JP5536721B2 - 油の微細分散組成物 - Google Patents
油の微細分散組成物 Download PDFInfo
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- JP5536721B2 JP5536721B2 JP2011154605A JP2011154605A JP5536721B2 JP 5536721 B2 JP5536721 B2 JP 5536721B2 JP 2011154605 A JP2011154605 A JP 2011154605A JP 2011154605 A JP2011154605 A JP 2011154605A JP 5536721 B2 JP5536721 B2 JP 5536721B2
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- 239000004006 olive oil Substances 0.000 description 1
- DXGLGDHPHMLXJC-UHFFFAOYSA-N oxybenzone Chemical compound OC1=CC(OC)=CC=C1C(=O)C1=CC=CC=C1 DXGLGDHPHMLXJC-UHFFFAOYSA-N 0.000 description 1
- 235000019629 palatability Nutrition 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 235000019271 petrolatum Nutrition 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 229920002432 poly(vinyl methyl ether) polymer Polymers 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 229920000120 polyethyl acrylate Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 235000019423 pullulan Nutrition 0.000 description 1
- 239000008165 rice bran oil Substances 0.000 description 1
- 235000005713 safflower oil Nutrition 0.000 description 1
- 239000003813 safflower oil Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 210000004761 scalp Anatomy 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000011803 sesame oil Nutrition 0.000 description 1
- 239000008159 sesame oil Substances 0.000 description 1
- 239000012176 shellac wax Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 229940031439 squalene Drugs 0.000 description 1
- TUHBEKDERLKLEC-UHFFFAOYSA-N squalene Natural products CC(=CCCC(=CCCC(=CCCC=C(/C)CCC=C(/C)CC=C(C)C)C)C)C TUHBEKDERLKLEC-UHFFFAOYSA-N 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229940012831 stearyl alcohol Drugs 0.000 description 1
- 235000003702 sterols Nutrition 0.000 description 1
- 150000003432 sterols Chemical class 0.000 description 1
- 239000002600 sunflower oil Substances 0.000 description 1
- 239000003784 tall oil Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- BORJONZPSTVSFP-UHFFFAOYSA-N tetradecyl 2-hydroxypropanoate Chemical compound CCCCCCCCCCCCCCOC(=O)C(C)O BORJONZPSTVSFP-UHFFFAOYSA-N 0.000 description 1
- DZKXJUASMGQEMA-UHFFFAOYSA-N tetradecyl tetradecanoate Chemical compound CCCCCCCCCCCCCCOC(=O)CCCCCCCCCCCCC DZKXJUASMGQEMA-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- GYDJEQRTZSCIOI-LJGSYFOKSA-N tranexamic acid Chemical compound NC[C@H]1CC[C@H](C(O)=O)CC1 GYDJEQRTZSCIOI-LJGSYFOKSA-N 0.000 description 1
- 229960000401 tranexamic acid Drugs 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
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- 235000013311 vegetables Nutrition 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 235000019155 vitamin A Nutrition 0.000 description 1
- 239000011719 vitamin A Substances 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 235000019166 vitamin D Nutrition 0.000 description 1
