轉體」,係指以假想軸使以假想軸及連續曲線而構成之封閉圖旋轉者,並不包含具有三角錐或圓柱等平面之形狀。就美觀之觀點而言,水凝膠粒子的形狀較好的是球狀或橢圓狀。
對本發明之水凝膠粒子之製造法並無特別限定,例如,將瓊脂等凝膠形成劑及聚合物A與離子交換水加以混合,加熱至其溶解溫度以上的溫度使其充分溶解。此處,添加兒茶酸類水溶液且加以混合後,可利用一般的滴加法、噴霧法、或者攪拌法等獲得水凝膠粒子。
滴加法,係將混合液自孔中吐出,利用被吐出的混合液經由其表面張力或界面張力而成為液滴之性質,使其液滴於空氣等氣相中或者液相中冷卻固化而製造水凝膠粒子之方法。再者,就製造粒徑均勻的水凝膠粒子之觀點而言,較好的是對自孔中吐出的混合液施加振動。
噴霧法,係使用噴霧噴嘴,自噴霧噴嘴中將混合液噴霧成氣相,同時藉由其表面張力形成液滴,使該液滴於氣相中冷卻固化而製造水凝膠粒子之方法。
攪拌法,係於具有未與混合液實質混合的性狀且調整為凝膠化溫度以上溫度的液中投入混合液,藉由攪拌所產生的切斷力使混合液微粒化,藉由界面張力使之成為液滴,利用此性質使該液滴於未與混合液實質混合的液中冷卻固化而製造水凝膠粒子之方法。
於滴加法、噴霧法及攪拌法之任一情形時,較好的是,將吐出時、噴霧時或投入時的混合液溫度設為凝膠化溫度以上且100℃以下之溫度。又,就可容易地製造美觀的球狀粒子之觀點而言,較好的是將該水包油型分散液之溫度設為凝膠化溫度+10℃以上,更好的是設為凝膠化溫度+20℃以上。再者,該溫度之上限為水的沸點即100℃。
本發明之水凝膠可調配入化粧料、清洗劑、浴劑等中。又,可調配入口腔用組合物,尤其是牙膏組合物中。
本發明之牙膏組合物中所含之水凝膠粒子,係含有上述兒茶酸類、及與上述兒茶酸類形成水不溶性複合物之水溶性聚合物(以下亦稱為聚合物A)者。
於本說明書中,所謂「水凝膠」係指以水為溶劑而形成之不溶於水之高分子(凝膠形成劑)含水膨潤體;至於凝膠形成劑,較好的是天然系高分子化合物。
就兒茶酸對牙齦充分起作用及水凝膠粒子的穩定性之觀點考慮,本發明之水凝膠粒子中兒茶酸類之含量,較好的是0.001~10質量%,更好的是0.001~6質量%,更好的是0.01~2質量%。又,就有效抑制兒茶酸類著色之觀點而言,聚合物A之含量相對於兒茶酸類而言,較好的是1~4倍質量,更好的是1~3倍質量,更好的是1.2~2.2倍質量。
又,就抑制水不溶性複合物形成塊狀凝集物且獲得微細的水不溶性複合物之觀點而言,水凝膠粒子中所含水不溶性複合物之含量,較好的是12質量%以下,更好的是8質量%以下,更好的是6質量%以下。
於本發明中,水凝膠粒子中所使用之凝膠形成劑係如上所述。
就防止將水凝膠粒子調配入牙膏組合物中時產生破壞之觀點而言,本發明之水凝膠粒子中凝膠形成劑之含量係如上所述。
本發明之水凝膠粒子,除兒茶酸類、聚合物A、凝膠形成劑以及水以外,如上所述,亦可含有糖類、多元醇等水溶性有機化合物,或者著色劑、防腐劑、水溶性香料等成分。
本發明之水凝膠粒子之製造法係如上所述。
本發明之牙膏組合物含有如上述之水凝膠粒子、黏結劑以及水。
至於本發明所使用之黏結劑,例如可舉出:海藻酸鈉、羧甲基纖維素鈉、角叉菜膠、三仙膠、聚丙烯酸鈉、羥乙基纖維素、羥丙基纖維素、果膠、黃蓍膠、阿拉伯膠、瓜爾膠、刺梧桐樹膠、刺槐豆膠、結蘭膠、羅望子膠、洋車前子膠、聚乙烯醇、軟骨素硫酸鈉以及甲氧基乙烯-馬來酸酐共聚物等,尤其好的是海藻酸鈉、羧甲基纖維素鈉、角叉菜膠以及三仙膠。
