東京都健康安全研究センター研究年報

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1 Ann. Rep. Tokyo Metr. Inst. P.H., 55, 2004 化粧品に配合される新規頭髪用染料の分析法 Analysis of ew Hair Colorants of Cosmetics ahomi UKI Yoshiaki AKAMURA Ken'ichiro MORI Kiyosi TERASHIMA Toshiro YOKOYAMA and Kouichi IT A rapid and simple analysis by HPLC was developed to determine the suitability of 14 new synthetic hair colorants for cosmetics. The analytical procedure was as follows The samples were diluted with 50% methanol and injected into HPLC The HPLC conditions were as follows HPLC column ODS (4.6 mm i.d. 150 mm), mobile phase 1 Methanol / H2O linear gradient mobile phase % phophoric acid including 0.5% sodium 1-decanesulfonate / Methanol(40:60), photodiode-array nm column temperature 40 The 14 new hair colorants were separated for about 30 min and were identified from the absorbant spectra of each peak By using this method new hair colorants used in 15 commercial cosmetics were determined to have good handling quality Keywords HPLC cosmetics hair colorant semipermanent hair dye preparation analysis はじめに 13 1) ) 3), ). Cosmetic Ingredient Review Expert Panel (CIR) 5) 14 HPLC 方法 1. 試薬 Fig.1 3( AO3 ) HC 3( HR3) HC 4( ) HC 1( ) HC 2( ) 9( ) Huwell Chemicals HC 1( HR1) HC 2( ) Jos. H. Lowenstein & Sons. Inc ( ACP) Aldrich 76( ) 57( ) 16( ) 17( ) 99( ) ( ) Tokyo Metropolitan Institute of Public Health , Hyakunin-cho, Shinjuku-ku, Tokyo Japan

2 80 Ann. Rep. Tokyo Metr. Inst. P.H., 55, 2004 O 2 SO 3 a O 2 O 2 O 2 H H H H 2 H 2 CH 2 CH H 2 AO1 HR1 HR3 O 2 H HCH 2 CH 2 O 2 OCH 2 CH 2 HCH 2 CH 2 HCH 2 CH 2 O 2 O 2 (CH 2 CH 2 ) 2 Cl H 2 O 2 ACP OCH 3 (CH 3 ) 3 (CH 3 ) 3 H 3 C CH 2 CH 2 CH 2 CH 2 H 2 O 2 H 2 Br O H H (CH 3 ) 3 (CH 3 ) 3 (CH 3 ) 3 Fig.1. Structure of ew Hair Colorants Table1. ICI ame of ew Hair Colorants ICI name Abbreviation Analytical Wavelength (nm) Acid Orange o.3 AO3 360 HC Red o.1 HR1 500 HC Red o.3 HR3 500 HC Orange o HC Yellow o HC Yellow o HC Blue o Disperse Black o amino-6-chloro-4- nitrophenol ACP 320 Basic red o Basic Yellow o Basic Brown o Basic Brown o Basic Blue o.99 6 ICI : International omenclature for Cosmetic Ingredients 97 0 % ICI Table1. ( ) ( ) 2. 試料標準溶液の調製 0.01 g 50 % ml 1,000 g/ml HR1 AO3 HR3 1.0 ml ml 0 g/ml g/ml ACP 4. 添加回収試験用試料溶液の調製 g mg ( ) HM g ml 5. 試験溶液の調製 ml 0.5 g / (1:1) ml (2,500 rpm )

