Patent ID: 12246083

EXAMPLES

Process of Manufacture of Sunscreen Compositions

The ingredients of part A, as well as the ingredients of part B as provided below in Tables 1.1, 1.2, 1.3 and 1.4 for each tested sunscreen composition were combined and heated to 80° C. respectively, wherein part A was added to part B under stirring and was further homogenized. Subsequently, the sunscreen composition was cooled down to room temperature under stirring and the pH of each composition was adjusted to 6.5-7.00 with NaOH (30%).

All amounts referred to in the following tables refer to the respective amounts in % by weight, based on the total weight of the composition.

Sunscreen Compositions

TABLE 1.1Recovery of EHTIngredientComparativeComparativeComp.Comp.Comp.Comp.Comp.Comp.Comp.Comp.Comp.(Trade Name)Comp. 1aComp. 1b2a2b2c2d2e2f2g2h2iPart ADibutyl adipate15.0015.0015.0015.0015.0015.0015.0015.0015.0015.0015.00(Cetiol B)C12-C15alkyl benzoate10.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.00(Cetiol AB)Stearyl alcohol (Lanette2.502.502.502.502.502.502.502.502.502.502.5018)Polyester-8——3.00————————(Polycrylene)Diethylhexyl 2,6-naph-———3.00———————thalate (Corapan TQ)Ethylhexyl methoxy-————3.00——————crylene (SolaStay S1)Trimethoxybenzylidene—————2.00—————pentanedione (SynoxylHSS)Polyester-25——————3.00————(Bis-Methoxycrylene/octyldodecyl adipicacid/methylpropane-diolcopolymer)Micah (=fused ring———————3.00———cyanoacrylatederivative)Butyloctyl Salicylate————————3.00——Benzotriazolyl Dodecyl—————————1.00—p CresolDiethylhexyl——————————1.00SyringylidenemalonateBMDBM—2.002.002.002.002.002.002.002.002.002.00EHT (Uvinul T150)1.001.001.001.001.001.001.001.001.001.001.00BEMT (Tinosorb S)———————————Part BWaterqspqspqspqspqspqspqspqspqspqspqsp100%100%100%100%100%100%100%100%100%100%100%Glycerin2.002.002.002.002.002.002.002.002.002.002.00Disodium EDTA0.200.200.200.200.200.200.200.200.200.200.20(EDTA BD)Acrylates/Beheneth-252.002.002.002.002.002.002.002.002.002.002.00methacrylate copolymer(Tinovis GTC UP)Xanthan Gum0.500.500.500.500.500.500.500.500.500.500.50(Rheocare XGN)

TABLE 1.2Recovery of BEMTIngredientComparativeComparativeComp.Comp.Comp.Comp.Comp.Comp.Comp.Comp.(Trade Name)Comp. 1cComp. 1d3a3b3c3d3e3f3g3hPart ADibutyl adipate10.0010.0010.0010.0010.0010.0010.0010.0010.0010.00(Cetiol B)C12-C15alkyl benzoate10.0010.0010.0010.0010.0010.0010.0010.0010.0010.00(Cetiol AB)Stearyl alcohol2.502.502.502.502.502.502.502.502.502.50(Lanette 18)Polyester-8——3.00———————(Polycrylene)Diethylhexyl 2,6-naph-———3.00——————thalate (Corapan TQ)Ethylhexyl methoxy-————3.00—————crylene (SolaStay Si)Trimethoxybenzylidene—————3.00————pentanedione (SynoxylHSS)Polyester-25———————3.00—(Bis-Methoxycrylene/octyldodecyl adipicacid/methylpropane-diolcopolymer)Micah (=fused ring———————3.00——cyanoacrylatederivative)Benzotriazolyl Dodecyl—————————1.00p CresolBMDBM—3.003.003.003.003.003.003.003.003.00EHT (Uvinul T150)——————————BEMT (Tinosorb S)1.001.001.001.001.001.001.001.001.001.00Part BWaterqspqspqspqspqspqspqspqspqspqsp100%100%100%100%100%100%100%100%100%100%Glycerin2.002.002.002.002.002.002.002.002.002.00Disodium EDTA0.200.200.200.200.200.200.200.200.200.20(EDTA BD)Acrylates/Beheneth-252.002.002.002.002.002.002.002.002.002.00methacrylate copolymer(Tinovis GTC UP)Xanthan Gum0.500.500.500.500.500.500.500.500.500.50(Rheocare XGN)

TABLE 1.3Recovery of DBTIngredientComparativeComparativeComp.Comp.Comp.(Trade Name)Comp. 1eComp. 1f4a4b4cPart ADibutyl adipate15.0015.0015.0015.0015.00(Cetiol B)C12-C15alkyl benzoate10.0010.0010.0010.0010.00(Cetiol AB)Stearyl alcohol2.502.502.502.502.50(Lanette 18)Polyester-8——3.00——(Polycrylene)Diethylhexyl 2,6-naph-———3.00—thalate (Corapan TQ)Butyloctyl Salicylate————3.00BMDBM—2.002.002.002.00DBT (Uvasorb H EB)1.001.001.001.001.00Part BWaterqspqspqspqspqspGlycerin100%100%100%100%100%Disodium EDTA2.002.002.002.002.00(EDTA BD)0.200.200.200.200.20Acrylates/Beheneth-252.002.002.002.002.00methacrylate copolymer(Tinovis GTC UP)Xanthan Gum0.500.500.500.500.50(Rheocare XGN)