上述黏結劑中,作為海藻酸鈉,較好的是由Kimica(股)、大日本製藥等市售可容易獲取之分子內甘露糖醛酸(mannuronic acid)/古洛糖醛酸(guluronic acid)(M/G比)為0.5~2.5者。羧甲基纖維素鈉,較好的是由Daicel化學、第一工業製藥等市售可容易獲取之醚化度為0.6~2.5者,更好的是醚化度為0.8~1.5者。角叉菜膠,可使用型、λ型、ι型3種異構體中之任一者,可使用由Kelco、MRC多醣、太陽化學等市售可容易獲取者,更好的是ι型、λ型。三仙膠,可使用由太陽化學、Kelco、大日本製藥等市售可容易獲取者;於將三仙膠與羧甲基纖維素併用之情形時,較好的是使用去除三仙膠中少量混入的纖維素酶之纖維素酶活性較低之三仙膠。
黏結劑,可使用1種或者將2種以上組合使用,就保存穩定性、組合物的黏性、獲得較高清涼感之觀點而言,組合物中之黏結劑之含量,較好的是0.1~3質量%,更好的是0.1~2質量%,更好的是0.2~1.2質量%。
就牙膏組合物的穩定性之觀點而言,本發明之牙膏組合物中之水凝膠粒子之含量,較好的是0.01~15質量%,更好的是0.1~10質量%,更好的是1~5質量%。
就保存穩定性、獲得較高清涼感之觀點而言,本發明之牙膏組合物中之水分量,較好的是1~50質量%,更好的是5~40質量%,更好的是10~30質量%。
就清涼感、冰涼感及味道之觀點而言,本發明之牙膏組合物中可進而調配入粒徑小於355 μm之粉末或者粒子狀赤蘚糖醇。至於赤蘚糖醇之結構,存在L-赤蘚糖醇、D-赤蘚糖醇、內消旋-赤蘚糖醇之3種異構體,本發明亦可使用該等中之任一種結構。至於赤蘚糖醇,可使用通常可獲取者,例如可舉出:將葡萄糖醱酵後進行再結晶而獲得之結晶狀赤蘚糖醇等。結晶狀赤蘚糖醇,作為市售品,可獲得日研化學(股)、三菱化學食品(股)、Celestar公司製等。又,粒徑較大者,亦可使用將其粉碎而調整粒徑者。赤蘚糖醇之粉碎,一般係使用輥磨機、錘碎機、高速粉碎機、粉碎機等,較好的是使用粒度調整為簡便且生產效率亦優異之高速粉碎機、錘磨機進行粉碎。
就於口腔內使冰涼感長期持續之觀點而言,赤蘚糖醇之粒徑,較好的是45 μm以上小於355 μm,更好的是53 μm以上小於300 μm,更好的是75 μm以上小於250 μm。赤蘚糖醇之粒徑為45 μm以上者,在口中不會瞬時溶化,冰涼感長期持續,故較好。又,小於355 μm者易在口腔內溶化可發揮冰涼感。
再者,赤蘚糖醇之粒徑係以如下之方式進行測定。
篩:JIS標準篩75 mm
篩孔:自上段開始,分別於具有500 μm、355 μm、250 μm、180 μm、125 μm、90 μm及45 μm孔徑之篩下有接受器。
振盪機:微型電磁振動機M-2型(筒井理化學器機(股))
方法:將15 g試料放置於500 μm篩上,以電磁振動機進行5分鐘分級。將於具有250 μm、180 μm、125 μm、90 μm及45 μm孔徑的篩上所存在的赤蘚糖醇之合計量作為粒徑45 μm以上小於355 μm之赤蘚糖醇。
就清涼感及冰涼感之觀點而言,本發明之牙膏組合物中之赤蘚糖醇之調配量,較好的是15~60質量%,更好的是20~55質量%,更好的是25~50質量%,尤其好的是30~50質量%。
較理想的是,將赤蘚糖醇以粉末狀態分散於牙膏組合物中。因此,較好的是,於製造的最終步驟,直接以粉體投入赤蘚糖醇。可藉由使用如此方法,而使赤蘚糖醇在幾乎不溶解於水的情況下以粉末狀態存在於牙膏組合物中。
