TW202228640A - 組合物及其製造方法以及化妝料 - Google Patents
組合物及其製造方法以及化妝料 Download PDFInfo
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Abstract
本發明之目的在於提供一種賦予優異之乳化穩定性及分散穩定性之組合物(特別是香妝品原料組合物)。上述目的可藉由如下組合物來達成,該組合物之特徵在於含有說明書中所記載之成分A及選自由成分B、成分C、成分D及成分E所組成之群中之1種以上之成分(其中,單為上述成分C除外或單為上述成分D除外)。
Description
本發明係關於一種組合物(特別是香妝品原料組合物)及其製造方法以及化妝料。
含有醯基之胺基酸衍生物即便是微量添加,其作為香妝品原料,亦會改善特別是接近毛髮或皮膚之pH值之弱酸性配方之穩定性或乳化性、分散性,故而近年來特別受重視。例如,於專利文獻1中揭示了具有含有醯基之胺基酸衍生物之凝膠狀組合物為穩定性、使用感優異之組合物。又,於專利文獻2中揭示了一種技術,其有助於藉由調配含有醯基之胺基酸衍生物所得之化妝料之配方穩定性或防腐效果或低刺激性。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本專利第4070768號公報
[專利文獻2]日本專利特開2006-160686號公報
[發明所欲解決之問題]
對於香妝品配方高度要求乳化能力或分散能力特別是在護膚、毛髮護理用途中常見。然而,於如專利文獻1、2等所記載之先前之香妝品配方中,至今仍不易獲得高度之乳化穩定性或分散穩定性。
因此,本發明之目的在於提供一種賦予優異之乳化穩定性及分散穩定性之組合物(特別是香妝品原料組合物)。
即,本發明人等為了達成上述目的反覆進行了銳意研究,結果發現藉由將具有特定結構之含有醯基之胺基酸衍生物與各種成分組合,可提供一種賦予優異之乳化穩定性及分散穩定性之組合物。
即,本發明如下。
[1]
一種組合物,其特徵在於:含有下述成分A、及
選自由下述成分B、下述成分C、下述成分D及下述成分E所組成之群中之1種以上之成分(其中,單為上述成分C除外或單為上述成分D除外),
・成分A:下述通式(A)所表示之含有醯基之胺基酸衍生物或其鹽
[化1]
(式(A)中,
R
1及R
2分別獨立地為飽和或不飽和之直鏈或支鏈狀烴基,
M
1、M
2及M
3分別獨立地為氫原子、鹼金屬、鹼土類金屬、有機或無機胺、鹼性胺基酸、膽鹼、鋁或鋅,
n
1及n
2為0及2,或者為2及0,
n
3及n
4為0及2,或者為2及0)
・成分B:下述通式(B)所表示之N-醯基吡咯啶酮羧酸或其鹽
[化2]
(式(B)中,
R
3為飽和或不飽和之直鏈或支鏈狀烴基,
M
4為氫原子、鹼金屬、鹼土類金屬、有機或無機胺、鹼性胺基酸、膽鹼、鋁或鋅)
・成分C:下述通式(C)所表示之醯基麩胺酸或其鹽
[化3]
(式(C)中,
R
4為飽和或不飽和之直鏈或支鏈狀烴基,
M
5及M
6分別獨立地為氫原子、鹼金屬、鹼土類金屬、有機或無機胺、鹼性胺基酸、膽鹼、鋁或鋅)
・成分D:下述通式(D)所表示之脂肪酸或其鹽
[化4]
(式(D)中,
R
5為飽和或不飽和之直鏈或支鏈狀烴基,
M
7為氫原子、鹼金屬、鹼土類金屬、有機或無機胺、鹼性胺基酸、膽鹼、鋁或鋅)
・成分E:下述通式(E)所表示之脂肪酸醯胺
[化5]
(式(E)中,
R
6為飽和或不飽和之直鏈或支鏈狀烴基)。
[2]
如[1]中所記載之組合物,其含有上述成分A及上述成分B。
[3]
如[1]中所記載之組合物,其含有上述成分A及上述成分E。
[4]
如[1]中所記載之組合物,其含有上述成分A、上述成分B及上述成分E。
[5]
如[1]至[4]中任一項所記載之組合物,其中上述通式(A)~(E)中之R
1~R
6分別獨立地為碳化數1~29之烴基。
[6]
如[1]至[5]中任一項所記載之組合物,其中上述通式(A)~(D)中之M
1~M
7分別獨立地為Na、K、三乙醇胺、Mg、Ca、Al、Zn、精胺酸或H。
[7]
如[1]、[2]、[4]、[5]及[6]中任一項所記載之組合物,其中上述成分B相對於上述成分A之比率為0.004%以上。
[8]
如[1]及[5]~[7]中任一項所記載之組合物,其中以上述成分A與上述成分C之合計質量為基準,上述成分C之量為0.8質量%以上,且
以上述成分A與上述成分D之合計質量為基準,上述成分D之量為0.06質量%以上。
[9]
如[1]及[3]~[8]中任一項所記載之組合物,其中以上述成分A之質量為基準,上述成分E之量為0.005質量%以上。
[10]
一種如[1]、[2]及[4]~[9]中任一項所記載之組合物之製造方法,其包括如下步驟:
1)於包含水及有機溶劑之混合溶劑中,使麩胺酸或其鹽與脂肪醯氯進行反應,獲得包含N-醯基麩胺酸或其鹽之反應液,利用酸使上述反應液之pH值成為1~6,於25~80℃之溫度下分層為有機層與水層;
2)於酸性下對上述有機層進行濃縮乾燥,將上述N-醯基麩胺酸或其鹽之一部分轉化為N-醯基吡咯啶酮羧酸或其鹽;
3)使上述N-醯基麩胺酸或其鹽與酸酐進行反應,而獲得N-醯基麩胺酸酐;及
4)使上述N-醯基麩胺酸酐與離胺酸或其鹽進行反應,而獲得含有醯基之胺基酸衍生物或其鹽。
[11]
如[10]中所記載之製造方法,其中於上述步驟2)中,對上述有機相進行濃縮乾燥直至乾燥減量達到10質量%以下。
[12]
如[10]或[11]中所記載之製造方法,其於減壓下且於50℃以上實施上述步驟2)中之濃縮乾燥。
[13]
如[1]~[9]中任一項所記載之組合物,其係香妝品原料組合物。
[14]
一種如[1]~[9]中任一項所記載之組合物之用途,其係用作香妝品原料。
[15]
一種化妝料,其調配有如[1]~[9]中任一項所記載之組合物。
[16]
如[15]中所記載之化妝料,其pH值為4以上。
[發明之效果]
根據本發明,可提供一種賦予優異之乳化穩定性及分散穩定性之組合物(特別是香妝品原料組合物)。
以下,對本發明之實施方式(以下,僅稱為「本實施方式」)進行詳細說明。以下之本實施方式為用於說明本發明之例示,本發明並不限定於以下之內容。本發明可於其主旨之範圍內適宜地變化而實施。
[組合物]
本實施方式係關於一種組合物(特別是香妝品原料組合物)及調配有該組合物之化妝料,該組合物之特徵在於含有:下述成分A及選自由下述成分B、下述成分C、下述成分D及下述成分E所組成之群中之1種以上之成分(其中,單為成分C除外或單為成分D除外)。作為成分之組合,例如可例舉:A+B、A+E、A+B+C、A+B+D、A+B+E、A+C+D、A+C+E、A+B+C+D、A+B+C+E、A+C+D+E。
成分A為下述通式(A)所表示之含有醯基之胺基酸衍生物或其鹽。
[化6]
(式(A)中,
R
1及R
2分別獨立地為飽和或不飽和之直鏈或支鏈狀烴基,
M
1、M
2及M
3分別獨立地為氫原子、鹼金屬、鹼土類金屬、有機或無機胺、鹼性胺基酸或膽鹼,
n
1及n
2為0及2,或者為2及0,
n
3及n
4為0及2,或者為2及0)
成分B為下述通式(B)所表示之N-醯基吡咯啶酮羧酸或其鹽。再者,於本說明書中,成分B亦稱為「醯基PCA(Pyrrolidone Carboxylate,吡咯啶酮羧酸)」。
[化7]
(式(B)中,
R
3為飽和或不飽和之直鏈或支鏈狀烴基,
M
4為氫原子、鹼金屬、鹼土類金屬、有機或無機胺、鹼性胺基酸或膽鹼)
成分C為下述通式(C)所表示之醯基麩胺酸或其鹽。
[化8]
(式(C)中,
R
4為飽和或不飽和之直鏈或支鏈狀烴基,
M
5及M
6分別獨立地為氫原子、鹼金屬、鹼土類金屬、有機或無機胺、鹼性胺基酸或膽鹼)
本實施方式之香妝品原料組合物可對香妝品配方賦予高度之初始乳化穩定性或分散穩定性,且亦可賦予良好之使用感。
通式(A)中之R
1及R
2為烴基即可,並不限定於飽和、不飽和、支鏈、支鏈之種類,均可使用。例如,R
1及R
2可分別獨立地為碳數9之烴基、碳數11之烴基、碳數13之烴基、碳數15之烴基、碳數17之烴基、碳數19之烴基、碳數21之烴基。特別是,R
1-C(=O)-結構及R
2-C(=O)-結構可使用己醯基、十一碳烯醯基、月桂醯基、肉豆蔻醯基、異肉豆蔻醯基、棕櫚醯基、異棕櫚醯基、硬脂醯基、異硬脂醯基、油基、亞油基、亞麻基、二十烷基、山萮基等社會上廣泛流通之烴基,亦可使用源自棕櫚油、棕櫚仁油、椰子油之組合物之混合烴基。例如,碳數1~29之烴基。較佳為碳數7~23之烴基。更佳為碳數7~17之烴基。特佳為使用烴基中之不難管理抗空氣氧化之飽和烴基。就經濟性觀點而言,R
1-C(=O)-結構及R
2-C(=O)-結構進而更佳為月桂醯基及/或肉豆蔻醯基。
通式(A)所代表之含有醯基之胺基酸衍生物之3個羧酸基可全部為游離羧酸,亦可全部為羧酸鹽,還可為游離羧酸與羧酸鹽之組合。
通式(A)中之羧酸鹽(COOM
1、COOM
2、COOM
3)並無特別限定,例如可例舉:鈉鹽、鉀鹽、鋰鹽、鎂鹽、鈣鹽等鹼金屬鹽或鹼土類金屬鹽;銨鹽、烷胺鹽、單乙醇胺鹽、二乙醇胺鹽、三乙醇胺鹽、胺甲基丙醇鹽等胺鹽(有機或無機銨鹽);離胺酸鹽、精胺酸鹽等鹼性胺基酸鹽;膽鹼鹽、鋁鹽、鋅鹽等之單一物質或混合物。就性能或獲得容易性之觀點而言,較佳為鈉鹽、鉀鹽、鎂鹽及三乙醇胺鹽、精胺酸,更佳為鈉鹽。
以香妝品原料組合物之質量為基準,成分A之含量較佳為0.003~3質量%,更佳為0.01~2質量%,進而較佳為0.02~0.5質量%。
通式(B)中之R
3為烴基即可,並不限定於飽和、不飽和、支鏈、支鏈之種類,均可使用。例如,R
3可為碳數9之烴基、碳數11之烴基、碳數13之烴基、碳數15之烴基、碳數17之烴基、碳數19之烴基、碳數21之烴基。特別是,R
3-C(=O)-結構可使用己醯基、十一碳烯醯基、月桂醯基、肉豆蔻醯基、異肉豆蔻醯基、棕櫚醯基、異棕櫚醯基、硬脂醯基、異硬脂醯基、油基、亞油基、亞麻基、二十烷基、山萮基等社會上廣泛流通之烴基,亦可使用源自棕櫚油、棕櫚仁油、椰子油之組合物之混合烴基。較佳為碳數7~23之烴基。例如,碳數1~29之烴基。更佳為碳數7~17之烴基。特佳為使用烴基中之不難管理抗空氣氧化之飽和烴基。就經濟性觀點而言,R
3-C(=O)-結構進而更佳為月桂醯基及/或肉豆蔻醯基。
通式(B)中之羧酸鹽(COOM
4)並無特別限定,例如可例舉:鈉鹽、鉀鹽、鋰鹽、鎂鹽、鈣鹽等鹼金屬鹽或鹼土類金屬鹽;銨鹽、烷胺鹽、單乙醇胺鹽、二乙醇胺鹽、三乙醇胺鹽、胺甲基丙醇鹽等胺鹽(有機或無機銨鹽);離胺酸鹽、精胺酸鹽等鹼性胺基酸鹽;膽鹼鹽、鋁鹽、鋅鹽等之單一物質或混合物。就性能或獲得容易性之觀點而言,較佳為鈉鹽、鉀鹽、鎂鹽及三乙醇胺鹽、精胺酸,更佳為鈉鹽。
就對香妝品配方賦予高度之初始乳化穩定性或分散穩定性之觀點及經濟性之觀點而言,成分B相對於成分A之比率較佳為0.004%以上7.0%以下,更佳為0.01%以上3.5%以下,進而較佳為0.02%以上2.0%以下。若成分B之含量為0.004%以上,則配方系統中之乳化性及乳化穩定性進一步提昇,又,若成分B為7.0%以下,則配方系統之溶解穩定性進一步提昇。上述比率可藉由下述實施例所記載之HPLC(high performance liquid chromatography,高效液相層析)分析法來測定。
以香妝品原料組合物之質量為基準,成分B之含量較佳為0.00003~0.03質量%,更佳為0.0001~0.02質量%,進而較佳為0.0002~0.005質量%。
通式(C)中之R
4為烴基即可,並不限定於飽和、不飽和、支鏈、支鏈之種類,均可使用。例如,R
4可為碳數9之烴基、碳數11之烴基、碳數13之烴基、碳數15之烴基、碳數17之烴基、碳數19之烴基、碳數21之烴基。特別是,R
4-C(=O)-結構可使用己醯基、十一碳烯醯基、月桂醯基、肉豆蔻醯基、異肉豆蔻醯基、棕櫚醯基、異棕櫚醯基、硬脂醯基、異硬脂醯基、油基、亞油基、亞麻基、二十烷基、山萮基等社會上廣泛流通之烴基,亦可使用源自棕櫚油、棕櫚仁油、椰子油之組合物之混合烴基。例如,碳數1~29之烴基。較佳為碳數7~23之烴基。更佳為碳數7~17之烴基。特佳為使用烴基中之不難管理抗空氣氧化之飽和烴基。就經濟性觀點而言,R
4-C(=O)-結構進而更佳為月桂醯基及/或肉豆蔻醯基。
通式(C)中之羧酸鹽(COOM
5、COOM
6)並無特別限定,例如可例舉:鈉鹽、鉀鹽、鋰鹽、鎂鹽、鈣鹽等鹼金屬鹽或鹼土類金屬鹽;銨鹽、烷胺鹽、單乙醇胺鹽、二乙醇胺鹽、三乙醇胺鹽、胺甲基丙醇鹽等胺鹽(有機或無機銨鹽);離胺酸鹽、精胺酸鹽等鹼性胺基酸鹽;膽鹼鹽、鋁鹽、鋅鹽等之單一物質或混合物。就性能或獲得容易性之觀點而言,較佳為鈉鹽、鉀鹽、鎂鹽及三乙醇胺鹽、精胺酸,更佳為鈉鹽。
以成分A與成分C之合計質量為基準,成分C之含量(%)較佳為0.8質量%以上,更佳為0.8質量%以上8.0質量%以下,進而較佳為1.1質量%以上8.0質量%以下,特佳為1.5質量%以上6.0質量%以下。上述比率可藉由下述實施例所記載之方法來測定。
通式(D)中之R
5為烴基即可,並不限定於飽和、不飽和、支鏈、支鏈之種類,均可使用。例如,R
5可為碳數9之烴基、碳數11之烴基、碳數13之烴基、碳數15之烴基、碳數17之烴基、碳數19之烴基、碳數21之烴基。特別是,R
5-C(=O)-結構可使用己醯基、十一碳烯醯基、月桂醯基、肉豆蔻醯基、異肉豆蔻醯基、棕櫚醯基、異棕櫚醯基、硬脂醯基、異硬脂醯基、油基、亞油基、亞麻基、二十烷基、山萮基等社會上廣泛流通之烴基,亦可使用源自棕櫚油、棕櫚仁油、椰子油之組合物之混合烴基。例如,碳數1~29之烴基。較佳為碳數7~23之烴基。更佳為碳數7~17之烴基。特佳為使用烴基中之不難管理抗空氣氧化之飽和烴基。就經濟性觀點而言,R
5-C(=O)-結構進而更佳為月桂醯基及/或肉豆蔻醯基。
通式(D)中之羧酸鹽(COOM
7)並無特別限定,例如可例舉:鈉鹽、鉀鹽、鋰鹽、鎂鹽、鈣鹽等鹼金屬鹽或鹼土類金屬鹽;銨鹽、烷胺鹽、單乙醇胺鹽、二乙醇胺鹽、三乙醇胺鹽、胺甲基丙醇鹽等胺鹽(有機或無機銨鹽);離胺酸鹽、精胺酸鹽等鹼性胺基酸鹽;膽鹼鹽、鋁鹽、鋅鹽等之單一物質或混合物。就性能或獲得容易性之觀點而言,較佳為鈉鹽、鉀鹽、鎂鹽及三乙醇胺鹽、精胺酸,更佳為鈉鹽。
以成分A與成分D之合計質量為基準,成分D之含量(%)較佳為0.06質量%以上,進而較佳為0.06質量%以上3.0質量%以下,進而較佳為0.11質量%以上3.0質量%以下,特佳為0.14質量%以上0.55質量%以下。上述比率可藉由下述實施例所記載之方法來測定。
通式(E)中之R
6為烴基即可,並不限定於飽和、不飽和、支鏈、支鏈之種類,均可使用。例如,R
6可為碳數9之烴基、碳數11之烴基、碳數13之烴基、碳數15之烴基、碳數17之烴基、碳數19之烴基、碳數21之烴基。特別是,R
6-C(=O)-結構可使用己醯基、十一碳烯醯基、月桂醯基、肉豆蔻醯基、異肉豆蔻醯基、棕櫚醯基、異棕櫚醯基、硬脂醯基、異硬脂醯基、油基、亞油基、亞麻基、二十烷基、山萮基等社會上廣泛流通之烴基,亦可使用源自棕櫚油、棕櫚仁油、椰子油之組合物之混合烴基。例如,碳數1~29之烴基。較佳為碳數7~23之烴基。更佳為碳數7~17之烴基。特佳為使用烴基中之不難管理抗空氣氧化之飽和烴基。就經濟性觀點而言,R
6-C(=O)-結構進而更佳為月桂醯基及/或肉豆蔻醯基。
就對香妝品配方賦予高度之初始乳化穩定性或分散穩定性之觀點及生產性之觀點而言,成分E相對於成分A之比率(成分A/成分E)較佳為0.005質量%以上5.00質量%以下,更佳為0.02質量%以上3.00質量%以下,進而較佳為0.08質量%以上0.6質量%以下。上述比率可藉由下述實施例所記載之方法來測定。
本實施方式之香妝品原料組合物及調配有該組合物之化妝料之pH值並無特別限定,較佳為4.0~9.0,更佳為4.5~8.5,進而較佳為5.0~8.0。
式(A)~(D)中之M
1~M
7較佳為分別獨立地選自由氫原子、鈉、鋰、鉀、鎂、銨、三乙醇胺及精胺酸所組成之群。
M
1~M
7更佳為分別獨立地選自由氫原子、鈉、鋰、鉀、鎂、銨、三乙醇胺及精胺酸所組成之群,M
1~M
7之至少1者為氫,M
1~M
7之至少1者選自由鈉、鋰、鉀、鎂、銨、三乙醇胺及精胺酸所組成之群。
M
1~M
7進而較佳為分別獨立地為氫或鈉,M
1~M
7之至少1者為氫,M
1~M
7之至少1者為鈉。
[組合物之製造方法]
本實施方式之組合物(特別是香妝品原料組合物)之製造方法包括如下步驟。
1)[第一步驟]於包含水及有機溶劑之混合溶劑中,使麩胺酸或其鹽與脂肪醯氯進行反應,獲得包含N-醯基麩胺酸或其鹽之反應液,利用酸使上述反應液之pH值成為1~6,於25~80℃之溫度下分層為有機層與水層。
2)[第二步驟]於酸性下對上述有機層進行濃縮乾燥,將上述N-醯基麩胺酸或其鹽之一部分轉化為N-醯基吡咯啶酮羧酸或其鹽(成分B)。
3)[第三步驟]使上述N-醯基麩胺酸或其鹽與酸酐進行反應,而獲得N-醯基麩胺酸酐。
4)[第四步驟]使上述N-醯基麩胺酸酐與離胺酸或其鹽進行反應,而獲得含有醯基之胺基酸衍生物或其鹽(成分A)。
[第一步驟]
本實施方式之醯化反應步驟係於水與例如第三丁醇、丙酮、甲基乙基酮、異丙醇等有機溶劑之混合溶劑中,在鹼性化合物之存在下,使麩胺酸與脂肪醯氯進行縮合反應之步驟,藉由醯化反應,生成粗N-醯基麩胺酸。
於醯化反應步驟中,脂肪醯氯相對於麩胺酸之莫耳比較佳為1.05以下,更佳為1.0以下,進而較佳為0.98以下。藉由使脂肪醯氯相對於麩胺酸之莫耳比為1.05以下,有容易降低游離脂肪酸之生成量之趨勢。
於醯化反應步驟中,作為混合溶劑之組成,水/有機溶劑之容量比較佳為90/10~20/80之範圍,更佳為85/15~50/50之範圍。藉由使上述容量比為90/10~20/80之範圍,麩胺酸、脂肪醯氯及鹼性化合物3者容易相溶,可提昇反應速度。
醯化反應步驟中之麩胺酸之添加濃度並無特別限定,由於反應中反應液之黏度隨時間上升,故而較佳為調整為於接近反應結束之時間點可攪拌混合之程度之添加濃度。
醯化反應步驟之反應溫度並無特別限定,就促進主反應及抑制副反應之觀點而言,較佳為-10~70℃之範圍,更佳為-10~20℃之範圍,進而較佳為-5~10℃之範圍。
醯化反應步驟所使用之鹼性化合物並無特別限制,例如可例舉氫氧化鈉、氫氧化鉀、氫氧化鈣、氫氧化鋇等無機鹼。
就促進主反應及抑制副反應之觀點而言,醯化反應步驟中之pH值較佳為維持於9~13.5,更佳為維持於10~13之範圍。