3 55, Table 2. Linear Gradient Condition of Mobile Phase1 Time(min) A(%) B(%) A:35%Methanol B:80%Methanol Retention time (min) AO3 HR1 HR3 6.HPLC 条件 ( ) TSKgel-ODS80TM 4.6 mm i.d. 150 mm ( ) ) 35 % 80 % Table % 1- (SDeS) 0.04 % (40 60) 40 1 ml/min nm L 結果および考察 1. 分析条件の検討 1) リニアグラジエント条件 HR1 AO3 HR3 TSKgel-ODS80TM 40 1 ml/min Fig.2 (30:70) HR3 30 HR1 AO % AO3 HR % % 30 2) 単一条件 ACP 0.04 % (4:6) 0.04 % (4:6) 0.5 % (SHS) (SOS) (SDeS Fig. 3 SDeS Retention time (min) Fig.2. Effect of Methanol Concentration in Methanol/H 2 O SolutionSystem on Retention Time of ew Hair Colorants % 35% 40% 50% Gradient condition Concentration of methanol (%) ACP 0% 0.5%SHS 0.5%SOS 0.5%SDeS Counter ion Fig.3. Effect of Counter Ions in 0.04% Phosphoric Acid/ Methanol (40:60) on Retention Time of ew Hair Colorants 1) 2) Fig.4 Fig g/ml R= (n=5) cv 1.3 % AO3 358nm ACP 320nm 382nm (Table 1) 0 g/ml AO3 ACP

4 82 Ann. Rep. Tokyo Metr. Inst. P.H., 55, Abs Abs (min) Fig.4. Chromatogram of ew Hair Colorants 1:HR3, 2:, 3:, 4:, 5:, 6:HR1, 7:, 8:AO3, 9:ACP, :, 11:, 12:, 13:, 14: A:Mobile Phase 1;Me/H2O gradient system (Table 2) B:Mobile Phase 2;0.04% phosphoric acid, 0.5% sodium 1- decanesulfonate/methanol (40:60) Detection:254nm AO HR1 HR (nm) 800 Fig.5-1. Spectrums Wavelength of ew [nm] Hair Colorants (1) ACP (nm) 800 Fig.5-2. Spectrums Wavelength of ew [nm] Hair Colorats (2) 14 A B Table 3. Recoveries of ew Hair Colorant Cosmetics Added hair Recovery Coefficient colorant rate (%) of Variation Shampoo HR HR AO ACP Hair rinse HR HR AO ACP added : 0.1%, n=5 2 g/ml HR1 5 g/ml g/ml 25 g/ml 2. 前処理法の検討 0.1 % 1 ml ml 0.5 g HPLC 3. 添加回収試験 % 5) 0.1

5 55, Cosmetics Shampoo Hair rinse Hair coloring preparation Table 4. Analytical Results of ew Hair Colorants Extracted from Commercial Cosmetics Country of origin Indication Result 1 Japan,,, 2 Japan,,,, HY5, HR3, 3 Malaysia hennna,,,,,, 1 Japan, HR3,,,,, HR3,,,, 2 Japan,,,, HY5,,,,,, HR3,, 3 Japan hennna,,,,, 4 Spain hennna,, 5 Malaysia hennna,,,,,,,, 1 Japan hennna,, 2 Japan hennna,, 3 Japan hennna,,,, 4 Malaysia hennna,,,,,,, 1) 5 Malaysia hennna,,,,,,, 1) 6 Malaysia hennna,,,,,,,, 7 Brazil hennna HR1,, HR1,, 1), 1), 1) 1) Un-indicated hair colorant was detected. Table % % % % 4. 市販化粧品の分析 15 Table ) まとめ HPLC g/ml g/ml 1.3 % 文献 1) ) FRAGRACE JOURAL, 1, 13-14, ) FRAGRACE JOURAL, 5, 13, ), 5) FRAGRACE JOURAL, 8, 16-27, ) Le Coz, C-J., Kuhne, S., and Engel, F. : COTACT DERMATITIS, 49, 3, 2003.

東京都健康安全研究センター研究年報

東京都健康安全研究センター研究年報東京健安研セ年報 Ann. Rep. Tokyo Metr. Inst.P.H., 56, 7-, 005 毛髪用化粧品に配合される新規染毛用色素の分析法大貫奈穂美 *, 中村義昭 *, 森謙一郎 *, 寺島潔 *, 横山敏郎 * *, 荻野周三 Analysis of ew Hair Colorants for Cosmetics ahomi UKI *,Yoshiaki AKAMURA *,Ken'ichiro