本發明之牙膏組合物可進一步含有研磨劑。至於研磨劑,除沈降性二氧化矽、二氧化矽凝膠、鋁矽酸鹽、鋯矽酸鹽、葡萄糖矽酸鹽等二氧化矽以外,可舉出:碳酸鈣、磷酸氫鈣、焦磷酸鈣、氫氧化鋁、氧化鋁、碳酸鎂、磷酸鎂等。研磨劑之含量,於本發明之牙膏組合物中,較好的是0~15質量%,尤其好的是0~12質量%。
於本發明之牙膏組合物中,在不妨礙本發明目的的範圍內,可適當調配入可使用於口腔用組合物之其他調配成分,例如抗氧化劑、濕潤劑、藥效成分、發泡劑、保存劑、香料、甜味劑、pH調整劑等。
至於抗氧化劑,可舉出:具有抗氧化能力或還原能力且可使用於口腔內組合物之成分,例如:L-抗壞血酸及其鹽、異抗壞血酸及其鹽、α-生育醇醋酸鹽、dl-α-生育醇、迷迭香萃取物、甜菊萃取物、葵花籽萃取物、沒食子酸丙酯、二丁基羥基甲苯、羥基茴香丁酯、L-半胱胺酸鹽酸鹽、植酸、對苯二酚及其配糖體、正二氫癒創酸、抗壞血酸高級脂肪酸酯(十二烷酸酯、硬脂酸酯、異硬脂酸酯、棕櫚酸酯等)、癒瘡木脂等。至於L-抗壞血酸、異抗壞血酸或者醋酸α-生育醇之鹽,可舉出:鈉鹽、鈣鹽、亞鐵鹽、棕櫚酸酯之鹽等。該等抗氧化劑,可單獨使用,亦可選擇2種以上使用。就抑制外觀顏色變化之效果而言,抗氧化劑於本發明之牙膏組合物中之含量,較好的是0.0005~50質量%,更好的是0.001~20質量%,尤其好的是0.01~5質量%。
至於濕潤劑,例如可舉出:丙三醇、山梨糖醇、聚乙二醇、丙二醇、乙二醇、1,3-丁二醇、聚丙二醇、木糖醇、赤蘚糖醇、麥芽糖醇、乳糖醇等,可調配入其中1種或者將2種以上組合調配。就確保透明性而言,該等濕潤劑於本發明之牙膏組合物中之含量,較好的是40~95質量%,更好的是60~80質量%。
本發明之牙膏組合物,可根據其用途依常法製成牙膏組合物、液狀牙膏組合物、凝膠狀牙膏組合物等。
以下實施例就木發明之實施加以說明。實施例係說明本發明之例示者,並不用以限定本發明。
於以下實施例中,水凝膠粒子之平均粒徑係以上述篩法進行測定。
將330 g離子交換水中溶解有20 g聚乙烯吡咯烷酮(ISP製,K-15,重量平均分子量為8000)而製備之水溶液(85℃)、及140 g離子交換水中溶解有10 g兒茶酸粉末(太陽化學(股)製,三苯酚100S)而製備之水溶液(20℃),以均質攪拌機加以混合(8000 r/min,1分鐘),獲得具有表1所示組成之兒茶酸/PVP複合物水分散液。
將321.5 g離子交換水中溶解有12.5 g瓊脂(伊那食品工業(股)製,UP-37)、4 g之PVP(ISP製,K-30,重量平均分子量為60000)、12 g之PVP(ISP製,K-90,重量平均分子量為1300000)而製備之水溶液(85℃)、及140 g離子交換水中溶解有10 g兒茶酸粉末(三苯酚100S)而製備之水溶液(20℃),以均質攪拌機加以混合(8000 r/min,1分鐘),然後於氣相中進行噴霧,藉此獲得具有表2所示組成之兒茶酸/PVP複合物內包水凝膠粒子。水凝膠粒子之平均粒徑為195 μm。
將10 g兒茶酸粉末(三苯酚100S)溶解於490 g離子交換水中,製備2重量%之兒茶酸水溶液。
使用實施例1中所獲得之兒茶酸/PVP複合物水分散液、實施例2中所獲得之兒茶酸/PVP複合物內包水凝膠粒子、比較例1中所獲得之兒茶酸水溶液,製備具有表3所示組成之製劑。將所獲得之製劑於50℃下保存1個月,依下述方法測定保存前後之明度差,根據該明度差來評價變色程度。結果示於表3。