例如利用如鹽酸、硫酸之酸(較佳為礦酸)使醯化反應液之pH值成為1~6,分離為有機層與水層之二層,獲得有機層。於醯化反應液中,所生成之N-醯基麩胺酸以鹼金屬鹽之形式存在。藉由向其中添加酸,使N-醯基麩胺酸中之羧基之一部分或全部成為游離酸,從而分層為有機層與水層(酸沈澱步驟)。由於酸沈澱時之pH值,羧基之解離狀態改變,分層狀態即有機層與水層之質量比或無機鹽類之去除性稍微改變,故而較佳為於pH值為1~3下實施,更佳為pH值為1~2.5。
酸沈澱步驟中之溫度較佳為25~80℃。更佳為40~70℃。藉由使該溫度為25℃以上,有可縮短達到分層平衡之時間,且可減少達到平衡時有機層中之無機鹽之殘存量之趨勢。
[第二步驟]
本發明形態之第二步驟係於酸性下對第一步驟所獲得之有機層進行濃縮乾燥,將N-醯基麩胺酸之一部分轉化為N-醯基吡咯啶酮羧酸(成分B)。濃縮乾燥較佳為進行加溫且於常壓下或減壓下實施。實施濃縮乾燥直至乾燥減量達到較佳為10質量%以下、更佳為3質量%以下、進而較佳為1質量%以下為止。由於在下一步驟中會對醯基麩胺酸進行酐化,故而為了減少水分,乾燥減量越少為好。
於本說明書中,「乾燥減量」意指因乾燥而減少之質量之比率。具體而言,為將1 g試樣於105℃下乾燥了3小時之時所減少之質量的比率,可利用下述式算出。
乾燥減量(%)=[{初始試樣質量(g)-乾燥試樣質量(g)}/初始試樣質量(g)]×100
濃縮乾燥較佳為於常壓下或減壓下,首先於較有機溶劑之沸點附近高之溫度或所使用之有機溶劑與水之共沸點附近,將有機溶劑及水蒸餾去除。若有機溶劑相對於水之質量比實質上成為3%以下,則共存之醯基麩胺酸容易發泡,因此需要於加熱時小心地控制減壓。即便將有機溶劑大致蒸餾去除,仍殘存有水分,作為實質操作,可於水之沸點附近繼續進行減壓。上述操作與在設定溫度下持續靜置之冷凍乾燥方法相比,需要控制發泡即適應發泡狀況之緩慢攪拌,但在醯基麩胺酸約為10質量%以下且於85℃以上之高溫下,可副產適量之醯基PCA,其有助於配方系統中之乳化性或分散性。
於該步驟中,例如操作使用冷凍乾燥處理。處理過程中幾乎不產生發泡,乾燥操作上無任何人為實施,故而簡便,但未觀察到醯基PCA。
若醯基麩胺酸相對於主體之有機物,乾燥減量減少,則發泡收斂。於極限減壓度200 kPa下,將極限溫度85℃以上維持20分鐘以上時,乾燥減量達到10質量%以下。
於欲更有效率地減少乾燥減量之情形時,極限減壓度較佳為50 kPa以下,更佳為20 kPa以下。極限溫度亦取決於醯基麩胺酸之熔點及減壓度,較理想為70℃以上,更佳為95℃以上,進而較佳為105℃以上。
藉由將乾燥減量設為10質量%以下,可由醯基麩胺酸副產成分B(醯基PCA)。
[第三步驟]
使如乙酸酐之羧酸酐與第二步驟所獲得之醯基麩胺酸主體之固形物進行反應,由所獲得之反應液進行過濾分離、乾燥,可獲得醯基麩胺酸酐主體之粗結晶。
此處,較佳之脫水劑為如乙酸酐之羧酸酐,就經濟性及環境性觀點而言,較佳為使用乙酸酐。對醯基麩胺酸進行酐化之反應後,藉由過濾分離去除過量之乙酸酐及乙酸。為了提昇醯基麩胺酸酐之純度,利用醚、繼而石油醚進行洗淨,其後,使其乾燥而可獲得該醯基麩胺酸酐主體之固形物。
[第四步驟]
按照日本專利第4070768號公報,以離胺酸成為1莫耳當量之方式,使第三步驟所獲得之醯基麩胺酸酐主體之固形物與2莫耳當量之醯基麩胺酸酐進行反應,可製作如下述所示之主成分為通式(A)所表示之含有醯基之胺基酸衍生物之水溶液。
本發明之香妝品係日本醫藥品與醫療器械法令中所謂之準藥品及化妝品之總稱,具體而言,作為準藥品,可例舉口腔清涼劑、腋臭防止劑、爽身粉類、養髮劑、脫毛劑、染毛劑、燙髮用劑、沐浴液、藥用化妝品、藥用牙膏類等,作為化妝品,可例舉:香皂、洗面乳(乳霜、糊狀,液體、凝膠狀,顆粒、粉末狀,霧劑用途等)、洗髮精、潤絲精等清潔用化妝品;染髮劑、頭髮護理劑(包括乳霜狀、霧狀、油狀、凝膠狀等形態者及毛髮分叉修復劑)、定髮劑(髮油、頭髮定型液、捲髮液、髮膏、髮蠟、鬢髮油、造型噴霧、髮妝水噴霧、整髮液、造型泡沫、髮膠、水性髮膏(water grease))等頭髮用化妝品;一般乳霜、乳液(潔面霜、冷霜、雪花膏(vanishing cream)、護手霜等)、剃鬚用乳霜(鬚後霜、剃鬚膏等)、化妝水(護手露、一般化妝水等)、古龍水、剃鬚用乳液(鬚後水、剃鬚液(shaving lotion)等)、化妝油、面膜等基礎化妝品;散粉(散粉霜、固體散粉、粉狀散粉、撲粉(talcum powder)、散粉膏、嬰兒爽身粉、香體粉、散粉液等)、撲面粉、粉底(乳霜狀、液態、固體等)、腮紅、眉筆、眼霜、眼影、睫毛膏等彩妝化妝品;一般香水、固體香膏、粉末香水等香水類;凝膠型、液體型、陶器型等之芳香劑、消臭劑、除臭劑;防曬霜、防曬乳液、防曬油等防曬化妝品;指甲霜、指甲油、指甲油卸除液等指甲化妝品;眼線化妝品;口紅、唇膏等唇部化妝品;牙膏等口腔化妝品;浴鹽、沐浴油、泡沫浴液等沐浴用化妝品等。
本實施方式之香妝品原料組合物中,除成分A及成分B~成分E以外,只要不損及本發明之目的,就可根據用途、目的與各種基材併用。
具體而言,可包括:阿拉伯膠、黃耆膠等天然橡膠類、皂苷等葡萄糖苷類、甲基纖維素、羧基纖維素、羥甲基纖維素等纖維素衍生物、木質素磺酸鹽、蟲膠等天然高分子、聚丙烯酸鹽、苯乙烯-丙烯酸共聚物之鹽、乙烯基萘-馬來酸共聚物之鹽、β-萘磺酸福馬林縮合物之鈉鹽、磷酸鹽等陰離子性高分子或聚乙烯醇、聚乙烯吡咯啶酮、聚乙二醇等非離子性高分子等分散劑;
高級脂肪酸鹽(肥皂)、疏水基部之碳數8~20之高級脂肪酸之鹽、N-醯基胺基酸型陰離子界面活性劑:作為醯基,可例舉碳數為8~20且如上述者,作為構成胺基酸:麩胺酸或天冬胺酸等上述酸性胺基酸類、或甘胺酸、丙胺酸、纈胺酸、白胺酸、異白胺酸、脯胺酸、甲硫胺酸、半胱胺酸、色胺酸、酪胺酸、苯丙胺酸、天冬醯胺、麩醯胺、絲胺酸、蘇胺酸、羥基脯胺酸、β-胺基丙酸、γ-胺基丁酸、鄰胺苯甲酸、間胺基苯甲酸、對胺基苯甲酸等胺基酸等、烷基醚羧酸鹽、醯胺基醚羧酸鹽等、烷基硫酸酯鹽(AS)、聚氧乙烯烷基醚硫酸酯鹽(AES)、烷基醚硫酸鹽、高級脂肪酸酯之硫酸鹽、高級脂肪酸羥烷基醯胺之硫酸鹽、硫酸化油脂、聚氧乙烯苯乙烯化苯醚硫酸鹽、α-烯烴磺酸鹽(AOS)、烷基苯磺酸鹽、烷基萘磺酸鹽、烷基磺酸鹽(SAS)、二烷基磺基琥珀酸鹽、α-磺化脂肪酸鹽、烷磺酸鹽、高級脂肪酸酯之磺酸鹽、α-磺化脂肪酸鹽、高級脂肪酸醯胺之磺酸鹽、N-醯基-N-烷基牛磺酸鹽、N-醯基-N-甲基牛磺酸鹽、烷基磷酸鹽、烷基醚磷酸鹽、聚氧乙烯烷基醚磷酸鹽、聚氧乙烯烷基苯醚磷酸鹽、萘磺酸鹽福馬林縮合物等陰離子性界面活性劑;
烷基甜菜鹼類、烷基醯胺甜菜鹼類、烷基磺基甜菜鹼類、咪唑啉鎓甜菜鹼類、乙酸甜菜鹼類、卵磷脂類等兩性界面活性劑;
聚氧乙烯烷基醚(AE)、聚氧乙烯烷基苯醚、聚氧乙烯聚苯乙烯基苯醚、聚氧乙烯聚氧丙烯二醇、聚氧乙烯聚氧丙烯烷基醚、聚氧伸烷基脂肪酸酯、聚氧伸烷基山梨醇酐脂肪酸酯、聚氧伸烷基脂肪酸烷醇醯胺、聚氧伸烷基烷基葡萄糖苷、聚氧伸烷基氫化蓖麻油、聚氧伸烷基烷基胺、聚氧伸烷基烷基苯醚等氧化乙烯縮合型、多元醇脂肪酸部分酯、聚氧乙烯多元醇脂肪酸部分酯、聚氧乙烯脂肪酸酯、(聚)甘油脂肪酸酯、聚氧乙烯氫化蓖麻油、聚氧乙烯烷基胺、三乙醇胺脂肪酸部分酯、烷基聚葡萄糖苷、丙二醇脂肪酸酯、山梨醇酐脂肪酸酯、蔗糖脂肪酸酯等多元醇酯、脂肪酸烷醇醯胺、糖胺醯化物、三乙醇胺脂肪酸部分酯、脂肪酸羥烷基醯胺、烷基氧化胺等非離子性界面活性劑;
一~三級脂肪酸胺鹽、氯化烷基銨鹽、四烷基銨鹽、三烷基苄基銨鹽、烷基吡啶鎓鹽、烷基羥基乙基咪唑啉鎓鹽、二烷基嗎啉鎓鹽、烷基異喹啉鎓鹽、苯銨松寧鹽、苄烷銨鹽等陽離子性界面活性劑;
海藻酸鈉、澱粉衍生物、黃耆膠等高分子界面活性劑;
磷脂質、卵磷脂、羊毛脂、膽固醇、皂苷等天然界面活性劑;
鱷梨油、龜油、玉米油、杏仁油、橄欖油、可可油、芝麻油、紅花油、大豆油、山茶油、桃仁油、蓖麻油、葡萄籽油、澳洲胡桃油、貂油、棉籽油、木蠟、椰子油、蛋黃油、棕櫚油、棕櫚仁油、三異辛酸甘油酯、三(2-乙基)己酸甘油酯、膽固醇脂肪酸酯、小麥胚芽油、山茶花油、亞麻籽油、月見草油、紫蘇油、花生油、茶籽油、榧子油、米糠油、中國桐油、日本桐油、荷荷芭油、胚芽油、三辛酸甘油酯、三異棕櫚酸甘油酯、馬油、氫化椰子油、牛油、牛蹄油、羊油、氫化牛油、豬油、牛骨油、木蠟核油、氫化油、木蠟、氫化蓖麻油等油脂;
液態石蠟、凡士林、地蠟、微晶蠟、異構石蠟、地蠟、角鯊烯、姥鮫烷、角鯊烷等烴;
蜂蠟、鯨蠟、羊毛脂、巴西棕櫚蠟、堪地里拉蠟、棉蠟、月桂果蠟、蟲蠟、褐煤蠟、米糠蠟、羊毛脂、木棉蠟、乙酸羊毛脂、液態羊毛脂、甘蔗蠟、羊毛脂脂肪酸異丙酯、月桂酸己酯、還原羊毛脂、荷荷芭蠟、硬質羊毛脂、蟲膠蠟、聚氧乙烯羊毛醇醚、聚氧乙烯羊毛醇乙酸酯、羊毛脂脂肪酸聚乙二醇、聚氧乙烯氫化羊毛醇醚及其衍生物等蠟;
月桂酸、肉豆蔻酸、棕櫚酸、硬脂酸、異硬脂酸、油酸、山萮酸、十一碳烯酸、羊毛脂脂肪酸、硬質羊毛脂脂肪酸、軟質羊毛脂脂肪酸、亞麻油酸、次亞麻油酸、二十碳五烯酸、12-羥基硬脂酸等脂肪酸;
月桂醇、鯨蠟醇、鯨蠟硬脂醇、硬脂醇、油醇、山萮醇、羊毛醇、氫化羊毛醇、己基癸醇、辛基十二烷醇等高級醇;
膽固醇、植固醇等固醇類;
肉豆蔻酸異丙酯、硬脂酸丁酯、辛酸鯨蠟酯、肉豆蔻酸辛基十二烷基酯、棕櫚酸異丙酯、月桂酸己酯、肉豆蔻酸肉豆蔻酯、油酸癸酯、二甲基辛酸己基癸酯、乳酸鯨蠟、乳酸肉豆蔻酯、羊毛脂乙酸酯、硬脂酸異鯨蠟、異硬脂酸異鯨蠟酯、12-羥基硬脂酸膽固醇酯、二-2-乙基己酸乙二醇酯、二季戊四醇脂肪酸酯、N-烷基二醇單異硬脂酸、二癸酸新戊二醇酯、蘋果酸二異硬脂酯、二-2-庚基十一酸甘油酯、三-2-乙基己酸三羥甲基丙酯、三異硬脂酸三羥甲基丙酯、四-2-乙基己酸季戊四醇酯、三-2-乙基己酸甘油酯、三異硬脂酸三羥甲基丙酯、2-乙基己酸鯨蠟酯、棕櫚酸2-乙基己酯、三肉豆蔻酸甘油酯、三-2-庚基十一酸甘油酯、蓖麻油脂肪酸甲酯、油酸油酯、鯨蠟硬脂醇、乙酸甘油酯、棕櫚酸-2-庚基十一烷基酯、己二酸二異丙酯、N-月桂醯-L-麩胺酸-2-辛基十二烷基酯、己二酸二-2-庚基十一烷基酯、月桂酸乙酯、癸二酸二-2-乙基己酯、肉豆蔻酸-2-己基癸酯、棕櫚酸-2-己基癸酯、己二酸-2-己基癸酯、癸二酸二異丙酯、琥珀酸-2-乙基己酯、乙酸乙酯、乙酸丁酯、乙酸戊酯、檸檬酸三乙酯等酯油;
二甲基聚矽氧烷、聚醚改性聚矽氧、醇改性聚矽氧、甲基苯基聚矽氧烷、環氧改性聚矽氧、氟改性聚矽氧、烷基改性聚矽氧、烷氧基改性聚矽氧、胺基改性聚矽氧、高分子聚矽氧、揮發性聚矽氧、環狀聚矽氧等揮發性及非揮發性聚矽氧;
甘油、雙甘油、聚甘油、1,3-丁二醇、丙二醇、聚乙二醇等多元醇類;
N-甲基甘胺酸、N,N-二甲基甘胺酸、N,N,N-三甲基甘胺酸、N-乙基甘胺酸、甘胺醯甜菜鹼等烷基甘胺酸類、山梨糖醇、棉子糖、吡咯啶酮羧酸鹽類、乳酸鹽類、玻尿酸鹽類、神經醯胺類、海藻糖、木二糖、麥芽糖、蔗糖、葡萄糖、植物性黏質多糖等(多)糖類及其衍生物、水溶性甲殼素、聚葡萄胺糖、果膠、硫酸軟骨素及其鹽等葡糖胺聚醣及其鹽、甘胺酸、絲胺酸、蘇胺酸、丙胺酸、天冬胺酸、酪胺酸、纈胺酸、白胺酸、精胺酸、麩胺酸、脯胺酸等胺基酸及其鹽等、胺基羰基反應物等糖胺基酸化合物、蘆薈、七葉樹等植物萃取液、尿素、尿酸、氨、葡萄糖胺、肌酸酐、DNA(Deoxyribonucleic Acid,去氧核糖核酸)、RNA(Ribonucleic Acid,核糖核酸)等核酸關連化合物等保濕劑;
羥乙基纖維素、羧甲基纖維素、羥乙基纖維素羥丙基三甲基氯化銨醚、甲基纖維素、乙基纖維素、羥丙基纖維素、甲基羥丙基纖維素、可溶性澱粉、羧甲基澱粉、甲基澱粉、海藻酸丙二醇酯、聚乙烯醇、聚乙烯吡咯啶酮、聚乙烯基甲醚、羧基乙烯基聚合物、聚丙烯酸鹽、瓜爾膠、刺槐豆膠、榅桲籽、鹿角菜膠、聚半乳糖、阿拉伯膠、果膠、甘露聚醣、澱粉、三仙膠、葡聚糖、琥珀醯聚糖、卡德蘭多糖、玻尿酸、明膠、酪蛋白、白蛋白、膠原蛋白、甲氧基乙烯馬來酸酐共聚物共聚物、兩性甲基丙烯酸酯共聚物、聚氯化二甲基亞甲基哌啶鎓、聚丙烯酸酯共聚物、聚乙酸乙烯酯、硝化纖維素、聚矽氧樹脂等水溶性及油溶性高分子;
陽離子化纖維素衍生物、陽離子性澱粉、陽離子化瓜爾膠衍生物、二烯丙基四級銨鹽/丙烯醯胺共聚物、四級化聚乙烯吡咯啶酮衍生物、四級化乙烯基吡咯啶酮/乙烯基咪唑聚合物、聚二醇/胺縮合物、四級化膠原蛋白多肽、聚伸乙基亞胺、陽離子性聚矽氧聚合物、己二酸/二甲基胺基羥丙基二伸乙基三胺共聚物、聚胺聚醯胺、陽離子性甲殼素衍生物、四級化聚合物等陽離子性高分子、聚乙二醇脂肪酸酯、聚氧乙烯脂肪酸酯甲基糖苷、十四烯磺酸鹽等增黏、增泡成分;
糊精脂肪酸酯、甘油脂肪酸酯、羥基硬脂酸等油膠化劑;
乙二胺四乙酸及其鹽類、羥基乙二胺三乙酸及其鹽類、磷酸、抗壞血酸、琥珀酸、葡萄糖酸、多磷酸鹽類、偏磷酸鹽、檜木醇類等金屬離子螯合劑;
對羥基苯甲酸酯類、苯甲酸及其鹽類、苯氧基乙醇、檜木醇、水楊酸及其鹽類、山梨酸及其鹽、去氫乙酸及其鹽、對氯間甲酚、六氯酚、硼酸、間苯二酚、三溴沙侖(Tribromsalan)、鄰苯基苯酚、福美雙(thiram)、感光素201、鹵卡班、三氯對稱二苯脲、乙酸維生素E酯、吡啶硫酮鋅、苯酚、異丙基甲基苯酚、2,4,4-三氯-2-羥基苯酚、六氯酚、雙氯苯雙胍己啶、苄索氯銨、氯化苄烷銨、西吡氯銨、地喹氯銨、氯化硬脂基二甲基銨、氯化硬脂基三甲基銨、氯化鯨蠟基三甲基銨、甲基苄索氯銨、氯化月桂基三甲基銨、拉吡氯銨、三氯沙、幽樂錠(Biozole)等防腐、抗菌劑;
檸檬酸、蘋果酸、己二酸、麩胺酸、天冬胺酸等pH調整劑;
以及三氯對稱二苯脲、水楊酸、吡啶硫酮鋅、異丙基甲基苯酚等抗頭屑劑、止癢劑;
二苯甲酮衍生物、對胺基苯甲酸衍生物、對甲氧基肉桂酸衍生物、水楊酸衍生物等紫外線吸收劑;
抗壞血酸及其鹽(除如鈉鹽、鉀鹽、鎂鹽、鈣鹽之鹼金屬鹽或鹼土類金屬鹽以外,還有銨鹽、胺基酸鹽等)、抗壞血酸衍生物(L-抗壞血酸烷基酯、L-抗壞血酸磷酸酯及其鹽、L-抗壞血酸-2-硫酸酯及其鹽、L-抗壞血酸葡萄糖苷等)、烷氧基水楊酸及其鹽(烷氧基例如為甲氧基、乙氧基、丙氧基、異丙氧基、丁氧基、異丁氧基等)、對苯二酚糖苷及其衍生物(熊果苷等)、麴酸及其衍生物、土耳其鞣酸、德國甘菊萃取物、蜀葵萃取物、甘草萃取物、桑白皮萃取物、樹莓萃取物、蘋果類黃酮、麥麩萃取物、維生素E及其衍生物、檜木醇、胎盤萃取物、白藜蘆醇、香菊ET、麩胱甘肽、丁香萃取物、茶萃取物、蝦紅素、牛胎盤萃取物、傳明酸及其衍生物、間苯二酚之衍生物、甘菊藍、γ-羥丁酸等美白劑;
當藥萃取物、頭花千金藤鹼、維生素E及其衍生物、γ-穀維素等血液循環促進劑;
辣椒酊、薑酊、斑蝥酊、菸鹼酸苄酯等局部刺激劑;
各種維生素或胺基酸等營養劑;
雌性激素劑;
髮根活化劑;
甘草次酸、甘草酸衍生物、尿囊素、甘菊藍、胺基己酸、氫化可體松等抗炎劑;
氧化鋅、硫酸鋅、尿囊素羥基鋁、氯化鋁、硫酸鋁、磺基石碳酸鋅(zinc sulfocarbolate)、單寧酸、檸檬酸、乳酸等收斂劑;
薄荷腦、樟腦等清涼劑;
鹽酸苯海拉明、馬來酸氯苯那敏、甘草酸衍生物等抗組織胺劑;
生育酚類、BHA(butyl hydroxy anisol,丁基羥基茴香醚)、BHT(Butylated Hydroxy Toluene,二丁基羥基甲苯)、沒食子酸、NDGA(nordihydroguaiaretic acid,正二氫愈創酸)等抗氧化劑;
雌二醇、雌酮、乙炔雌二醇等皮脂抑制劑;
硫、水楊酸、間苯二酚等角質剝離、溶解劑;
乙醇酸、乳酸、蘋果酸、酒石酸、檸檬酸等α-羥酸;
水楊酸等β-羥酸;
滑石、高嶺土、絹雲母、碳酸鈣、氧化鋅、氧化鋁、氧化鎂、氧化鋯、碳酸鎂、碳酸鈣、硫酸鋇、氧化鉻、氫氧化鉻、焦油系色素等、雲母、(合成)絹雲母、碳化矽、氮化硼、二氧化鈦、氧化鈦黑、普魯士藍、氧化鐵紅、氧化鐵黑、氧化鐵黃、群青、鈦被覆雲母(titanium coated mica)、氧氯化鉍、鐵丹、黏結顏料、群青粉紅(Ultramarine Pink)、群青紫、氫氧化鉻、雲母鈦、氧化鉻、氧化鋁鈷、碳黑、矽酸酐、矽酸鎂、膨潤土、(合成)雲母、氧化鋯、矽酸鋁鎂、鋁矽酸鈣、聚乙烯粉末、尼龍粉末、聚甲基丙烯酸甲酯、聚對苯二甲酸乙二酯-聚甲基丙烯酸甲酯積層粉末、丙烯腈-甲基丙烯酸共聚粉末、偏二氯乙烯-甲基丙烯酸共聚粉末、羊毛粉(Wool powder)、蠶絲粉、結晶纖維素、N-醯基離胺酸、聚甲基倍半矽氧烷粉末、使植物之籽或皮成為粉末狀而得者、氧氯化鉍、雲母鈦、氧化鐵被覆雲母、氧化鐵雲母鈦、有機顏料處理雲母鈦、鋁粉、微粒子氧化鈦、微粒子氧化鋅、微粒子氧化鈦被覆雲母鈦、微粒子氧化鋅被覆雲母鈦、硫酸鋇被覆雲母鈦、洋紅、β-胡蘿蔔素、金屬皂、葉綠素、日落黃FCF、麗春紅SX、曙紅YS、四溴螢光素、玫瑰紅B、喹啉黃SS、喹啉黃WS、茜素花青綠、溶劑綠、立索爾寶紅B、立索爾寶紅BCA、紅色4號(Permaton Red)、赫林頓粉紅CN、酞菁藍、β-衍-8-胡蘿蔔素醛(β-Apo-8-carotenal)、辣椒紅素、riroppy、胭脂素、藏花素、斑螫黃素、紫蘇素、萊菔素、尼諾花菁素(ninocyanine)、紅花素、黃樟素(Safrole)、芸香苷、槲皮素、可可色素、核黃素(riboflavin)、蟲漆酸、洋紅酸、胭脂紅酸(kermesic acid)、茜素、紫草寧、紫草素(Alkannin)、尼奇諾絡(nichinochrome)、血色素、薑黃素、甜菜苷(betanin)等化妝品用有色材料:
純化水、以及火棘萃取物、N-甲基-L-絲胺酸、乳清、菸鹼醯胺、二異丙胺二氯乙酸、甲基二羥戊酸、γ-胺基丁酸(包括γ-胺基-β-羥丁酸)、蜀葵萃取物、蘆薈萃取物、杏仁萃取物、薑黃萃取物、烏龍茶萃取物、海水乾燥物、水解小麥粉、水解蠶絲、胡蘿蔔萃取物、青瓜萃取物、龍膽萃取物、酵母萃取物、米胚芽油、康富力萃取物、肥皂草萃取物、地黃萃取物、紫根萃取物、白樺萃取物、胡椒薄荷萃取物、當藥萃取物、甜沒藥醇、蜂膠、絲瓜萃取物、菩提樹萃取物、啤酒花萃取物、七葉樹萃取物、無患子萃取物、蜜蜂花萃取物、桉樹萃取物、虎耳草萃取物、迷迭香萃取物、羅馬洋甘菊萃取物、蜂王漿萃取物、海草、米糠、甘草、陳皮、當歸、桃葉之粉碎物、鞘脂、愈創薁、維生素C等。
[實施例]
以下,使用實施例及比較例進一步對本發明進行詳細說明,但本發明之技術範圍並不限定於此。
再者,實施例中之各種值可設為本發明之實施方式中之較佳之下限值或上限值,亦可與上述本發明之實施方式中之同種值(包括數值範圍之下限值及上限值)適宜地組合而設為較佳之數值範圍。又,還可將實施例中之同種之2個值適宜地組合而設為較佳之數值範圍。
[製造例1]
向104 g(0.56 mol)之L-麩胺酸單鈉一水合物、265.2 g之純水、69.6 g之32%氫氧化鈉水溶液(以氫氧化鈉計,為0.56 mol)之混合溶液中添加93.2 g之87質量%第三丁醇水溶液,將該溶液維持於3℃,並且利用32%氫氧化鈉將pH值調整為12,同時於攪拌下滴加117.8 g(0.54 mol)之月桂醯氯。