- 239000011710 vitamin D Substances 0.000 description 1
- 150000003710 vitamin D derivatives Chemical class 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
- 229940045997 vitamin a Drugs 0.000 description 1
- 229940046008 vitamin d Drugs 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 239000010497 wheat germ oil Substances 0.000 description 1
- 229940105125 zinc myristate Drugs 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
- GBFLQPIIIRJQLU-UHFFFAOYSA-L zinc;tetradecanoate Chemical compound [Zn+2].CCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCC([O-])=O GBFLQPIIIRJQLU-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Colloid Chemistry (AREA)
- Cosmetics (AREA)
Description
HM4500/50℃
ホモミキサー(特殊機化社製)を用いて9000rpmの回転速度で剪断混合しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水相に添加した後、ホモミキサーの回転速度を4500rpmにしてさらに剪断混合しながら、氷水中で2.5分間かけて50℃まで冷却した。ホモミキサーを停止し、次にプロペラミキサー(HEIDON社製)を用いて150rpmで攪拌しながら30℃まで冷却した。
HM4500/40℃
ホモミキサーを用いて9000rpmの回転速度で剪断混合しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水相に添加した後、ホモミキサーの回転速度を4500rpmにしてさらに剪断混合しながら、氷水中で5分間かけて40℃まで冷却した。ホモミキサーを停止し、次にプロペラミキサーを用いて150rpmで攪拌しながら30℃まで冷却した。
HM9000/50℃
ホモミキサーを用いて9000rpmの回転速度で剪断混合しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水相に添加した後、9000rpmの回転速度のままホモミキサーでさらに剪断混合しながら、氷水中で2.5分間かけて50℃まで冷却した。ホモミキサーを停止し、次にプロペラミキサーを用いて150rpmで攪拌しながら30℃まで冷却した。
HM9000/40℃
ホモミキサーを用いて9000rpmの回転速度で剪断混合しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水相に添加した後、9000rpmの回転速度のままホモミキサーでさらに剪断混合しながら、氷水中で5分間かけて40℃まで冷却した。ホモミキサーを停止し、次にプロペラミキサーを用いて150rpmで攪拌しながら30℃まで冷却した。
PM175/70℃
プロペラミキサーを用いて175rpmの回転速度で攪拌しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水相に添加した後、プロペラミキサーの回転速度を150rpmにしてさらに攪拌しながら、氷水中で30℃まで冷却した。
PM300/70℃
プロペラミキサーを用いて300rpmの回転速度で攪拌しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水相に添加した後、プロペラミキサーの回転速度を150rpmにしてさらに攪拌しながら、氷水中で30℃まで冷却した。
PM500/70℃
プロペラミキサーを用いて500rpmの回転速度で攪拌しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水相に添加した後、プロペラミキサーの回転速度を150rpmにしてさらに攪拌しながら、氷水中で30℃まで冷却した。
HM4500/70℃
ホモミキサーを用いて4500rpmの回転速度で攪拌しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水相に添加した後、ホモミキサーを停止し、次にプロペラミキサーを用いて150rpmで攪拌しながら30℃まで冷却した。
HM9000/70℃
ホモミキサーを用いて9000rpmの回転速度で攪拌しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水相に添加した後、ホモミキサーを停止し、次にプロペラミキサーを用いて150rpmで攪拌しながら30℃まで冷却した。
分散組成物中の油の粒子の形状、分散状態および平均最大寸法は、55mmφのシャーレに3gの試料を広げ、光学顕微鏡で観察し、上部よりスケールと共にデジタルカメラで画像を取り込み、光学顕微鏡写真を用いて評価した。平均最大寸法は、無作為に選択した50個の粒子の最大寸法をスケール(1目盛2.5μm)から読み取り、平均値を計算して求めた。図1に、実施例1から4の各分散処理条件によって作成した分散組成物の製造直後の光学顕微鏡写真を示す。
分散組成物の経時安定性は、各温度で3ヶ月放置した後の組成物の光学顕微鏡写真を用いて、以下の評価基準で評価した:
○:粒子の凝集に変化なし
△:粒子の凝集が若干増加した
×:粒子の凝集が顕著に増加した
図2に、実施例1の分散処理条件によって作成した分散組成物の、製造直後、ならびに、−5℃、0℃、室温(RT)、37℃、および50℃で3ヶ月放置後の光学顕微鏡写真を示す。
微細分散組成物の使用性(指どれ、肌なじみ)および使用感(しっとり感、ふっくら感)の評価は、専門パネルによる官能試験により行った。20名の女性パネルの前腕部に各試料を塗布し、以下の評価基準で評価させた:
(指どれ)
○:指でとりやすいと評価したパネルが15名以上
△:指でとりやすいと評価したパネルが6〜14名
×:指でとりやすいと評価したパネルが5名以下
(肌なじみ)
○:肌になじみやすいと評価したパネルが15名以上
△:肌になじみやすいと評価したパネルが6〜14名
×:肌になじみやすいと評価したパネルが5名以下
(しっとり感)
○:塗布後の肌にしっとり感があると評価したパネルが15名以上