將保存後之製劑裝滿於透明且容量為3 cm×3 cm×1 cm之盒(AS ONE公司,PS CASE No.1)中。與該盒一起,將作為顏色濃度標準之KODAK GRAY SCALE之A、2、4、6、8、10、12、14、B之9點(設為顏色濃度1~9)、及CASMATCH(大日本印刷製)置於相同視野中,於白紙上進行攝影。攝影係以環形光同樣的照明下,以固定的快門速度、光圈、焦距之條件進行。對以ADOBE PHOTOSHOP且採用CASMATCH為基準而對攝影圖像進行顏色補正後,以WINROOF(三谷商事股份有限公司)將被測定部位之明度(HSB彩色模式之Brightness)定量化,以下述式求出於50℃下保存1個月品之明度與初期之明度的差異,將其作為變色度。
變色度=(於50℃下保存1個月後之明度)-(初期之明度)
由表3可明瞭,於調配有實施例1之兒茶酸/PVP複合物水分散液、實施例2之兒茶酸/PVP複合物內包水凝膠粒子之情形時,與調配有比較例1之兒茶酸水溶液之情形相比,可抑制變色,尤其於調配有實施例2之水凝膠粒子之情形時,可大幅抑制變色。因此,可知於實施例1之兒茶酸/PVP複合物水分散液、實施例2之兒茶酸/PVP複合物內包水凝膠粒子中,可抑制由於兒茶酸的氧化及/或聚合而引起變色,從而使兒茶酸穩定化。
使用實施例1中所獲得之兒茶酸/PVP複合物水分散液、實施例2中所獲得之兒茶酸/PVP複合物內包水凝膠粒子、比較例1中所獲得之兒茶酸水溶液,製備具有表4所示組成之十二烷基硫酸鈉水溶液。以下述方法對於室溫下保存1個月後溶出至十二烷基硫酸鈉水溶液中的兒茶酸量進行定量,求出溶析率。結果示於表4。
採取1.0 g試料(十二烷基硫酸鈉水溶液),混合入19.0 g磷酸緩衝液、及5.0 g酒石酸鐵試藥。測定所製備的混合液於540 nm處之吸光度。繼而,使用兒茶酸粉末(三苯酚100S)製備濃度已知的兒茶酸水溶液,根據已製成的校準曲線計算試料中之兒茶酸濃度,且求出溶出率。再者,酒石酸鐵試藥,係將100 mg硫酸亞鐵(7水合鹽)及500 mg酒石酸鈉鉀溶於水中製備為100 ml;磷酸緩衝液,係將M/15磷酸氫二鈉溶液與M/15磷酸氫二鉀溶液以84:16之比例混合而製備。
利用試驗例1之明度差之測定結果,將描繪試驗例2中所獲得兒茶酸的溶出率與明度差的關係之結果示於圖1。由圖1可知,對十二烷基硫酸鈉水溶液的溶出率越少則明度差越小。即,可知將PVP/兒茶酸複合物與十二烷基硫酸鈉水溶液混合時,兒茶酸對十二烷基硫酸鈉水溶液中的溶出率越低則變色抑制效果越高,可抑制兒茶酸的氧化及/或聚合,因而兒茶酸之穩定性較高。
將327.5 g離子交換水中溶解有12.5 g瓊脂(UP-37)、10.0 g之PVP(K-30,重量平均分子量為60000)而製備之水溶液(85℃)、及145 g離子交換水中溶解有5 g兒茶酸粉末(三苯酚100S)而製備之水溶液(20℃),以均質攪拌機加以混合(8000 r/min,1分鐘),然後於氣相中進行噴霧,藉此獲得具有表5所示組成及平均粒徑之兒茶酸/PVP複合物內包水凝膠粒子。
除使用10.0 g之PVP(ISP製,K-60,重量平均分子量為400000)作為PVP以外,其餘以與實施例3同樣之方式獲得具有表5所示組成及平均粒徑之兒茶酸/PVP複合物內包水凝膠粒子。