繼而,滴加75%硫酸而將液體之pH值調整為2,又,將液體之溫度調整為65℃,靜置1小時而分層為有機層與水層後,分取有機層。
此時之有機層中之以月桂醯基麩胺酸為主體之固形物成分/第三丁醇/水之成分重量比為62/24/14。
[製造例2]
向104 g(0.56 mol)之L-麩胺酸單鈉一水合物、145.8 g之純水、69.6 g之32%氫氧化鈉水溶液(以氫氧化鈉計,為0.56 mol)之混合溶液中添加126 g之丙酮,將該溶液維持於3℃,並且利用32%氫氧化鈉將pH值調整為12,同時於攪拌下滴加117.8 g(0.54 mol)之月桂醯氯。
繼而,滴加75%硫酸而將液體之pH值調整為2,又,將液體之溫度調整為50℃,靜置1小時而分層為有機層與水層後,分取有機層。
此時之有機層中之以月桂醯基麩胺酸為主體之固形物成分/丙酮/水之成分重量比為55/30/15。
[製造例3]
向104 g(0.56 mol)之L-麩胺酸單鈉一水合物、265.2 g之純水、69.6 g之32%氫氧化鈉水溶液(以氫氧化鈉計,為0.56 mol)之混合溶液中添加93.2 g之87質量%第三丁醇水溶液,將該溶液維持於3℃,並且利用32%氫氧化鈉將pH值調整為12,同時於攪拌下滴加26.6 g(0.11 mol)之肉豆蔻醯氯,繼而於攪拌下滴加94.2 g(0.43 mol)之月桂醯氯。
繼而,滴加75%硫酸而將液體之pH值調整2,又,將液體之溫度調整為65℃,靜置1小時而分層為有機層與水層後,分取有機層。
此時之有機層中之以醯基麩胺酸(月桂醯基麩胺酸及肉豆蔻醯基麩胺酸)為主體之固形物成分/第三丁醇/水之成分重量比為62/27/11。
<HPLC分析法>
於下述包含成分B之實施例及比較例中,成分A、成分B根據下述藉由使用HPLC之分析而獲得之波峰區域面積進行測定。
檢測器:UV(ultraviolet,紫外線)檢測器(205 nm)
測定機器例如可使用島津製作所股份有限公司之SPD-10Avp、SPD-10AVvp、SPD-20A及SPD-20AV等。
分離管:向內徑6 mm、長度150 mm之不鏽鋼管中填充於粒徑5 μm、孔徑12 nm之矽膠上修飾有十八烷基矽烷基者。
分離管溫度:60℃左右之一定溫度
流動相:甲醇/水/磷酸=2000/400/0.31
流量:每分鐘0.8 mL左右之一定量
更具體而言,根據藉由使用HPLC之分析而獲得之成分A、成分B等所檢測出之物質各者之波峰區域面積,算出成分比。自總成分比100%中,首先減去所獲得之乾燥減量,以利用HPLC分析所獲得之波峰面積比分配該減去後之值。另外,以下式算出成分B比率(%)。相當於下述表中之「成分B比率(%)」。
成分B比率(%)=[成分B之波峰區域面積/成分A之波峰區域面積]×100
若如上所述使用UV檢測,則醯基PCA(成分B)之波峰感度高於其他物質,故而於成分B(%)比率下亦可保持較高之測定感度。
[實施例1]
一面緩慢攪拌100 g之製造例1所獲得之月桂醯基麩胺酸等固形物成分/第三丁醇/水之成分重量比為62/24/14之有機層,一面於常壓下使其升溫直至液溫達到90℃為止。其後,一面慢慢減壓,一面使其升溫,緩慢提昇減壓度以免過度發泡,於極限減壓度20 kPa下,將極限溫度105℃維持20分鐘。其後,緩慢恢復至常壓,回收釜內之熔融物。將所獲得之固形物於冷藏庫中放置一夜,利用榨汁攪拌器進行粉碎,結果獲得56.6 g之固形物。該固形物之乾燥減量為0.25%,經HPLC分析,結果,月桂醯基麩胺酸為94.9%,月桂醯基PCA為3.7%,月桂酸為0.44%。未檢測出其他明顯之雜質。
於50℃下使54.0 g之該固形物溶解於36.4 g之乙酸酐中,進而添加18.2 g之乙酸酐,直接於50℃下反應3小時。其後,冷卻至室溫,自反應液中過濾分離出產物,藉此,獲得以N-月桂醯基-L-麩胺酸酐為主體之粗結晶。對於該結晶,利用80 ml之醚,繼而利用15 ml之石油醚,對其進行洗淨、乾燥,而獲得34.0 g之固形物。該固形物之乾燥減量為0.24%,經HPLC分析,結果,月桂醯基麩胺酸酐為95.2%,月桂醯基PCA為2.3%,月桂醯基麩胺酸為2.2%,未檢測出月桂酸。未檢測出其他明顯之雜質。
進而,將9.1 g(0.05 mol)之L-離胺酸鹽酸鹽與57 g之水加以混合。利用25%氫氧化鈉水溶液將該液體之pH值範圍調整為10~11,又,將反應溫度維持於5℃,並且於攪拌下歷時2小時添加31.1 g之上述經洗淨、乾燥而獲得之固形物,實施反應。進而繼續攪拌30分鐘後,以液中濃度成為20質量%之方式添加第三丁醇後,滴加75%硫酸而將液體之pH值調整為2,又,將液體之溫度調整為65℃。滴加結束後,停止攪拌,於65℃下靜置20分鐘,則分層為有機層與水層,自其中分離出有機層。未反應之離胺酸幾乎被水層回收。對所獲得之有機層反覆進行相同之水洗操作後,自所獲得之有機層中去除溶劑,利用氫氧化鈉以成為固形物成分為30質量%、pH值為7(25℃)之水溶液之方式進行中和製備。進而,一面添加水,一面進行減壓蒸餾,對第三丁醇於減壓度13~22 kPa、液溫45~60℃下繼續進行減壓蒸餾直至液中濃度達到10質量ppm以下為止。最終所獲得者為以含有式(A)所示之醯基化合物之組合物為主體之pH值為7(25℃)之32重量%水溶液,成分A為96.9%,成分B之醯基PCA為0.031%,月桂醯基麩胺酸為2.98%。未檢測出其他明顯之雜質。上述利用HPLC分析法所得之醯基PCA(%)比率為0.032%。
[比較例1]
對100 g之製造例1所獲得之月桂醯基麩胺酸等固形物成分/第三丁醇/水之成分重量比為62/24/14之有機層進行冷凍乾燥。
進行預冷凍,即,將櫃循環溫度設定為-60℃,試樣溫度達到-40℃後,冷卻2小時。將櫃循環溫度設定為-40℃,乾燥2小時後,設定為-10℃,大致於5 Pa下進行乾燥。其後,將設定溫度提昇至0℃、10℃、30℃。
確認容器內溫度為27.5℃、極限真空度為1 Pa以下後,利用乾燥氮氣解除真空。實施以上之乾燥步驟所需之時間為40小時。所獲得之固形物為平板狀,利用榨汁攪拌器將其粉碎,獲得57.1 g之固形物。該固形物之乾燥減量為1.2%,經HPLC分析,結果,月桂醯基麩胺酸為98.1%,未檢測出月桂醯基PCA,月桂酸為0.40%。未檢測出其他明顯之雜質。
於50℃下使54.0 g之該固形物溶解於36.4 g之乙酸酐中,進而添加18.2 g之乙酸酐,直接於50℃下反應3小時。其後,冷卻至室溫,自反應液中過濾分離出產物,藉此,獲得N-月桂醯基-L-麩胺酸酐之粗結晶。對於該結晶,利用80 ml之醚,繼而利用15 ml之石油醚,對其進行洗淨、乾燥,而獲得34.3 g之固形物。該固形物之乾燥減量為1.2%,經HPLC分析,結果,月桂醯基麩胺酸酐為96.6%,月桂醯基麩胺酸為2.1%,未檢測出月桂醯基PCA及月桂酸。未檢測出其他明顯之雜質。
進而,將9.1 g(0.05 mol)之L-離胺酸鹽酸鹽與57 g之水加以混合,之後,利用與實施例1相同之方法繼續製作成分A,結果,獲得以含有成分A之組合物為主體之pH值為7(25℃)之32重量%水溶液。此時,成分A為97.1%,月桂醯基麩胺酸為2.62%。未檢測出月桂醯基PCA及月桂酸,亦未檢測出其他明顯之雜質。利用HPLC分析法所得之醯基PCA(%)比率為0%。
[實施例2]
一面緩慢攪拌115.0 g之製造例2所獲得之月桂醯基麩胺酸等固形物成分/丙酮/水之成分重量比為55/30/15之有機層,一面於常壓下使其升溫直至液溫達到50℃為止。其後,一面慢慢減壓,一面使其升溫,緩慢提昇減壓度以免過度發泡,於極限減壓度為20 kPa下,達到極限溫度105℃。於極限減壓度為20 kPa下,將極限溫度105℃維持80分鐘。其後,緩慢恢復至常壓,回收釜內之熔融物。自濃縮開始後至結束需要10小時。將所獲得之固形物於冷藏庫中放置一夜,利用榨汁攪拌器進行粉碎,結果獲得58.9 g之固形物。該固形物之乾燥減量為0.21%,經HPLC分析,結果,月桂醯基麩胺酸為83.5%,月桂醯基PCA為15.6%,月桂酸為0.14%。未檢測出其他明顯之雜質。
於50℃下使54.0 g之該固形物溶解於36.4 g之乙酸酐中,進而添加18.2 g之乙酸酐,直接於50℃下反應3小時。其後,冷卻至室溫,自反應液中過濾分離出產物,藉此,獲得N-月桂醯基-L-麩胺酸酐之粗結晶。對於該結晶,利用80 ml之醚,繼而利用15 ml之石油醚,對其進行洗淨、乾燥,而獲得34.2 g之固形物。該固形物之乾燥減量為0.21%,經HPLC分析,結果,月桂醯基麩胺酸酐為83.7%,月桂醯基麩胺酸為1.9%,月桂醯基PCA為13.4%,未檢測出月桂酸。未檢測出其他明顯之雜質。
進而,將9.1 g(0.05 mol)之L-離胺酸鹽酸鹽與57 g之水加以混合,之後,利用與實施例1相同之方法繼續製作成分A,結果,獲得以含有成分A之組合物為主體之pH值為7(25℃)之32重量%水溶液。此時,成分A為95.3%,成分B之醯基PCA為1.27%,月桂醯基麩胺酸為3.33%。未檢測出其他明顯之雜質。上述利用HPLC分析法所得之醯基PCA(%)比率為1.33%。
[比較例2]
對115.0 g之製造例2所獲得之月桂醯基麩胺酸等固形物成分/丙酮/水之成分重量比為55/30/15之有機層進行冷凍乾燥。
進行預冷凍,即,將櫃循環溫度設定為-60℃,試樣溫度達到-40℃後,冷卻2小時。將櫃循環溫度設定為-40℃,乾燥2小時後,設定為-10℃,大致於12 Pa下進行乾燥。其後,將設定溫度提昇至0℃、15℃、30℃。
確認容器內溫度為27.5℃、極限真空度為1 Pa以下後,利用乾燥氮氣解除真空。實施以上之乾燥步驟所需之時間為70小時下。
所獲得之固形物為平板狀,利用榨汁攪拌器將其粉碎,獲得59.5 g之固形物。該固形物之乾燥減量為0.51%,經HPLC分析,結果,月桂醯基麩胺酸為98.9%,未檢測出月桂醯基PCA及月桂酸。未檢測出其他明顯之雜質。
於50℃下使54.0 g之該固形物溶解於36.4 g之乙酸酐中,進而添加18.2 g之乙酸酐,直接於50℃下反應3小時。其後,冷卻至室溫,自反應液中過濾分離出產物,藉此,獲得N-月桂醯基-L-麩胺酸酐之粗結晶。對於該結晶,利用80 ml之醚,繼而利用15 ml之石油醚,對其進行洗淨、乾燥,而獲得34.2 g之固形物。該固形物之乾燥減量為1.2%,經HPLC分析,結果,月桂醯基麩胺酸酐為96.0%,月桂醯基麩胺酸為2.4%,未檢測出月桂醯基PCA及月桂酸。未檢測出其他明顯之雜質。
進而,將9.1 g(0.05 mol)之L-離胺酸鹽酸鹽與57 g之水加以混合,之後,利用與實施例1相同之方法繼續製作成分A,結果,獲得以含有成分A之組合物為主體之pH值為7(25℃)之32重量%水溶液。此時,成分A為96.3%,月桂醯基麩胺酸為3.30%。未檢測出月桂醯基PCA及月桂酸,未檢測出其他明顯之雜質。利用HPLC分析法所得之醯基PCA(%)比率為0%。
[實施例3]
一面緩慢攪拌100.0 g之製造例3所獲得之醯基麩胺酸等固形物成分/第三丁醇/水之成分重量比為62/27/11之有機層,一面於常壓下使其升溫直至液溫達到70℃為止。其後,一面慢慢減壓,一面使其升溫,緩慢提昇減壓度以免過度發泡,於極限減壓度為20 kPa下,達到到極限溫度115℃,將其維持20分鐘。其後,緩慢恢復至常壓,回收釜內之熔融物。將所獲得之固形物於冷藏庫中放置一夜,利用榨汁攪拌器進行粉碎,結果獲得55.5 g之固形物。該固形物之乾燥減量為0.14%,經HPLC分析,結果,醯基麩胺酸為90.9%,醯基PCA為7.7%,游離脂肪酸(月桂酸與肉豆蔻酸之總計)為0.74%。未檢測出其他明顯之雜質。
於50℃下使54.0 g之該固形物溶解於36.4 g之乙酸酐中,進而添加18.2 g之乙酸酐,直接於50℃下反應3小時。其後,冷卻至室溫,自反應液中過濾分離出產物,藉此,獲得N-醯基-L-麩胺酸酐之粗結晶。對於該結晶,利用80 ml之醚,繼而利用15 ml之石油醚,對其進行洗淨、乾燥,而獲得33.7 g之固形物。該固形物之乾燥減量為0.20%,經HPLC分析,結果,醯基麩胺酸酐為91.6%,醯基麩胺酸為1.7%,醯基PCA為6.1%,未檢測出游離脂肪酸。未檢測出其他明顯之雜質。
進而,將9.1 g(0.05 mol)之L-離胺酸鹽酸鹽與57 g之水加以混合,之後,利用與實施例1相同之方法繼續製作成分A,結果,獲得以含有成分A之組合物為主體之pH值為7(25℃)之32重量%水溶液。此時,成分A為96.2%,成分B之醯基PCA為0.293%,醯基麩胺酸為2.61%。未檢測出游離脂肪酸。未檢測出其他明顯之雜質。上述利用HPLC分析法所得之醯基PCA(%)比率為0.312%。
[比較例3]
對100 g之製造例3所獲得之醯基麩胺酸等固形物成分/第三丁醇/水之成分重量比為62/27/11之有機層進行冷凍乾燥。
進行預冷凍,即,將櫃循環溫度設定為-60℃,試樣溫度達到-40℃後,冷卻2小時。將櫃循環溫度設定為-40℃,乾燥2小時後,設定為-10℃,大致於5 Pa下進行乾燥。其後,將設定溫度提昇至0℃、20℃、30℃。
確認容器內溫度為27.5℃、極限真空度為1 Pa以下後,利用乾燥氮氣解除真空。實施以上之乾燥步驟所需之時間為55小時下。
所獲得之固形物為平板狀,利用榨汁攪拌器將其粉碎,獲得57.2 g之固形物。該固形物之乾燥減量為0.61%,經HPLC分析,結果,醯基麩胺酸為98.6%,未檢測出醯基PCA,游離脂肪酸為0.54%。未檢測出其他明顯之雜質。
於50℃下使54.0 g之該固形物溶解於36.4 g之乙酸酐中,進而添加18.2 g之乙酸酐,直接於50℃下反應3小時。其後,冷卻至室溫,自反應液中過濾分離出產物,藉此,獲得N-醯基-L-麩胺酸酐之粗結晶。對於該結晶,利用80 ml之醚,繼而利用15 ml之石油醚,對其進行洗淨、乾燥,而獲得32.8 g之固形物。該固形物之乾燥減量為1.5%,經HPLC分析,結果,醯基麩胺酸酐為96.0%,醯基麩胺酸為2.1%,未檢測出醯基PCA及游離脂肪酸。未檢測出其他明顯之雜質。
進而,將9.1 g(0.05 mol)之L-離胺酸鹽酸鹽與57 g之水加以混合,之後,利用與實施例1相同之方法繼續製作成分A,結果,獲得以含有成分A之組合物為主體之pH值為7(25℃)之32重量%水溶液。此時,成分A為96.6%,醯基麩胺酸為3.15%。未檢測出醯基PCA及游離脂肪酸,未檢測出其他明顯之雜質。利用HPLC分析法所得之醯基PCA(%)比率為0%。
[實施例4]
另外,再次實施與製造例1同等之操作,獲得月桂醯基麩胺酸等固形物成分/第三丁醇/水之成分重量比為64/25/11之有機層。一面緩慢攪拌125 g之該有機層,一面於常壓下使其升溫直至液溫達到90℃為止。其後,一面慢慢減壓,一面使其升溫,緩慢提昇減壓度以免過度發泡,於極限減壓度40 kPa下,將極限溫度105℃維持120分鐘。其後,緩慢恢復至常壓,回收釜內之熔融物。將所獲得之固形物於冷藏庫中放置一夜,利用榨汁攪拌器進行粉碎,結果獲得70.6 g之固形物。該固形物之乾燥減量為0.20%,經HPLC分析,結果,月桂醯基麩胺酸為80.7%,月桂醯基PCA為14.1%,月桂酸為4.7%。未檢測出其他明顯之雜質。
於50℃下使54.0 g之該固形物溶解於36.4 g之乙酸酐中,進而添加18.2 g之乙酸酐,直接於50℃下反應3小時。其後,冷卻至室溫,自反應液中過濾分離出產物,藉此,獲得以N-月桂醯基-L-麩胺酸酐為主體之粗結晶。對於該結晶,利用80 ml之醚,進而再次利用80 ml之醚,對其進行洗淨、乾燥,而獲得32.7 g之固形物。該固形物之乾燥減量為0.19%,經HPLC分析,結果,月桂醯基麩胺酸酐為84.5%,月桂醯基PCA為13.0%,月桂醯基麩胺酸為1.9%,未檢測出月桂酸。未檢測出其他明顯之雜質。
進而,將9.1 g(0.05 mol)之L-離胺酸鹽酸鹽與57 g之水加以混合。利用25%氫氧化鈉水溶液將該液體之pH值範圍調整為10~11,又,將反應溫度維持於5℃,並且於攪拌下歷時2小時添加32.7 g之上述經洗淨、乾燥而獲得之固形物,實施反應。進而繼續攪拌30分鐘後,以液中濃度成為20質量%之方式添加第三丁醇後,滴加75%硫酸而將液體之pH值調整為2,又,將液體之溫度調整為65℃。滴加結束後,停止攪拌,於65℃下靜置20分鐘,則分層為有機層與水層,自其中分離出有機層。未反應之離胺酸幾乎被水層回收。對所獲得之有機層反覆進行相同之水洗操作後,自所獲得之有機層中去除溶劑,利用氫氧化鈉以成為固形物成分為30質量%、pH值為7(25℃)之水溶液之方式進行中和製備。進而,一面添加水,一面進行減壓蒸餾,對第三丁醇於減壓度13~22 kPa、液溫45~60℃下繼續進行減壓蒸餾直至液中濃度達到10質量ppm以下為止。最終所獲得者為以含有式(A)所示之醯基化合物之組合物為主體之pH值為7(25℃)之32重量%水溶液,成分A為91.2%,成分B之醯基PCA為6.25%,月桂醯基麩胺酸為2.32%。未檢測出其他明顯之雜質。上述利用HPLC分析法所得之醯基PCA(%)比率為6.85%。
<HPLC分析法及固形物成分測定法>
算出成分C及成分D相對於成分A之比率時,根據下述藉由使用HPLC之分析而獲得之波峰區域面積算出純度。
檢測器:RI檢測器
分離管:向內徑6 mm、長度150 mm之不鏽鋼管中填充於粒徑5 μm、孔徑12 nm之矽膠上修飾有十八烷基矽烷基者。
分離管溫度:60℃左右之一定溫度
流動相:甲醇/水/磷酸=2000/400/0.31
流量:每分鐘0.8 mL
繼而,成分C/成分A+C、成分D/成分A+D由下式所示,相當於下述表中之「成分C質量(%)」、「成分D質量(%)」。
成分C/成分A+C=
[成分C之淨重(g)/成分A淨重(g)+成分C淨重(g)]×100(%)
成分D/成分A+D=
[成分D之淨重(g)/成分A淨重(g)+成分D淨重(g)]×100(%)
<高純度之成分A之製作>
以旭化成FineChem股份有限公司製造之Pellicer L-30之冷凍乾燥物(水分為2.0%)或於實施例1變更醯氯而製造之該冷凍乾燥物作為原料,實施下述操作。將上述冷凍乾燥物、蒸餾水及第三丁醇以重量比45/33/22於60℃下進行攪拌。達到60℃後,緩慢添加硫酸,繼續添加硫酸直至於65℃下pH值成為2為止,30分鐘後停止攪拌,靜置。靜置30分鐘後,去除分層之下層(水層)。稱量下層(水層),將相同重量之20重量%第三丁醇水溶液(第三丁醇/蒸餾水之重量比為2/8)添加至上層,於60℃下進行攪拌。30分鐘後停止攪拌,靜置30分鐘。同樣地去除下層。注入與上述下層相同重量之20重量%第三丁醇水溶液後,將攪拌、靜置、去除下層之步驟(水洗脫鹽步驟)進一步進行2次,共計重複3次。對結束水洗脫鹽步驟後之有機層進行冷凍乾燥。