△:塗布後の肌にしっとり感があると評価したパネルが6〜14名
×:塗布後の肌にしっとり感があると評価したパネルが5名以下
(ふっくら感)
○:塗布後の肌にふっくら感があると評価したパネルが15名以上
△:塗布後の肌にふっくら感があると評価したパネルが6〜14名
×:塗布後の肌にふっくら感があると評価したパネルが5名以下
ホモミキサー(特殊機化社製)を用いて9000rpmの回転速度で剪断混合しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水相に添加した後、9000rpmのまま剪断混合しながら、氷水中で5分間かけて40℃まで冷却した。ホモミキサーを停止し、次にプロペラミキサー(HEIDON社製)を用いて150rpmで攪拌しながら30℃まで冷却した。
プロペラミキサーを用いて180rpmの回転速度で攪拌しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水に添加した後、残りの成分を添加し、プロペラミキサーの回転速度を150rpmにしてさらに攪拌しながら、氷水中で30℃まで冷却した。
スキンケアパネル7名に、使用性および使用感に関する様々な項目につき、実施例5と比較例6の組成物を比較して以下の評価基準で評価させた:
−2:比較例6が顕著に優れている
−1:比較例6が僅かに優れている
0: 同程度である
1: 実施例5が僅かに優れている
2: 実施例5が顕著に優れている
各項目につき7名のパネルの採点の平均値を求め、図4のグラフに示す。
寒天配合処方
水溶性増粘剤として寒天を用い、以下の処方(表4)および製造方法に基づき調製した:
ホモミキサー(特殊機化社製)を用いて9000rpmの回転速度で剪断混合しながら、寒天を溶解させた70℃の水相に、70℃〜75℃に加熱した液状の油相を1分間かけて添加した後、ホモミキサーの回転速度を4500rpmにしてさらに剪断混合しながら、氷水中で55℃まで冷却した。ホモミキサーを停止し、寒天が完全に固化するまで放置冷却した後、さらにホモミキサーを用いて4500rpmで10分間剪断混合した。
ミクロゲル配合処方(1)
水溶性増粘剤としてミクロゲル(特開2004−43785号公報参照)を用い、以下の処方(表5)および製造方法に基づき調製した:
ホモミキサー(特殊機化社製)を用いて9000rpmの回転速度で剪断混合しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水相に添加した後、ホモミキサーの回転速度を6500rpmにしてさらに剪断混合しながら、氷水中で8分間かけて45℃まで冷却した。
ミクロゲル配合処方(2)
水溶性増粘剤としてミクロゲル(特開2004−43785号公報参照)を用い、以下の処方(表6)および製造方法に基づき調製した:
ホモミキサー(特殊機化社製)を用いて9000rpmの回転速度で剪断混合しながら、約70℃〜75℃に加熱して融解させた液状の油相を、約70℃に加熱した水相に添加した後、氷水中で冷却しながら、55℃まで9000rpmのまま剪断混合し、55℃から50℃まで6000rpmで剪断混合し、さらに50℃のまま4500rpmで剪断混合した。
処方例1:乳液(KOH中和)
処方例2:乳液(AMPD中和)
処方例3:乳液(アルギニン中和/保湿剤配合量が少ないさっぱりタイプ)
処方例4:乳液(AMPD中和/保湿剤および油分配合量が少ないさらさらタイプ)
処方例5:乳液(AMPD中和/油分配合量が少ないさっぱりタイプ)
処方例6:水添ポリイソブテン配合処方(使用性リッチタイプ)
処方例7:アルコール配合処方(さっぱり感付与タイプ)
処方例8:固形油分リッチ処方(使用性硬いタイプ)
処方例9:ベヘニルアルコール配合処方(使用性柔らかいタイプ)
処方例10:アクリル酸・メタクリル酸アルキル共重合体配合処方
処方例11:単純処方
Claims (11)
- 油の微細分散組成物であって、固形油分および液状油分を含有する油相と、水溶性増粘剤を含有する水相とから成り、界面活性剤を含まず、前記油相の配合量が組成物の全質量に対して1〜20質量%であり、前記油相が、該油相の全質量に対して10〜50質量%の固形油分および50〜90質量%の液状油分を含有し、該油相が、一次粒子の平均最大寸法が0.1〜30μmの微粒子として前記水相中に分散しており、該微粒子において前記固形油分が結晶化していることを特徴とする、油の微細分散組成物(但し、油相中に液状油分を吸着させる高分子成分を含むものを除く)。
- 前記一次粒子の平均最大寸法が1〜15μmであることを特徴とする、請求項1記載の油の微細分散組成物。
- 前記油相が、該油相の全質量に対して10〜20質量%の固形油分、および80〜90質量%の液状油分を含有することを特徴とする、請求項1または2記載の油の微細分散組成物。
- 前記固形油分が、キャンデリラロウおよび炭素数16以上の高級アルコールより成る群から選択される1種または2種以上を含むことを特徴とする、請求項1から3いずれか1項記載の油の微細分散組成物。
- 前記油相が、親油性ゲル化剤をさらに含有することを特徴とする、請求項1から4いずれか1項記載の油の微細分散組成物。
- 前記水溶性増粘剤が、カルボキシビニルポリマーまたは寒天を含むことを特徴とする、請求項1から5いずれか1項記載の油の微細分散組成物。
- 請求項1から6いずれか1項記載の油の微細分散組成物を含有する皮膚外用剤。
- 油の微細分散組成物の製造方法であって、
固形油分および液状油分を含有する油相を、該固形油分の融点より高い温度で、水溶性増粘剤を含有する前記固形油分の融点より高い温度にある水相に添加する工程;
前記油相と水相との混合物を、前記固形油分の融点以下の温度まで、高速剪断分散装置または高圧剪断分散装置によって剪断混合して、前記油相を微粒子として水相中に分散させる工程;および
前記分散工程の後、さらに攪拌する工程;を含み、
前記油相および水相が界面活性剤を含まず、
前記微粒子の一次粒子の平均最大寸法が0.1〜30μmであることを特徴とする、油の微細分散組成物の製造方法。 - 前記微粒子の一次粒子の平均最大寸法が1〜15μmであることを特徴とする、請求項8記載の製造方法。
- 前記剪断混合を、ホモミキサー、ホモディスパー、フロージェットミキサー、ウルトラミキサー、コロイドミル、またはホモジナイザーによって行うことを特徴とする、請求項8または9記載の製造方法。
- 前記攪拌工程を、プロペラミキサー、パドルミキサー、アンカーミキサー、ゲートミキサー、またはプラネタリーミキサーによって行うことを特徴とする、請求項8から10いずれか1項記載の製造方法。
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