除使用10.0 g之PVP(K-90,重量平均分子量為1300000)作為PVP以外,其餘以與實施例3相同之方式獲得具有表5所示組成及平均粒徑之兒茶酸/PVP複合物內包水凝膠粒子。
使用實施例3~5中製作之兒茶酸/PVP複合物內置水凝膠粒子,製備具有表6所示組成之十二烷基硫酸鈉水溶液。以與試驗例2相同之方式對於室溫下保存10天後溶出至十二烷基硫酸鈉水溶液中的兒茶酸量進行定量,求出溶出率。結果示於表6。
由表6之結果可知,若水凝膠粒子中的PVP分子量越高則越可降低溶出入十二烷基硫酸鈉水溶液的溶出率。若利用與試驗例1的明度差之關係,則可知PVP的分子量越高則變色抑制效果越高,越可抑制兒茶酸的氧化及/或聚合,兒茶酸之穩定性越高。
將325.5 g離子交換水中溶解有12.5 g瓊脂(UP-37)、3.0 g之PVP(K-30)、9.0 g之PVP(K-90)而製備之水溶液(85℃)、及140 g離子交換水中溶解有10 g兒茶酸粉末(三苯酚100S)而製備之水溶液(20℃),以均質攪拌機加以混合(8000 r/min,1分鐘),然後於氣相中進行噴霧,藉此獲得具有表7所示組成及平均粒徑之兒茶酸/PVP複合物內包水凝膠粒子。
將323.5 g離子交換水中溶解有12.5 g瓊脂(UP-37)、3.5 g之PVP(K-30)、10.5 g之PVP(K-90)而製備之水溶液(85℃)、及140 g離子交換水中溶解有10 g兒茶酸粉末(三苯酚100S)而製備之水溶液(20℃),以均質攪拌機加以混合(8000 r/min,1分鐘),然後於氣相中進行噴霧,藉此獲得具有表7所示組成及平均粒徑之兒茶酸/PVP複合物內包水凝膠粒子。
將323.5 g離子交換水中溶解有12.5 g瓊脂(UP-37)、5.0 g之PVP(K-30)、15.0 g之PVP(K-90)而製備之水溶液(85℃)、及140 g離子交換水中溶解有10 g兒茶酸粉末(三苯酚100S)而製備之水溶液(20℃),以均質攪拌機加以混合(8000 r/min,1分鐘),然後於氣相中進行噴霧,藉此獲得具有表7所示組成及平均粒徑之兒茶酸/PVP複合物內包水凝膠粒子。
將323.5 g離子交換水中溶解有12.5 g瓊脂(UP-37)、5.5 g之PVP(K-30)、16.5 g之PVP(K-90)而製備之水溶液(85℃)、及140 g離子交換水中溶解有10 g兒茶酸粉末(三苯酚100S)而製備之水溶液(20℃),以均質攪拌機加以混合(8000 r/min,1分鐘),然後於氣相中進行噴霧,藉此製備具有表7所示組成及平均粒徑之兒茶酸/PVP複合物內包水凝膠粒子。
使用實施例2、實施例6~9中所獲得之兒茶酸/PVP複合物內包水凝膠粒子,製備具有表8所示組成之十二烷基硫酸鈉水溶液。以與試驗例2相同之方式,對於室溫下保存20天後溶出至十二烷基硫酸鈉水溶液中的兒茶酸量進行定量,求出溶析率。結果示於表8。
由表8可明瞭,於調配有兒茶酸/PVP的重量比率為1.0/1.6之水凝膠粒子之情形時,溶出率變為極小值。即,可知於將水凝膠粒子中的兒茶酸/PVP比率設為1.0/1.6之情形時,變色抑制效果最高,可抑制兒茶酸的著色,兒茶酸穩定性較高。
以下沿用實施例說明本發明之牙膏組合物。
只要未特別說明,則例中之%為質量%。