對於上述乾燥物,於室溫下利用100 ml之醚,繼而利用50 ml之石油醚,對其進行洗淨、乾燥。再次實施此操作,獲得成分A。利用上述HPLC對其進行分析,未檢測出波峰率0.1%以上之其他成分。
<高純度之成分B之製作>
於氮氣氛圍10℃之條件下,將90 mmol之焦麩胺酸、180 mmol之三乙胺、150 mL之乙腈於燒瓶內加以攪拌混合。繼而,添加向60 mL之乙腈中添加90 mmol之各種醯氯而成之溶液後,自冰浴中取出,將反應混合物於室溫下攪拌2小時。利用玻璃過濾器過濾反應混合物後,於減壓下使用蒸發器進行濃縮。添加150 mL之水及120 mL之1 M鹽酸後,利用100 mL之乙酸乙酯將殘渣萃取4次。利用硫酸鎂使合併之有機層乾燥後,於真空中進行濃縮。利用庚烷/乙酸乙酯=5:4(90 mL)使殘渣再結晶,以純度95%以上獲得醯基焦麩胺酸。
<高純度之成分C之製作>
對旭化成FineChem股份有限公司製造之Aminosurfact ALMS-P1或變更醯氯並利用與製造例1相同之方法製造之組合物重複2次水洗操作後,自所獲得之有機層中去除溶劑,將利用氫氧化鈉以成為固形物成分為30質量%、pH值為7(25℃)之水溶液之方式進行中和製備並乾燥而成之組合物作為原料,實施下述操作。將上述製品、蒸餾水及第三丁醇以重量比45/33/22於60℃下加以攪拌。達到60℃後,緩慢添加硫酸,繼續添加硫酸直至於65℃下pH值成為2為止,30分鐘後停止攪拌,靜置。靜置30分鐘後,去除分層之下層(水層)。稱量下層(水層),將相同重量之20重量%第三丁醇水溶液(第三丁醇/蒸餾水之重量比為2/8)添加至上層,於60℃下進行攪拌。30分鐘後停止攪拌,靜置30分鐘。同樣地去除下層。注入與上述下層相同重量之20重量%第三丁醇水溶液後,將攪拌、靜置、去除下層之步驟(水洗脫鹽步驟)進一步進行2次,共計重複3次。對結束水洗脫鹽步驟後之有機層進行冷凍乾燥。
對於上述乾燥物,於室溫下利用120 ml之醚,繼而利用60 ml之石油醚,對其進行洗淨、乾燥。再次實施此操作,獲得成分C。利用上述HPLC對其進行分析,未檢測出波峰率0.1%以上之其他成分。
<高純度之成分D之獲取>
自東京化成工業股份有限公司,獲取辛酸(O0027)、月桂酸(L0011)、肉豆蔻酸(M0476)、棕櫚酸(P1145)、硬脂酸(S0163)、山萮酸(B1248)。
<高純度之成分E之獲取>
自富士膠片和光純藥股份有限公司,獲取辛醯胺(O237203)、月桂醯胺(516472)、肉豆蔻醯胺(B22610)、棕櫚醯胺(QE-1627)、硬脂醯胺(192-04015)、山萮醯胺(B131150)。
<LC-MS(liquid chromatography-mass spectrometry,液相層析-質譜法)分析法>
於實施例及比較例中,成分E係藉由下述使用LC-MS之分析來確認純度。
(LC-MS裝置)
分離管:向內徑2mm、長度30 mm之不鏽鋼管中填充於粒徑3 μm之粒子上修飾有苯基者。
分離管溫度:40℃左右之一定溫度
流動相:10 mM乙酸銨水溶液及乙腈之梯度溶出法
流量:每分鐘0.3 mL左右之一定量
測定機器例如可使用島津製作所股份有限公司之LCMS-9030等。
離子化:ESI+
掃描範圍:m/z50~1200
M+H:200.203
<HPLC分析法>
於實施例及比較例中,算出成分E及成分A之比率時,藉由下述使用HPLC之分析來確認純度。
檢測器:UV檢測器(205 nm)
測定機器例如可使用島津製作所股份有限公司之SPD-10Avp、SPD-10AVvp、SPD-20A及SPD-20AV等。
分離管:向內徑6 mm、長度150 mm之不鏽鋼管中填充於粒徑5 μm、孔徑12 nm之矽膠上修飾有十八烷基矽烷基者。
分離管溫度:60℃左右之一定溫度
流動相:甲醇/水/磷酸=2000/400/0.31
流量:每分鐘0.8 mL左右之一定量
更具體而言,成分E/成分A由下式所示,相當於下述表中之「成分E質量(%)」。
成分E/成分A=[成分E之淨重(g)/成分A淨重(g)]×100(%)
實施例、比較例所使用之椰子醯胺MEA使用川研精細化學股份有限公司之Amisol CME,月桂醯胺MEA使用川研精細化學股份有限公司之Amisol LME。
實施例27、30、33、36、42、45、48、51、54、57、60、63、66、69、72、75、78、81、84、87係將實施例1之32%水溶液與上述高純度成分A、成分C、成分D、成分E加以混合,以成為表中所記載之抗衡鹽、pH值之方式來製備,實施例28、31、34、37、43、46、49、52、55、58、61、64、67、70、73、76、79、82、85、88係將實施例2之32%水溶液與上述高純度成分A、成分C、成分D、成分E加以混合,以成為表中所記載之抗衡鹽、pH值之方式來製備,實施例29、32、35、38、44、47、50、53、56、59、62、65、68、71、74、77、80、83、86、89係將實施例4之32%水溶液與上述高純度成分A、成分C、成分D、成分E加以混合,以成為表中所記載之抗衡鹽、pH值之方式來製備。關於其他實施例、比較例,準確稱量高純度之成分A、成分C~成分E,向所獲得之固體粉末中混合計算量之可成為抗衡鹽之氫氧化鈉或氫氧化鉀或三乙醇胺或精胺酸,製作調整了pH值及固形物成分之水溶液。將該等水溶液最終調整為指定之pH值及固形物成分32%。比較例7~9、10、12、14、16、18、20、22、24、26、28、30係將成分A置換為同量之聚山梨糖醇酯60,成分B~成分E之比率記載為聚山梨糖醇酯60為成分A時之比率。於實施例9,將1%之硬脂醯基麩胺酸Na置換為純化水並添加,於實施例10中,將3%之肉豆蔻酸、2%之棕櫚酸置換為純化水並添加。
<乳化穩定性確認試驗1>
製作下述組成。
組成 wt%
・實施例或比較例之32%水溶液 0.09
・油(棕櫚酸乙基己酯、橄欖油
礦物油、環甲矽脂、矽靈) 20.0
・卡波姆(Carbopol 981) 0.2
・30 wt/v%之NaOH水溶液 0.28
・純化水 79.43
上述組成按照下述1.~4.之製作順序。
1.使卡波姆溶解於純化水中。
2.利用KOH或三乙醇胺或精胺酸或NaOH水溶液將卡波姆水溶液調整為指定之pH值。
3.添加實施例或比較例之32%水溶液及各種油。
4.於室溫下使用均質攪拌機(6000 rpm)乳化5分鐘。
將上述組成於55℃下保存2個月後、2.5個月後、3.0個月後,利用目視進行確認。
評價基準
5:液體深度全部乳化
4:液體深度之90%以上乳化
3:液體深度之80%以上乳化
2:液體深度之70%以上乳化
1:乳化之液體深度不滿70%
<乳化穩定性確認試驗2>
製作下述組成。
組成 wt%
・實施例或比較例之32%水溶液 0.09
・礦物油(5.8~8.9 mm2/s) 16.0
・固體油(鯨蠟硬脂醇、肉豆蔻醇) 4.0
・卡波姆(Carbopol 981) 0.2
・30 wt/v%之NaOH水溶液 0.28
・純化水 79.43
上述組成按照下述1.~4.之製作順序。
1.使卡波姆溶解於純化水中,利用KOH或三乙醇胺或精胺酸或NaOH水溶液將卡波姆水溶液調整為指定之pH值。
2.添加實施例或比較例之32%水溶液及純化水而製成水相。將其加溫至70℃。
3.以礦物油及固體油作為油相,加溫至70℃。
4.將水相及油相加以混合,利用3000 rpm之均質攪拌機攪拌升溫至80℃。
5.利用6000 rpm之均質攪拌機實施5分鐘乳化。
6.利用3000 rpm之均質攪拌機攪拌、冷卻至25℃。
7.進行脫氣。
將上述組成於55℃下保存靜置2個月、2.5個月、3.0個月,利用目視確認乳化性。
評價基準
5:液體深度全部乳化。
4:液體深度之90%以上乳化。
3:液體深度之80%以上乳化。
2:液體深度之70%以上乳化。
1:乳化之液體深度不滿70%。
<分散穩定性確認試驗>
以成為1%濃度之方式向實施例、比較例各者之固形物成分0.0075%之水溶液中添加氧化鈦,以成為指定之pH值之方式添加KOH或三乙醇胺或精胺酸或NaOH水溶液。其後,實施30秒超音波處理,均質化(10000 rpm,2分鐘)後,測定於50℃下靜置時之上清液之吸光度(波長為300 nm),確認水中分散性。
任一吸光度初始值均為1.8左右,利用200小時後、224小時後、248小時後之吸光度測定來實施下述評價。
評價基準
5:吸光度為1.7以上
4:吸光度為1.5以上且未達1.7
3:吸光度為1.3以上且未達1.5
2:吸光度為1.0以上且未達1.3
1:吸光度未達1.0
<使用感評價>
對乳化穩定性確認試驗1所製備之矽靈之配方進行如下評價。藉由5名官能檢查員進行官能評價,將平均值作為評價分。
(評價項目:融合過程中之水潤性)
非常水潤 5
具有水潤性 4
稍微具有水潤性 3
幾乎沒有水潤性 2
沒有水潤性 1
(評價項目:融合後是否黏膩)
不黏膩 5
幾乎不黏膩 4
稍微黏膩 3
黏膩 2
非常黏膩 1
(評價項目:塗佈時之濃厚感)
非常濃厚 5
具有濃厚感 4
稍微具有濃厚感 3
幾乎沒有濃厚感 2
沒有濃厚感 1
(評價項目:融合過程中之延展之良好性)
延展非常好 5
延展較好 4
延展稍好 3
延展不太好 2
延展不好 1
(評價項目:融合後之光滑性)
非常光滑 5
具有光滑性 4
稍微具有光滑性 3
幾乎沒有光滑性 2
沒有光滑性 1
分別使用實施例、比較例之組合物實施上述乳化穩定性確認試驗1、乳化穩定性確認試驗2、分散穩定性確認試驗及使用感評價之4個試驗、評價。將結果示於表1~5。
再者,如上所述,表中之「成分B比率(%)」係相對於成分A者,「成分C質量(%)」係相對於成分A及成分C之合計者,「成分D質量(%)」係相對於成分A及成分D之合計者,「成分E質量(%)」係相對於成分A者。
[表1-1]
表1-1 | ||||||||||||||||||||||||||||||||||||||||
編號 | 實施例1 | 實施例2 | 實施例3 | 實施例4 | 比較例1 | 比較例2 | 比較例3 | 實施例5 | 實施例6 | 實施例7 | 實施例8 | 實施例9 | 實施例10 | |||||||||||||||||||||||||||
組合物 | ||||||||||||||||||||||||||||||||||||||||
成分A | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | |||||||||||||||||||||||||||
成分B比率(%) | 0.032 | 1.33 | 0.312 | 6.85 | 0 | 0 | 0 | - | - | - | - | - | - | |||||||||||||||||||||||||||
成分C質量(%) | - | - | - | - | - | - | - | 1.3 | 5.1 | 6.5 | 5.8 | 1.3 | 1.3 | |||||||||||||||||||||||||||
成分D質量(%) | - | - | - | - | - | - | - | 0.08 | 0.14 | 2.1 | 0.55 | 0.08 | 0.08 | |||||||||||||||||||||||||||
成分E質量(%) | - | - | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||||||
椰子醯胺MEA | - | - | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||||||
月桂醯胺MEA | - | - | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||||||
成分A~E之R 1~R 6之碳數 | (A,11) (B,11) | (A,11) (B,11) | (A,11) (B,11) | (A,11) (B,11) | (A,11) | (A,11) | (A,11) | (A,11) (C,11) (D,11) | (A,11) (C,11) (D,11) | (A,11) (C,11) (D,11) | (A,11) (C,11) (D,11) | (A,11) (C,11) (D,11) | (A,11) (C,11) (D,11) | |||||||||||||||||||||||||||
成分A~D之M 1~M 7 | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | |||||||||||||||||||||||||||
混合溶液之pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||||||||||
配方評價 | ||||||||||||||||||||||||||||||||||||||||
pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||||||||||
乳化穩定性確認試驗1 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | |
棕櫚酸乙基己酯 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 1 | 5 | 3 | 1 | 5 | 3 | 1 | 4 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 3 | 5 | 3 | 2 | 4 | 3 | 1 | 4 | 3 | 1 | |
橄欖油 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 2 | 1 | 5 | 2 | 1 | 4 | 2 | 1 | 4 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | |
礦物油 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 1 | 5 | 3 | 1 | 5 | 2 | 1 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 4 | 3 | 3 | 5 | 3 | 3 | |
環甲矽脂 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 4 | 2 | 1 | 4 | 2 | 1 | 4 | 2 | 1 | 5 | 3 | 2 | 5 | 3 | 2 | 4 | 3 | 2 | 5 | 3 | 3 | 5 | 4 | 3 | 5 | 3 | 3 | |
矽靈 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 4 | 2 | 1 | 5 | 2 | 1 | 4 | 2 | 1 | 5 | 3 | 3 | 5 | 3 | 2 | 4 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 3 | 4 | 3 | 3 | |
乳化穩定性確認試驗2 | ||||||||||||||||||||||||||||||||||||||||
鯨蠟硬脂醇 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 4 | 2 | 1 | 4 | 2 | 1 | 5 | 3 | 1 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | |
肉豆蔻醇 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 4 | 2 | 1 | 5 | 2 | 1 | 4 | 2 | 1 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 4 | 2 | 5 | 4 | 2 | |
分散穩定性確認試驗 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | |
5 | 3 | 2 | 5 | 3 | 2 | 4 | 4 | 3 | 4 | 3 | 2 | 4 | 2 | 1 | 3 | 1 | 1 | 4 | 2 | 1 | 5 | 3 | 1 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 4 | 2 | 5 | 3 | 1 | 5 | 3 | 1 | ||
官能評價 | ||||||||||||||||||||||||||||||||||||||||
水潤性 | 5 | 5 | 5 | 4 | 4 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | |||||||||||||||||||||||||||
是否黏膩 | 5 | 5 | 5 | 4 | 4 | 4 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | |||||||||||||||||||||||||||
濃厚感 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 5 | 5 | 5 | 5 | 5 | 5 | |||||||||||||||||||||||||||
延展之良好性 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | |||||||||||||||||||||||||||
光滑性 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 |
[表1-2]
表1-2 | ||||||||||||||||||||||||||||||||||
編號 | 實施例11 | 實施例12 | 實施例13 | 比較例4 | 比較例5 | 比較例6 | 實施例14 | 實施例14 | 實施例15 | 實施例16 | 實施例17 | |||||||||||||||||||||||