TABLE 1.4Recovery of BEMT + EHTIngredientComparativeComparativeComp.Comp.Comp.Comp.(Trade Name)Comp. 1gComp. 1h5a5b5c5dPart ADibutyl adipate15.0015.0015.0015.0015.0015.00(Cetiol B)C12-C15alkyl benzoate10.0010.0010.0010.0010.0010.00(Cetiol AB)Stearyl alcohol2.502.502.502.502.502.50(Lanette 18)Polyester-8——————(Polycrylene)Diethylhexyl 2,6-naph-———3.00thalate (Corapan TQ)Ethylhexyl3.00methoxycrylene(SolaStay Si)Trimethoxybenzyli-———3.00dene pentanedione(Synoxyl HSS)Butyloctyl Salicylate3.00BMDBM—3.003.003.003.003.00EHT (Uvinul T150)1.001.001.001.001.001.00BEMT (Tinosorb S)1.001.001.001.001.001.00Part BWaterqspqspqspqspqspqsp100%100%100%100%100%100%Glycerin2.002.002.002.002.002.00Disodium EDTA0.200.200.200.200.200.20(EDTA BD)Acrylates/Beheneth-252.002.002.002.002.002.00methacrylate copolymer(Tinovis GTC UP)Xanthan Gum0.500.500.500.500.500.50(Rheocare XGN)
Recovery Measurements on Photo Stability of EHT

The UV filter compositions as defined in Tables 1.1 to 1.4 are applied on roughened quartz plates (2 ml/cm2). Plates are irradiated using Atlas CPS device at different duration times (MED=Minimal Erythema Dose):0 h (0 MED, no irradiation)1 h (5 MED),2 h (10 MED),4 h (20 MED).

In total, four plates are prepared for each irradiation condition. After irradiation, each plate is rinsed off with tetrahydrofuran. The rinsing solution is further analyzed via HPLC to determine the recovery of EHT.

TABLE 2.1ComparativeComparativeComp.Comp.Comp.Comp. 1aComp. 1b2a2b2c0 MED100%100%100%100%100%5 MED97%92%97%94%102%10 MED94%79%100%87%101%20 MED90%31%88%79%100%Comp. 2dComp. 2eComp. 2fComp. 2gComp. 2hComp. 2i0 MED100%100%100%100%100%100%5 MED99%106%102%92%101%99%10 MED102%100%102%87%96%85%20 MED96%96%98%68%85%49%A person skilled in the art is aware that data above 100% after irradiation are due to common measurement fluctuations.
Recovery Measurements on Photo Stability of BEMT

The UV filter compositions as defined in Table 1.2 are applied on roughened quartz plates (2 ml/cm2). Plates are irradiated using Atlas CPS device at different duration times (MED=Minimal Erythema Dose):0 h (0 MED, no irradiation)1 h (5 MED),2 h (10 MED),4 h (20 MED).

In total, four plates are prepared for each irradiation condition. After irradiation, each plate is rinsed off with tetrahydrofuran. The rinsing solution is further analyzed via HPLC to determine the recovery of BEMT.

TABLE 2.2ComparativeComparativeComp.Comp.Comp.Comp. 1cComp. 1d3a3b3c0 MED100%100%100%100%100%5 MED96%93%104%94%106%10 MED99%84%99%93%104%20 MED98%78%96%86%100%Comp. 3dComp. 3eComp. 3fComp. 3gComp. 3h0 MED100%100%100%100%100%5 MED94%96%98%102%102%10 MED94%92%99%98%98%20 MED92%86%95%90%90%A person skilled in the art is aware that data above 100% after irradiation are due to common measurement fluctuations.
Recovery Measurements on Photo Stability of DBT

The UV filter compositions as defined in Table 1.3 are applied on roughened quartz plates (2 ml/cm2). Plates are irradiated using Atlas CPS device at different duration times (MED=Minimal Erythema Dose):0 h (0 MED, no irradiation)1 h (5 MED),2 h (10 MED),4 h (20 MED).

In total, four plates are prepared for each irradiation condition. After irradiation, each plate is rinsed off with tetrahydrofuran. The rinsing solution is further analyzed via HPLC to determine the recovery of DBT.

TABLE 2.3ComparativeComparativeComp.Comp.Comp.Comp. 1eComp. if4a4b4c0 MED100%100%100%100%100%5 MED92%85%101%95%91%10 MED84%60%101%82%83%20 MED62%30%85%68%71%A person skilled in the art is aware that data above 100% after irradiation are due to common measurement fluctuations.

Recovery Measurements on Photo Stability of BEMT+EHT

The UV filter compositions as defined in Table 1.4 are applied on roughened quartz plates (2 ml/cm2). Plates are irradiated using Atlas CPS device at different duration times (MED=Minimal Erythema Dose):0 h (0 MED, no irradiation)1 h (5 MED),2 h (10 MED),4 h (20 MED),10 h (50 MED).

In total, four plates are prepared for each irradiation condition. After irradiation, each plate is rinsed off with tetrahydrofuran. The rinsing solution is further analyzed via HPLC to determine the recovery of BEMT+EHT.

TABLE 2.4ComparativeComparativeComp. 1gComp. 1hComp. 5aBEMTEHTBEMTEHTBEMTEHT0 MED100%100%100%100%100%100%5 MED102%103%93%95%97%97%10 MED99%99%87%89%99%99%20 MED100%100%74%76%97%98%50 MED99%99%53%47%92%95%Comp. 5bComp. ScComp. 5dBEMTEHTBEMTEHTBEMTEHT0 MED100%100%100%100%100%100%5 MED103%103%97%98%97%98%10 MED104%103%89%94%95%98%20 MED101%100%85%90%90%95%50 MED95%89%69%68%70%73%A person skilled in the art is aware that data above 100% after irradiation are due to common measurement fluctuations.