將319 g離子交換水中溶解有15 g瓊脂(伊那食品工業(股),UP-37)、16 g之PVP(ISP公司,K-90,重量平均分子量為1300000)而製備之水溶液(85℃)、及140 g離子交換水中溶解有10 g茶萃取物(三苯酚100S太陽化學(股),兒茶酸含量為60~70%)而製備之水溶液(20℃),以均質攪拌機加以混合(8000 r/min,1分鐘),然後於氣相中進行噴霧,藉此獲得具有表9所示組成之水凝膠粒子。水凝膠粒子之平均粒徑為200 μm。
使用製造例1中所獲得之水凝膠粒子或者茶萃取物(三苯酚100S太陽化學(股),兒茶酸含量為60~70%),製備具有表10所示組成之牙膏組合物A(比較品)及牙膏組合物B(本發明品)。以下述方法對所獲得牙膏組合物A及B之變色及味道進行評價。結果示於表10。又,以下述方法調查對牙齦之效果。結果示於圖2及圖3。
將所獲得之牙膏組合物填充於容器中,於50℃下保存1個月,利用下述方法測定保存後之明度差,根據該明度差來評價變色程度。將保存後之牙膏組合物裝滿於透明且容量為3 cm×3 cm×1 cm之盒(AS ONE公司,PS CASE No.1)中。與該盒一起,將作為色濃度標準之KODAK GRAY SCALE之A、2、4、6、8、10、12、14、B之9點(設為色濃度1~9)、及CASMATCH(大日本印刷製)置於相同視野中,於白紙上進行攝影。攝影係以於環形光同樣照明下,以固定的快門速度、光圈、焦離之條件進行。以ADOBE PHOTOSHOP採用CASMATCH為基準對攝影圖像進行色修正後,以WINROOF(三谷商事股份有限公司)將被測定部位之明度(HSB彩色模式之Brightness)定量化,以下述式(I)求出於50℃下保存1個月的產品的明度與剛製造出(初始)的明度之差異作為變色度。
變色度=[於50℃下保存1個月後之明度]-[初期之明度](I)
由9名官能檢查員以下述3階段的基準,對牙膏組合物A及B之香味進行味道評價,以其平均值表示味道。
.評價標準1:不澀2:不太澀3:澀
給9名20多歲~50多歲男女分別使用牙膏組合物A及B達一週,調查使用前、使用後之BOP(Bleeding On Probing,探針出血)之變化。所謂BOP(Bleeding On Probing)係指將WHO探針插入至牙周囊袋(牙與牙齦之間隙)的牙肉底,拔出後之出血狀態,若牙齦健康則不出血,若囊袋及底部有炎症則簡單地引起出血。即,該BOP部位數之值越多則表示牙齦狀態越差。
由表10可明瞭,含有將兒茶酸類內包化的本發明水凝膠粒子之牙膏組合物B,與未將兒茶酸類內包化而直接含有之牙膏組合物A相比,可顯著抑制變色,味道亦優異。
又,由圖2及圖3可明瞭,於使用牙膏組合物A之情形時,於1週時間內BOP值幾乎未變化,並未改善牙齦狀態,但於使用牙膏組合物B之情形時,於1週時間內BOP值降低,牙齦狀態改善。一般認為,藉由使用水凝膠粒子化之兒茶酸而使得改善牙齦炎的效果提昇,為有用。
使用製造例1中所獲得之水凝膠粒子或者茶萃取物(三苯酚100S太陽化學(股),兒茶酸含量為60~70%),製備具有表11所示組成之牙膏組合物C(比較品)及牙膏組合物D(本發明品)。以與實施例10相同之方法對所獲得牙膏組合物C及D之變色及味道進行評價。結果示於表11。
由表11可明瞭,含有將兒茶酸類內包化的本發明之水凝膠粒子之牙膏組合物D,與未將兒茶酸類內包化而直接含有之牙膏組合物C相比,可顯著抑制變色,味道亦優異。