組合物 | ||||||||||||||||||||||||||||||||||
成分A | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | |||||||||||||||||||||||
成分B比率(%) | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||
成分C質量(%) | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||
成分D質量(%) | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||
成分E質量(%) | 0.009 | 0.215 | 4.309 | 0 | 0 | 0 | 0.03 | 0.091 | 0.215 | 0.215 | 2.153 | |||||||||||||||||||||||
椰子醯胺MEA | - | - | - | 0 | 0.064 | 0 | 0 | 0 | 0.064 | 0 | 0 | |||||||||||||||||||||||
月桂醯胺MEA | - | - | - | 0 | 0 | 0.064 | 0 | 0 | 0 | 0.064 | 0 | |||||||||||||||||||||||
成分A~E之R 1~R 6之碳數 | (A,11) (E,11) | (A,11) (E,11) | (A,11) (E,11) | (A,11) | (A,11) | (A,11) | (A,11) (E,11) | (A,11) (E,11) | (A,11) (E,11) | (A,11) (E,11) | (A,11) (E,11) | |||||||||||||||||||||||
成分A~D之M 1~M 7 | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | |||||||||||||||||||||||
混合溶液之pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||||||
配方評價 | ||||||||||||||||||||||||||||||||||
pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||||||
乳化穩定性確認試驗1 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | |
棕櫚酸乙基己酯 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 1 | 5 | 3 | 1 | 5 | 2 | 1 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | |
橄欖油 | 5 | 3 | 3 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 2 | 1 | 5 | 2 | 1 | 5 | 3 | 1 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | |
礦物油 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 2 | 1 | 5 | 3 | 1 | 5 | 3 | 1 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 3 | |
環甲矽脂 | 5 | 3 | 3 | 5 | 3 | 3 | 5 | 3 | 2 | 4 | 2 | 1 | 4 | 2 | 1 | 4 | 2 | 1 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 3 | |
矽靈 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 1 | 4 | 2 | 1 | 5 | 2 | 1 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | |
乳化穩定性確認試驗2 | ||||||||||||||||||||||||||||||||||
鯨蠟硬脂醇 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 3 | 4 | 2 | 1 | 4 | 2 | 1 | 4 | 2 | 1 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | |
肉豆蔻醇 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 3 | 4 | 2 | 1 | 4 | 2 | 1 | 4 | 2 | 1 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | |
分散穩定性確認試驗 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | |
4 | 2 | 2 | 5 | 3 | 3 | 4 | 3 | 2 | 3 | 2 | 1 | 3 | 1 | 1 | 3 | 1 | 1 | 4 | 3 | 1 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | ||
官能評價 | ||||||||||||||||||||||||||||||||||
水潤性 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | |||||||||||||||||||||||
是否黏膩 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | |||||||||||||||||||||||
濃厚感 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | |||||||||||||||||||||||
延展之良好性 | 5 | 5 | 4 | 4 | 3 | 3 | 5 | 5 | 5 | 5 | 5 | |||||||||||||||||||||||
光滑性 | 4 | 5 | 5 | 3 | 3 | 3 | 5 | 5 | 5 | 5 | 5 |
[表2-1]
表2-1 | ||||||||||||||||||||||||||||
編號 | 實施例18 | 實施例19 | 實施例20 | 實施例21 | 實施例22 | 實施例23 | 實施例24 | 實施例25 | 實施例26 | |||||||||||||||||||
組合物 | ||||||||||||||||||||||||||||
成分A | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | |||||||||||||||||||
成分B比率(%) | 0.032 | 1.33 | 6.85 | 0.032 | 1.33 | 6.85 | - | - | - | |||||||||||||||||||
成分C質量(%) | - | - | - | 1.3 | 5.1 | 6.5 | 1.3 | 5.1 | 6.5 | |||||||||||||||||||
成分D質量(%) | - | - | - | 0.08 | 0.14 | 2.1 | 0.08 | 0.14 | 2.1 | |||||||||||||||||||
成分E質量(%) | 0.009 | 0.215 | 4.309 | - | - | - | 0.009 | 0.215 | 4.309 | |||||||||||||||||||
椰子醯胺MEA | - | - | - | - | - | - | - | - | - | |||||||||||||||||||
月桂醯胺MEA | - | - | - | - | - | - | - | - | - | |||||||||||||||||||
成分A~E之R 1~R 6之碳數 | (A,11) (B,11) (E,11) | (A,11) (B,11) (E,11) | (A,11) (B,11) (E,11) | (A,11) (B,11) (C,11) (D,11) | (A,11) (B,11) (C,11) (D,11) | (A,11) (B,11) (C,11) (D,11) | (A,11) (C,11) (D,11) (E,11) | (A,11) (C,11) (D,11) (E,11) | (A,11) (C,11) (D,11) (E,11) | |||||||||||||||||||
成分A~D之M 1~M 7 | Na | Na | Na | Na | Na | Na | Na | Na | Na | |||||||||||||||||||
混合溶液之pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||
配方評價 | ||||||||||||||||||||||||||||
pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||
乳化穩定性確認試驗1 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | |
棕櫚酸乙基己酯 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | |
橄欖油 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | |
礦物油 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | |
環甲矽脂 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 4 | 3 | 5 | 4 | 4 | 5 | 4 | 3 | |
矽靈 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 4 | 3 | |
乳化穩定性確認試驗2 | ||||||||||||||||||||||||||||
鯨蠟硬脂醇 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 3 | |
肉豆蔻醇 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | |
分散穩定性確認試驗 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | |
5 | 5 | 3 | 5 | 5 | 3 | 5 | 5 | 2 | 5 | 5 | 3 | 5 | 5 | 3 | 5 | 5 | 2 | 5 | 5 | 3 | 5 | 5 | 3 | 5 | 5 | 1 | ||
官能評價 | ||||||||||||||||||||||||||||
水潤性 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 3 | 3 | |||||||||||||||||||
是否黏膩 | 5 | 5 | 4 | 5 | 5 | 5 | 3 | 3 | 3 | |||||||||||||||||||
濃厚感 | 3 | 3 | 3 | 5 | 5 | 5 | 5 | 5 | 5 | |||||||||||||||||||
延展之良好性 | 5 | 5 | 5 | 3 | 3 | 3 | 5 | 5 | 5 | |||||||||||||||||||
光滑性 | 4 | 5 | 5 | 3 | 3 | 3 | 5 | 5 | 5 |
[表2-2]
表2-2 | |||||||||||||||||||
編號 | 實施例27 | 實施例28 | 實施例29 | 比較例7 | 比較例8 | 比較例9 | |||||||||||||
組合物 | |||||||||||||||||||
成分A | 有 | 有 | 有 | 無 | 無 | 無 | |||||||||||||
成分B比率(%) | 0.032 | 1.33 | 6.85 | 0.032 | 1.33 | 6.85 | |||||||||||||
成分C質量(%) | 1.3 | 5.1 | 6.5 | 1.3 | 5.1 | 6.5 | |||||||||||||
成分D質量(%) | 0.08 | 0.14 | 2.1 | 0.08 | 0.14 | 2.1 | |||||||||||||
成分E質量(%) | 0.009 | 0.215 | 4.309 | 0.009 | 0.215 | 4.309 | |||||||||||||
椰子醯胺MEA | - | - | - | - | - | - | |||||||||||||
月桂醯胺MEA | - | - | - | - | - | - | |||||||||||||
成分A~E之R 1~R 6之碳數 | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (B,11) (C,11) (D,11) (E,11) | (B,11) (C,11) (D,11) (E,11) | (B,11) (C,11) (D,11) (E,11) | |||||||||||||
成分A~D之M 1~M 7 | Na | Na | Na | Na | Na | Na | |||||||||||||
混合溶液之pH值 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||
配方評價 | |||||||||||||||||||
pH值 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||
乳化穩定性確認試驗1 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | |
棕櫚酸乙基己酯 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 2 | 3 | 2 | 2 | 4 | 2 | 2 | |
橄欖油 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | 4 | 2 | 2 | |
礦物油 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 2 | 3 | 2 | 2 | 4 | 2 | 2 | |
環甲矽脂 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 4 | 2 | 1 | 3 | 2 | 1 | 3 | 2 | 1 | |
矽靈 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 2 | 4 | 2 | 2 | 3 | 2 | 1 | |
乳化穩定性確認試驗2 | |||||||||||||||||||
鯨蠟硬脂醇 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 3 | 1 | 1 | 3 | 2 | 1 | |
肉豆蔻醇 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 3 | 2 | 1 | 3 | 2 | 1 | |
分散穩定性確認試驗 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | |
5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 4 | 1 | 1 | 3 | 1 | 1 | 3 | 1 | 1 | ||
官能評價 | |||||||||||||||||||
水潤性 | 5 | 5 | 5 | 3 | 3 | 2 | |||||||||||||
是否黏膩 | 5 | 5 | 4 | 2 | 2 | 3 | |||||||||||||
濃厚感 | 5 | 5 | 5 | 3 | 2 | 3 | |||||||||||||
延展之良好性 | 5 | 5 | 5 | 2 | 3 | 2 | |||||||||||||
光滑性 | 5 | 5 | 5 | 3 | 3 | 2 |
[表3-1]
表3-1 | |||||||||||||||||||||||||||||||
編號 | 實施例30 | 實施例31 | 實施例32 | 比較例10 | 比較例11 | 實施例33 | 實施例34 | 實施例35 | 比較例12 | 比較例13 | |||||||||||||||||||||
組合物 | |||||||||||||||||||||||||||||||
成分A | 有 | 有 | 有 | 無 | 有 | 有 | 有 | 有 | 無 | 有 | |||||||||||||||||||||
成分B比率(%) | 0.032 | 1.33 | 6.85 | 1.33 | - | 0.032 | 1.33 | 6.85 | 1.33 | - | |||||||||||||||||||||
成分C質量(%) | 1.3 | 5.1 | 6.5 | 5.1 | - | 1.3 | 5.1 | 6.5 | 5.1 | - | |||||||||||||||||||||
成分D質量(%) | 0.08 | 0.14 | 2.1 | 0.14 | - | 0.08 | 0.14 | 2.1 | 0.14 | - | |||||||||||||||||||||
成分E質量(%) | 0.009 | 0.215 | 4.309 | 0.215 | - | 0.009 | 0.215 | 4.309 | 0.215 | - | |||||||||||||||||||||
椰子醯胺MEA | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||