圖1係表示試驗例1中所獲得明度差與試驗例2中所獲得兒茶酸的溶出率之關係之圖。
圖2係表示牙膏組合物A對牙齦之效果之圖。
圖3係表示牙膏組合物B對牙齦之效果之圖。
(無元件符號說明)
Claims (9)
- 一種水凝膠粒子,其係含有兒茶酸類以及與兒茶酸類形成水不溶性複合物的聚合物A,其中聚合物A為聚乙烯吡咯烷酮。
- 如請求項1之水凝膠粒子,其中水凝膠為瓊脂。
- 如請求項1或2之水凝膠粒子,其中聚合物A之重量平均分子量為6000~3000000。
- 如請求項1或2之水凝膠粒子,其中相對於兒茶酸類,添加1~4倍重量之聚合物A。
- 如請求項1或2之水凝膠粒子,其中水凝膠粒子中之兒茶酸類之含有量為0.001~10質量%。
- 如請求項1或2之水凝膠粒子,其中水凝膠粒子之平均粒徑為5~10000μm。
- 一種牙膏組合物,其含有:請求項1~6中任一項之水凝膠粒子、黏結劑、以及水。
- 如請求項7之牙膏組合物,其中黏結劑為選自由海藻酸鈉、羧甲基纖維素鈉、角叉菜膠、三仙膠、聚丙烯酸鈉、羥乙基纖維素、羥丙基纖維素、果膠、黃蓍膠、阿拉伯膠、瓜爾膠、刺梧桐樹膠、刺槐豆膠、結蘭膠、羅望子膠、洋車前子膠、聚乙烯醇、軟骨素硫酸鈉及甲氧基乙烯-馬來酸酐共聚物所組成之群中之至少1種。
- 一種兒茶酸類著色抑制方法,其係使用請求項1~6中任一項之水凝膠粒子。
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2007
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- 2007-06-26 US US12/374,099 patent/US20100008869A1/en not_active Abandoned
- 2007-07-18 TW TW096126176A patent/TWI395745B/zh not_active IP Right Cessation
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2015
- 2015-04-07 US US14/680,145 patent/US10213376B2/en active Active
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Also Published As
Publication number | Publication date |
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US20150209267A1 (en) | 2015-07-30 |
WO2008010403A1 (fr) | 2008-01-24 |
US10213376B2 (en) | 2019-02-26 |
TW200821290A (en) | 2008-05-16 |
EP2045248A4 (en) | 2012-07-11 |
US20100008869A1 (en) | 2010-01-14 |
EP2045248A1 (en) | 2009-04-08 |
EP2045248B1 (en) | 2013-09-25 |
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