月桂醯胺MEA | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||
成分A~E之R 1~R 6之碳數 | (A,7) (B,7) (C,7) (D,7) (E,7) | (A,7) (B,7) (C,7) (D,7) (E,7) | (A,7) (B,7) (C,7) (D,7) (E,7) | (B,7) (C,7) (D,7) (E,7) | (A,7) | (A,13) (B,13) (C,13) (D,13) (E,13) | (A,13) (B,13) (C,13) (D,13) (E,13) | (A,13) (B,13) (C,13) (D,13) (E,13) | (B,13) (C,13) (D,13) (E,13) | (A,13) | |||||||||||||||||||||
成分A~D之M 1~M 7 | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | |||||||||||||||||||||
混合溶液之pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||||
配方評價 | |||||||||||||||||||||||||||||||
pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||||
乳化穩定性確認試驗1 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | |
棕櫚酸乙基己酯 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 3 | 1 | 5 | 3 | 1 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 1 | 5 | 3 | 1 | |
橄欖油 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 3 | 1 | 4 | 2 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
礦物油 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 5 | 3 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 1 | 5 | 3 | 1 | |
環甲矽脂 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 4 | 2 | 1 | 4 | 2 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 5 | 3 | 1 | |
矽靈 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 4 | 4 | 2 | 1 | 3 | 2 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 4 | 2 | 1 | 3 | 2 | 1 | |
乳化穩定性確認試驗2 | |||||||||||||||||||||||||||||||
鯨蠟硬脂醇 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 1 | 4 | 2 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
肉豆蔻醇 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 1 | 4 | 2 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
分散穩定性確認試驗 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | |
5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 3 | 1 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 3 | 1 | 1 | ||
官能評價 | |||||||||||||||||||||||||||||||
水潤性 | 5 | 5 | 5 | 3 | 3 | 5 | 5 | 4 | 3 | 3 | |||||||||||||||||||||
是否黏膩 | 5 | 5 | 4 | 1 | 2 | 5 | 5 | 5 | 2 | 3 | |||||||||||||||||||||
濃厚感 | 5 | 5 | 5 | 2 | 2 | 5 | 5 | 5 | 2 | 2 | |||||||||||||||||||||
延展之良好性 | 5 | 5 | 5 | 2 | 2 | 5 | 5 | 5 | 2 | 2 | |||||||||||||||||||||
光滑性 | 4 | 5 | 5 | 2 | 3 | 4 | 5 | 5 | 3 | 3 |
[表3-2]
表3-2 | ||||||||||||||||||||||||||||||||||
編號 | 實施例36 | 實施例37 | 實施例38 | 比較例14 | 比較例15 | 實施例39 | 實施例40 | 實施例41 | 實施例42 | 實施例43 | 實施例44 | |||||||||||||||||||||||
組合物 | ||||||||||||||||||||||||||||||||||
成分A | 有 | 有 | 有 | 無 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | |||||||||||||||||||||||
成分B比率(%) | 0.032 | 1.33 | 6.85 | 1.33 | - | - | - | - | 0.032 | 1.33 | 6.85 | |||||||||||||||||||||||
成分C質量(%) | 1.3 | 5.1 | 6.5 | 5.1 | - | - | - | - | - | - | - | |||||||||||||||||||||||
成分D質量(%) | 0.08 | 0.14 | 2.1 | 0.14 | - | - | - | - | - | - | - | |||||||||||||||||||||||
成分E質量(%) | 0.009 | 0.215 | 4.309 | 0.215 | - | 0.009 | 0.215 | 4.309 | 0.009 | 0.215 | 4.309 | |||||||||||||||||||||||
椰子醯胺MEA | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||
月桂醯胺MEA | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||
成分A~E之R 1~R 6之碳數 | (A,15) (B,15) (C,15) (D,15) (E,15) | (A,15) (B,15) (C,15) (D,15) (E,15) | (A,15) (B,15) (C,15) (D,15) (E,15) | (B,15) (C,15) (D,15) (E,15) | (A,15) | (A,17) (E,17) | (A,17) (E,17) | (A,17) (E,17) | (A,11) (B,11) (E,17) | (A,11) (B,11) (E,17) | (A,11) (B,11) (E,17) | |||||||||||||||||||||||
成分A~D之M 1~M 7 | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | |||||||||||||||||||||||
混合溶液之pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||||||
配方評價 | ||||||||||||||||||||||||||||||||||
pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||||||
乳化穩定性確認試驗1 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | |
棕櫚酸乙基己酯 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 1 | 5 | 3 | 1 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 4 | 2 | 5 | 5 | 4 | 5 | 5 | 3 | 5 | 5 | 4 | |
橄欖油 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 1 | 1 | 4 | 2 | 1 | 5 | 3 | 3 | 5 | 4 | 3 | 5 | 3 | 2 | 5 | 5 | 5 | 5 | 5 | 4 | 5 | 5 | 4 | |
礦物油 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 1 | 5 | 3 | 1 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 3 | |
環甲矽脂 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 1 | 1 | 5 | 3 | 1 | 5 | 3 | 3 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 4 | 3 | 5 | 5 | 3 | 5 | 4 | 3 | |
矽靈 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 4 | 2 | 1 | 4 | 2 | 1 | 5 | 4 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 3 | 5 | 5 | 3 | |
乳化穩定性確認試驗2 | ||||||||||||||||||||||||||||||||||
鯨蠟硬脂醇 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 4 | 2 | 1 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 5 | 3 | 5 | 5 | 4 | 5 | 5 | 4 | |
肉豆蔻醇 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 5 | 3 | 1 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 5 | 3 | 5 | 5 | 4 | 5 | 5 | 4 | |
分散穩定性確認試驗 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | |
5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 1 | 1 | 5 | 3 | 2 | 5 | 4 | 3 | 4 | 3 | 2 | 5 | 5 | 3 | 5 | 5 | 4 | 5 | 4 | 2 | ||
官能評價 | ||||||||||||||||||||||||||||||||||
水潤性 | 5 | 5 | 5 | 2 | 2 | 3 | 3 | 3 | 5 | 5 | 5 | |||||||||||||||||||||||
是否黏膩 | 5 | 5 | 5 | 1 | 3 | 3 | 3 | 3 | 5 | 5 | 5 | |||||||||||||||||||||||
濃厚感 | 5 | 5 | 5 | 2 | 2 | 3 | 3 | 3 | 5 | 5 | 5 | |||||||||||||||||||||||
延展之良好性 | 5 | 5 | 4 | 2 | 2 | 5 | 5 | 4 | 5 | 5 | 5 | |||||||||||||||||||||||
光滑性 | 4 | 5 | 5 | 3 | 3 | 4 | 5 | 5 | 4 | 5 | 5 |
[表3-3]
表3-3 | ||||||||||||||||||||||||||||||||||||||||
編號 | 實施例45 | 實施例46 | 實施例47 | 比較例16 | 比較例17 | 實施例48 | 實施例49 | 實施例50 | 實施例51 | 實施例52 | 實施例53 | 比較例18 | 比較例19 | |||||||||||||||||||||||||||
組合物 | ||||||||||||||||||||||||||||||||||||||||
成分A | 有 | 有 | 有 | 無 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 無 | 有 | |||||||||||||||||||||||||||
成分B比率(%) | 0.032 | 1.33 | 6.85 | 1.33 | - | 0.032 | 1.33 | 6.85 | 0.032 | 1.33 | 6.85 | 1.33 | - | |||||||||||||||||||||||||||
成分C質量(%) | 1.3 | 5.1 | 6.5 | 5.1 | - | - | - | - | 1.3 | 5.1 | 6.5 | 5.1 | - | |||||||||||||||||||||||||||
成分D質量(%) | 0.08 | 0.14 | 2.1 | 0.14 | - | - | - | - | 0.08 | 0.14 | 2.1 | 0.14 | - | |||||||||||||||||||||||||||
成分E質量(%) | 0.009 | 0.215 | 4.309 | 0.215 | - | 0.009 | 0.215 | 4.309 | 0.009 | 0.215 | 4.309 | 0.215 | - | |||||||||||||||||||||||||||
椰子醯胺MEA | - | - | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||||||
月桂醯胺MEA | - | - | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||||||
成分A~E之R 1~R 6之碳數 | (A,17) (B,17) (C,17) (D,17) (E,17) | (A,17) (B,17) (C,17) (D,17) (E,17) | (A,17) (B,17) (C,17) (D,17) (E,17) | (B,17) (C,17) (D,17) (E,17) | (A,17) | (A,11) (B,11) (E,21) | (A,11) (B,11) (E,21) | (A,11) (B,11) (E,21) | (A,21) (B,21) (C,21) (D,21) (E,21) | (A,21) (B,21) (C,21) (D,21) (E,21) | (A,21) (B,21) (C,21) (D,21) (E,21) | (B,21) (C,21) (D,21) (E,21) | (A,21) | |||||||||||||||||||||||||||
成分A~D之M 1~M 7 | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | |||||||||||||||||||||||||||
混合溶液之pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||||||||||
配方評價 | ||||||||||||||||||||||||||||||||||||||||
pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||||||||||
乳化穩定性確認試驗1 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | |
棕櫚酸乙基己酯 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 4 | 2 | 1 | |
橄欖油 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | 5 | 5 | 5 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 1 | 1 | 4 | 2 | 1 | |
礦物油 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 1 | 5 | 3 | 1 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 5 | 3 | 1 | |
環甲矽脂 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 1 | 1 | 3 | 1 | 1 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 4 | 2 | 1 | 4 | 2 | 1 | |
矽靈 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 2 | 1 | 4 | 2 | 1 | 5 | 5 | 4 | 5 | 5 | 3 | 5 | 5 | 3 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 1 | 5 | 3 | 1 | |
乳化穩定性確認試驗2 | ||||||||||||||||||||||||||||||||||||||||
鯨蠟硬脂醇 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 1 | 4 | 2 | 1 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 4 | 3 | 1 | 4 | 2 | 1 | |
肉豆蔻醇 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 5 | 3 | 1 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
分散穩定性確認試驗 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | |
5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 3 | 2 | 1 | 5 | 5 | 3 | 5 | 5 | 4 | 5 | 5 | 2 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 4 | 2 | 1 | ||
官能評價 | ||||||||||||||||||||||||||||||||||||||||
水潤性 | 5 | 5 | 5 | 3 | 2 | 5 | 5 | 5 | 5 | 5 | 5 | 2 | 3 | |||||||||||||||||||||||||||
是否黏膩 | 5 | 5 | 4 | 1 | 3 | 5 | 5 | 5 | 5 | 5 | 4 | 1 | 2 | |||||||||||||||||||||||||||
濃厚感 | 5 | 5 | 5 | 2 | 2 | 5 | 5 | 5 | 5 | 5 | 5 | 2 | 2 | |||||||||||||||||||||||||||
延展之良好性 | 5 | 5 | 5 | 2 | 3 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 3 | |||||||||||||||||||||||||||
光滑性 | 5 | 5 | 5 | 3 | 2 | 5 | 5 | 5 | 5 | 5 | 5 | 2 | 3 |
[表4-1]
表4-1 | |||||||||||||||||||||||||||||||
編號 | 實施例54 | 實施例55 | 實施例56 | 比較例20 | 比較例21 | 實施例57 | 實施例58 | 實施例59 | 比較例22 | 比較例23 | |||||||||||||||||||||
組合物 | |||||||||||||||||||||||||||||||
成分A | 有 | 有 | 有 | 無 | 有 | 有 | 有 | 有 | 無 | 有 | |||||||||||||||||||||
成分B比率(%) | 0.032 | 1.33 | 6.85 | 1.33 | - | 0.032 | 1.33 | 6.85 | 1.33 | - | |||||||||||||||||||||
成分C質量(%) | 1.3 | 5.1 | 6.5 | 5.1 | - | 1.3 | 5.1 | 6.5 | 5.1 | - | |||||||||||||||||||||
成分D質量(%) | 0.08 | 0.14 | 2.1 | 0.14 | - | 0.08 | 0.14 | 2.1 | 0.14 | - | |||||||||||||||||||||
成分E質量(%) | 0.009 | 0.215 | 4.309 | 0.215 | - | 0.009 | 0.215 | 4.309 | 0.215 | - | |||||||||||||||||||||
椰子醯胺MEA | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||
月桂醯胺MEA | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||
成分A~E之R 1~R 6之碳數 | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (B,11) (C,11) (D,11) (E,11) | (A,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (B,11) (C,11) (D,11) (E,11) | (A,11) | |||||||||||||||||||||
成分A~D之M 1~M 7 | K | K | K | K | K | TEA | TEA | TEA | TEA | TEA | |||||||||||||||||||||
混合溶液之pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||||
配方評價 | |||||||||||||||||||||||||||||||
pH值 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | 7 | |||||||||||||||||||||
乳化穩定性確認試驗1 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | |
棕櫚酸乙基己酯 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 1 | 4 | 2 | 1 | |
橄欖油 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 1 | 1 | 4 | 2 | 1 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 3 | 1 | 4 | 2 | 1 | |
礦物油 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 4 | 3 | 1 | 5 | 3 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 1 | 5 | 3 | 1 | |
環甲矽脂 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 4 | 2 | 1 | 4 | 2 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 4 | 2 | 1 | |
矽靈 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 5 | 3 | 1 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
乳化穩定性確認試驗2 | |||||||||||||||||||||||||||||||
鯨蠟硬脂醇 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
肉豆蔻醇 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 4 | 2 | 1 | |
分散穩定性確認試驗 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | |
5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 3 | 2 | 1 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 5 | 2 | 1 | ||
官能評價 | |||||||||||||||||||||||||||||||
水潤性 | 5 | 5 | 5 | 3 | 3 | 5 | 5 | 5 | 3 | 3 | |||||||||||||||||||||
是否黏膩 | 5 | 5 | 4 | 1 | 2 | 5 | 5 | 5 | 2 | 2 | |||||||||||||||||||||
濃厚感 | 5 | 5 | 5 | 3 | 2 | 5 | 5 | 5 | 3 | 3 | |||||||||||||||||||||
延展之良好性 | 5 | 5 | 5 | 2 | 3 | 5 | 5 | 4 | 2 | 3 | |||||||||||||||||||||
光滑性 | 5 | 5 | 5 | 2 | 2 | 4 | 5 | 5 | 1 | 3 |
[表4-2]
表4-2 | ||||||||||||||||
編號 | 實施例60 | 實施例61 | 實施例62 | 比較例24 | 比較例25 | |||||||||||
組合物 | ||||||||||||||||
成分A | 有 | 有 | 有 | 無 | 有 | |||||||||||
成分B比率(%) | 0.032 | 1.33 | 6.85 | 1.33 | - | |||||||||||
成分C質量(%) | 1.3 | 5.1 | 6.5 | 5.1 | - | |||||||||||
成分D質量(%) | 0.08 | 0.14 | 2.1 | 0.14 | - | |||||||||||
成分E質量(%) | 0.009 | 0.215 | 4.309 | 0.215 | - | |||||||||||
椰子醯胺MEA | - | - | - | - | - | |||||||||||
月桂醯胺MEA | - | - | - | - | - | |||||||||||
成分A~E之R 1~R 6之碳數 | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (B,11) (C,11) (D,11) (E,11) | (A,11) | |||||||||||
成分A~D之M 1~M 7 | Arg | Arg | Arg | Arg | Arg | |||||||||||
混合溶液之pH值 | 7 | 7 | 7 | 7 | 7 | |||||||||||
配方評價 | ||||||||||||||||
pH值 | 7 | 7 | 7 | 7 | 7 | |||||||||||
乳化穩定性確認試驗1 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | |
棕櫚酸乙基己酯 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 1 | 4 | 2 | 1 | |
橄欖油 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 5 | 3 | 1 | |
礦物油 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
環甲矽脂 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
矽靈 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 4 | 2 | 1 | |
乳化穩定性確認試驗2 | ||||||||||||||||
鯨蠟硬脂醇 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 4 | 2 | 1 | |
肉豆蔻醇 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
分散穩定性確認試驗 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | |
5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 1 | 1 | 3 | 1 | 1 | ||
官能評價 | ||||||||||||||||
水潤性 | 5 | 5 | 4 | 2 | 3 | |||||||||||
是否黏膩 | 5 | 5 | 5 | 1 | 3 | |||||||||||
濃厚感 | 5 | 5 | 5 | 2 | 3 | |||||||||||
延展之良好性 | 5 | 5 | 5 | 3 | 2 | |||||||||||
光滑性 | 4 | 5 | 5 | 2 | 3 |
[表5-1]
表5-1 | ||||||||||||||||||||||||||||||||||
編號 | 實施例63 | 實施例64 | 實施例65 | 實施例66 | 實施例67 | 實施例68 | 實施例69 | 實施例70 | 實施例71 | 比較例26 | 比較例27 | |||||||||||||||||||||||
組合物 | ||||||||||||||||||||||||||||||||||
成分A | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 無 | 有 | |||||||||||||||||||||||
成分B比率(%) | 0.032 | 1.33 | 6.85 | 0.032 | 1.33 | 6.85 | 0.032 | 1.33 | 6.85 | 1.33 | - | |||||||||||||||||||||||
成分C質量(%) | - | - | - | - | - | - | 1.3 | 5.1 | 6.5 | 5.1 | - | |||||||||||||||||||||||
成分D質量(%) | - | - | - | - | - | - | 0.08 | 0.14 | 2.1 | 0.14 | - | |||||||||||||||||||||||
成分E質量(%) | - | - | - | 0.009 | 0.215 | 4.309 | 0.009 | 0.215 | 4.309 | 0.215 | - | |||||||||||||||||||||||
椰子醯胺MEA | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||
月桂醯胺MEA | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||
成分A~E之R 1~R 6之碳數 | (A,11) (B,11) | (A,11) (B,11) | (A,11) (B,11) | (A,11) (B,11) (E,11) | (A,11) (B,11) (E,11) | (A,11) (B,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (B,11) (C,11) (D,11) (E,11) | (A,11) | |||||||||||||||||||||||
成分A~D之M 1~M 7 | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | |||||||||||||||||||||||
混合溶液之pH值 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | |||||||||||||||||||||||
配方評價 | ||||||||||||||||||||||||||||||||||
pH值 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | |||||||||||||||||||||||
乳化穩定性確認試驗1 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | |
棕櫚酸乙基己酯 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 4 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 4 | 3 | 1 | 4 | 1 | 1 | |
橄欖油 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 2 | 2 | 1 | 5 | 3 | 1 | |
礦物油 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 1 | 4 | 2 | 1 | |
環甲矽脂 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 1 | 1 | 4 | 2 | 1 | |
矽靈 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 3 | 2 | 1 | |
乳化穩定性確認試驗2 | ||||||||||||||||||||||||||||||||||
鯨蠟硬脂醇 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
肉豆蔻醇 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 5 | 3 | 1 | |
分散穩定性確認試驗 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | |
5 | 3 | 2 | 5 | 4 | 3 | 4 | 2 | 1 | 5 | 5 | 2 | 5 | 5 | 4 | 5 | 4 | 2 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 4 | 2 | 1 | ||
官能評價 | ||||||||||||||||||||||||||||||||||
水潤性 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 3 | 2 | |||||||||||||||||||||||
是否黏膩 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 1 | 3 | |||||||||||||||||||||||
濃厚感 | 3 | 3 | 3 | 3 | 3 | 3 | 5 | 5 | 5 | 2 | 2 | |||||||||||||||||||||||
延展之良好性 | 3 | 3 | 3 | 5 | 5 | 4 | 5 | 5 | 4 | 2 | 3 | |||||||||||||||||||||||
光滑性 | 3 | 3 | 3 | 4 | 5 | 5 | 4 | 5 | 5 | 2 | 3 |
[表5-2]
表5-2 | ||||||||||||||||||||||||||||||||||
編號 | 實施例72 | 實施例73 | 實施例74 | 實施例75 | 實施例76 | 實施例77 | 實施例78 | 實施例79 | 實施例80 | 比較例28 | 比較例29 | |||||||||||||||||||||||
組合物 | ||||||||||||||||||||||||||||||||||
成分A | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 無 | 有 | |||||||||||||||||||||||
成分B比率(%) | 0.032 | 1.33 | 6.85 | 0.032 | 1.33 | 6.85 | 0.032 | 1.33 | 6.85 | 1.33 | - | |||||||||||||||||||||||
成分C質量(%) | - | - | - | - | - | - | 1.3 | 5.1 | 6.5 | 5.1 | - | |||||||||||||||||||||||
成分D質量(%) | - | - | - | - | - | - | 0.08 | 0.14 | 2.1 | 0.14 | - | |||||||||||||||||||||||
成分E質量(%) | - | - | - | 0.009 | 0.215 | 4.309 | 0.009 | 0.215 | 4.309 | 0.215 | - | |||||||||||||||||||||||
椰子醯胺MEA | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||
月桂醯胺MEA | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||
成分A~E之R 1~R 6之碳數 | (A,11) (B,11) | (A,11) (B,11) | (A,11) (B,11) | (A,11) (B,11) (E,11) | (A,11) (B,11) (E,11) | (A,11) (B,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (B,11) (C,11) (D,11) (E,11) | (A,11) | |||||||||||||||||||||||
成分A~D之M 1~M 7 | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | |||||||||||||||||||||||
混合溶液之pH值 | 9 | 9 | 9 | 9 | 9 | 9 | 9 | 9 | 9 | 9 | 9 | |||||||||||||||||||||||
配方評價 | ||||||||||||||||||||||||||||||||||
pH值 | 9 | 9 | 9 | 9 | 9 | 9 | 9 | 9 | 9 | 9 | 9 | |||||||||||||||||||||||
乳化穩定性確認試驗1 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | |
棕櫚酸乙基己酯 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 4 | 4 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 1 | 4 | 2 | 1 | |
橄欖油 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 4 | 3 | 5 | 5 | 5 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 5 | 3 | 1 | |
礦物油 | 5 | 3 | 3 | 5 | 4 | 3 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 1 | 4 | 2 | 1 | |
環甲矽脂 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 3 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
矽靈 | 5 | 3 | 2 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 1 | 1 | 5 | 3 | 1 | |
乳化穩定性確認試驗2 | ||||||||||||||||||||||||||||||||||
鯨蠟硬脂醇 | 5 | 3 | 2 | 5 | 4 | 3 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
肉豆蔻醇 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 2 | 1 | 1 | 3 | 1 | 1 | |
分散穩定性確認試驗 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | |
5 | 4 | 2 | 5 | 4 | 2 | 4 | 2 | 1 | 5 | 5 | 3 | 5 | 5 | 3 | 5 | 5 | 2 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | ||
官能評價 | ||||||||||||||||||||||||||||||||||
水潤性 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 3 | |||||||||||||||||||||||
是否黏膩 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 2 | 3 | |||||||||||||||||||||||
濃厚感 | 3 | 3 | 3 | 3 | 3 | 3 | 5 | 5 | 5 | 2 | 2 | |||||||||||||||||||||||
延展之良好性 | 3 | 3 | 3 | 5 | 5 | 4 | 5 | 5 | 5 | 3 | 3 | |||||||||||||||||||||||
光滑性 | 3 | 3 | 3 | 4 | 5 | 5 | 5 | 5 | 5 | 3 | 2 |
[表5-3]
表5-3 | ||||||||||||||||||||||||||||||||||
編號 | 實施例81 | 實施例82 | 實施例83 | 實施例84 | 實施例85 | 實施例86 | 實施例87 | 實施例88 | 實施例89 | 比較例30 | 比較例31 | |||||||||||||||||||||||
組合物 | ||||||||||||||||||||||||||||||||||
成分A | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 有 | 無 | 有 | |||||||||||||||||||||||
成分B比率(%) | 0.032 | 1.33 | 6.85 | 0.032 | 1.33 | 6.85 | 0.032 | 1.33 | 6.85 | 1.33 | - | |||||||||||||||||||||||
成分C質量(%) | - | - | - | - | - | - | 1.3 | 5.1 | 6.5 | 5.1 | - | |||||||||||||||||||||||
成分D質量(%) | - | - | - | - | - | - | 0.08 | 0.14 | 2.1 | 0.14 | - | |||||||||||||||||||||||
成分E質量(%) | - | - | - | 0.009 | 0.215 | 4.309 | 0.009 | 0.215 | 4.309 | 0.215 | - | |||||||||||||||||||||||
椰子醯胺MEA | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||
月桂醯胺MEA | - | - | - | - | - | - | - | - | - | - | - | |||||||||||||||||||||||
成分A~E之R 1~R 6之碳數 | (A,11) (B,11) | (A,11) (B,11) | (A,11) (B,11) | (A,11) (B,11) (E,11) | (A,11) (B,11) (E,11) | (A,11) (B,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (A,11) (B,11) (C,11) (D,11) (E,11) | (B,11) (C,11) (D,11) (E,11) | (A,11) | |||||||||||||||||||||||
成分A~D之M 1~M 7 | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | Na | |||||||||||||||||||||||
混合溶液之pH值 | 12 | 12 | 12 | 12 | 12 | 12 | 12 | 12 | 12 | 12 | 12 | |||||||||||||||||||||||
配方評價 | ||||||||||||||||||||||||||||||||||
pH值 | 12 | 12 | 12 | 12 | 12 | 12 | 12 | 12 | 12 | 12 | 12 | |||||||||||||||||||||||
乳化穩定性確認試驗1 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | 2.0個月後 | 2.5個月後 | 3.0個月後 | |
棕櫚酸乙基己酯 | 5 | 4 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 4 | 2 | 1 | |
橄欖油 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 2 | 2 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 5 | 3 | 1 | |
礦物油 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 2 | 1 | 4 | 2 | 1 | |
環甲矽脂 | 5 | 4 | 3 | 5 | 4 | 3 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 4 | 2 | 1 | |
矽靈 | 5 | 3 | 2 | 5 | 4 | 3 | 5 | 3 | 2 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 5 | 3 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 2 | 1 | 1 | 4 | 2 | 1 | |
乳化穩定性確認試驗2 | ||||||||||||||||||||||||||||||||||
鯨蠟硬脂醇 | 5 | 4 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 4 | 3 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 1 | 3 | 1 | 1 | |
肉豆蔻醇 | 5 | 3 | 3 | 5 | 3 | 2 | 5 | 3 | 2 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 3 | 1 | 1 | |
分散穩定性確認試驗 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | 200小時後 | 224小時後 | 248小時後 | |
5 | 4 | 2 | 5 | 4 | 3 | 4 | 2 | 1 | 5 | 5 | 3 | 5 | 5 | 3 | 5 | 4 | 3 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | 1 | 4 | 1 | 1 | ||
官能評價 | ||||||||||||||||||||||||||||||||||
水潤性 | 5 | 5 | 4 | 5 | 5 | 5 | 5 | 5 | 5 | 3 | 3 | |||||||||||||||||||||||
是否黏膩 | 5 | 5 | 5 | 5 | 5 | 4 | 5 | 5 | 5 | 3 | 3 | |||||||||||||||||||||||
濃厚感 | 3 | 3 | 3 | 3 | 3 | 3 | 5 | 5 | 5 | 2 | 2 | |||||||||||||||||||||||
延展之良好性 | 3 | 3 | 3 | 5 | 5 | 5 | 5 | 5 | 4 | 3 | 2 | |||||||||||||||||||||||
光滑性 | 3 | 3 | 3 | 5 | 5 | 5 | 4 | 5 | 5 | 2 | 3 |
實施例之組合物至少包含成分A及B;或至少包含成分A、C及D;或至少包含成分A及E,因此乳化穩定性、分散穩定性及使用感評價均良好。另一方面,比較例為不屬於發明之組合物,故而與實施例相比,乳化穩定性及分散穩定性均較差。
[產業上之可利用性]
根據本發明之香妝品原料組合物,可提供一種不僅初始之乳化性能或分散性能良好,而且乳化穩定性及分散性長期良好等優異之香妝品配方。
Claims (16)
- 一種組合物,其特徵在於含有:下述成分A、及 選自由下述成分B、下述成分C、下述成分D及下述成分E所組成之群中之1種以上之成分(其中,單為上述成分C除外或單為上述成分D除外), 成分A:下述通式(A)所表示之含有醯基之胺基酸衍生物或其鹽 [化1] (式(A)中, R 1及R 2分別獨立地為飽和或不飽和之直鏈或支鏈狀烴基, M 1、M 2及M 3分別獨立地為氫原子、鹼金屬、鹼土類金屬、有機或無機胺、鹼性胺基酸、膽鹼、鋁或鋅, n 1及n 2為0及2,或者為2及0, n 3及n 4為0及2,或者為2及0) 成分B:下述通式(B)所表示之N-醯基吡咯啶酮羧酸或其鹽 [化2] (式(B)中, R 3為飽和或不飽和之直鏈或支鏈狀烴基, M 4為氫原子、鹼金屬、鹼土類金屬、有機或無機胺、鹼性胺基酸、膽鹼、鋁或鋅) 成分C:下述通式(C)所表示之醯基麩胺酸或其鹽 [化3] (式(C)中, R 4為飽和或不飽和之直鏈或支鏈狀烴基, M 5及M 6分別獨立地為氫原子、鹼金屬、鹼土類金屬、有機或無機胺、鹼性胺基酸、膽鹼、鋁或鋅) 成分D:下述通式(D)所表示之脂肪酸或其鹽 [化4] (式(D)中, R 5為飽和或不飽和之直鏈或支鏈狀烴基, M 7為氫原子、鹼金屬、鹼土類金屬、有機或無機胺、鹼性胺基酸、膽鹼、鋁或鋅) 成分E:下述通式(E)所表示之脂肪酸醯胺 [化5] (式(E)中, R 6為飽和或不飽和之直鏈或支鏈狀烴基)。
- 如請求項1之組合物,其含有上述成分A及上述成分B。
- 如請求項1之組合物,其含有上述成分A及上述成分E。
- 如請求項1之組合物,其含有上述成分A、上述成分B及上述成分E。
- 如請求項1至4中任一項之組合物,其中上述通式(A)~(E)中之R 1~R 6分別獨立地為碳化數1~29之烴基。
- 如請求項1至5中任一項之組合物,其中上述通式(A)~(D)中之M 1~M 7分別獨立地為Na、K、三乙醇胺、Mg、Ca、Al、Zn、精胺酸或H。
- 如請求項1、2、4、5及6中任一項之組合物,其中上述成分B相對於上述成分A之比率為0.004%以上。
- 如請求項1及5至7中任一項之組合物,其中以上述成分A與上述成分C之合計質量為基準,上述成分C之量為0.8質量%以上,且 以上述成分A與上述成分D之合計質量為基準,上述成分D之量為0.06質量%以上。
- 如請求項1及3至8中任一項之組合物,其中以上述成分A之質量為基準,上述成分E之量為0.005質量%以上。
- 一種如請求項1、2及4至9中任一項之組合物之製造方法,其包括如下步驟: 1)於包含水及有機溶劑之混合溶劑中,使麩胺酸或其鹽與脂肪醯氯進行反應,獲得包含N-醯基麩胺酸或其鹽之反應液,利用酸使上述反應液之pH值成為1~6,於25~80℃之溫度下分層為有機層與水層; 2)於酸性下對上述有機層進行濃縮乾燥,將上述N-醯基麩胺酸或其鹽之一部分轉化為N-醯基吡咯啶酮羧酸或其鹽; 3)使上述N-醯基麩胺酸或其鹽與酸酐進行反應,而獲得N-醯基麩胺酸酐;及 4)使上述N-醯基麩胺酸酐與離胺酸或其鹽進行反應,而獲得含有醯基之胺基酸衍生物或其鹽。
- 如請求項10之製造方法,其中於上述步驟2)中,對上述有機相進行濃縮乾燥直至乾燥減量達到10質量%以下為止。
- 如請求項10或11之製造方法,其於減壓下且於50℃以上實施上述步驟2)中之濃縮乾燥。
- 如請求項1至9中任一項之組合物,其係香妝品原料組合物。
- 一種如請求項1至9中任一項之組合物之用途,其係用作香妝品原料。
- 一種化妝料,其調配有如請求項1至9中任一項之組合物。
- 如請求項15之化妝料,其pH值為4以上。
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