Preservation mixtures, and polymer solutions stabilized therewith
11737961 · 2023-08-29
Assignee
Inventors
- Bernd de Potzolli (Bad Duerkheim, DE)
- Monika Rausch (Dannstadt-Schauernheim, DE)
- Karin Juhkason (Niederkirchen, DE)
Cpc classification
A61K2800/30
HUMAN NECESSITIES
A61Q5/06
HUMAN NECESSITIES
International classification
Abstract
The present invention describes specific biocidally effective preservative mixtures and aqueous polymer solutions stabilized with these preservative mixtures and their use in cosmetic preparations, such as skin care and hair care compositions, and hairstyling products and in products for the home care sector.
Claims
1. An aqueous 2-methylisothiazolin-3-one-free polymer solution stabilized with a preservative mixture of phenoxyethanol and at least one further alcohol, wherein the polymer is selected from the group consisting of vinyllactam polymers, polyurethanes, and mixtures thereof, and wherein the preservative mixture comprises the following constituents as active biocidal ingredients: from 25 to 50% by weight of a mixture composed of 50% 3-phenylpropanol, 25% 1,3-propanediol, and 25% 1,2-octanediol, and from 50 to 75% by weight of phenoxyethanol, and the preservative mixture is used in an amount of from 0.10 to 1.40% by weight in the aqueous polymer solution, or the preservative mixture comprises the following constituents as active biocidal ingredients: from 20 to 57% by weight of a mixture composed of 50% 1,2-pentanediol, 30% 1,2-octanediol, and 20% 1,2-decanediol, and from 43 to 80% by weight of phenoxyethanol, and the preservative mixture is used in an amount of from 0.20 to 1.40% by weight in the aqueous polymer solution.
2. The polymer solution according to claim 1, wherein the vinyllactam polymer is a homopolymer or a copolymer of N-vinylpyrrolidone, 3-methyl-N-vinylpyrrolidone, 4-methyl-N-vinylpyrrolidone, 5-methyl-N-vinylpyrrolidone, N-vinylpiperidone, or N-vinylcaprolactam.
3. A cosmetic preparation or a product for the home care sector comprising the aqueous polymer solution according to claim 1.
4. The preparation or product according to claim 3 comprising skin care and hair care compositions.
5. A hairstyling product or a decorative cosmetics product or a hair and body cleaning product comprising the aqueous polymer solution according to claim 1.
6. The polymer solution according to claim 1 wherein the preservative mixture comprises from 25 to 50% by weight of a mixture composed of 50% 3-phenylpropanol, 25% 1,3-propanediol and 25% 1,2-octanediol, and from 50 to 75% by weight of phenoxyethanol, and the preservative mixture is used in an amount of from 0.10 to 0.65% by weight in the aqueous polymer solution.
7. The polymer solution according to claim 6 wherein the preservative mixture is used in an amount of from 0.10 to 0.40% by weight of the aqueous polymer solution.
8. The polymer solution according to claim 1 wherein the preservative mixture comprises from 20 to 57% by weight of a mixture composed of 50% 1,2-pentanediol, 30% 1,2-octanediol, and 20% 1,2-decanediol, and from 43 to 80% by weight of phenoxyethanol, and the preservative mixture is used in an the amount of from 0.20 to 0.80% by weight in the aqueous polymer solution.
9. The polymer solution according to claim 8 wherein the preservative mixture is used in an amount from 0.40 to 0.60% by weight in the aqueous polymer solution.
Description
EXAMPLES
(1) To ascertain the freedom from germs of the aqueous polymer solutions, germ loading tests were carried out which satisfy the requirements of the pharmacopeia for topical applications (e.g. PhEur., USP and JP). Furthermore, the “Koko test” was carried out which, compared to PhEur., provides up to six-fold inoculations with germs.
(2) The passed germ loading test according to Ph. Eur., 7th Edition with the stabilized aqueous polymer solutions exhibited after 28 days freedom from germs with regard to the tested strains Pseudomonas aeruginosa (ATCC 9027), Staphylococcus aureus (ATCC 6638), Candida albicans (ATCC 10231) and Aspergillus brasiliensis (ATCC 16404).
(3) Table 1 below shows by way of examples 1 to 18 polymer solutions according to the invention stabilized with various preservative mixtures in different concentrations. As can be seen, all of the stabilized polymer solutions pass the germ loading test. The polymer solutions of examples 1 to 15 comprise the preservative mixture in a very low concentration in the range from 0.4 to 0.8% by weight, the products being clear and not very odor-intensive. No phase separations are noted. It is noteworthy that the aqueous Luviskol K85/90 solutions with ethanol or isopropanol of examples 16 to 18 in combination with relatively high fractions of phenoxyethanol in a concentration in the range from 0.85 to 1.35% by weight can be effectively stabilized. Here, the boosting effect of ethanol or isopropanol on the phenoxyethanol is clear to see.
(4) The preservative used as a) comprises phenoxyethanol as individual component.
(5) The preservative mixture used as b) comprises the individual components in the following fractions:
(6) 42 to 48% phenylpropanol, 23 to 27% 1,2-octanediol and 27 to 33% 1,3-propanediol.
(7) The preservative mixture c) comprises the individual components as follows:
(8) 25 to 50% 1,2-pentanediol, 25 to 50% 1,2-octanediol and 10 to 25% 1,2-decanediol.
(9) The preservative mixture d) comprises 90% phenoxyethanol and 10% ethylhexylglyceryl.
(10) The preservative e) is either ethanol or isopropanol.
(11) TABLE-US-00001 TABLE 1 Concentration of Polymer in the individual Appearance aqueous components in the Germ of the polymer polymer solution loading stabilized Example solution Preservative mixture (% by weight test solution 1 Luviset a) 2-Phenoxyethanol a) 0.10 Passed Almost Clear * b) Phenylpropanol b) 0.30 clear 1,2-Octanediol 1,3-Propanediol 2 Luviset a) 2-Phenoxyethanol a) 0.40 Passed clear/almost Clear * b) Phenylpropanol b) 0.10 clear 1,2-Octanediol 1,3-Propanediol 3 Luviset a) Phenoxyethanol a) 0.1 Passed Almost Clear * c) 1,2-Pentanediol c) 0.45 clear, very 1,2-Octanediol slightly 1,2-Decanediol cloudy 4 Luviset a) Phenoxyethanol a) 0.45 Passed Almost Clear * c) 1,2-Pentanediol c) 0.25 clear 1,2-Octanediol 1,2-Decanediol) 5 Luvigel a) 2-Phenoyxethanol a) 0.35 Passed Clear Star ** b) Phenylpropanol b) 0.35 1,2-Octanediol 1,3-Propanediol 6 Luvigel a) Phenoxyethanol a) 0.2 Passed Clear Star ** c) 1,2-Pentanediol c) 0.6 1,2-Octanediol 1,2-Decanediol 7 Luvigel a) Phenoxyethanol a) 0.55 Passed Clear Star ** c) 1,2-Pentanediol c) 0.25 1,2-Octanediol 1,2-Decanediol 8 Luvigel a) 2-Phenoyxethanol a) 0.25 Passed Clear Star ** b) Phenylpropanol b) 0.55 1,2-Octanediol 1,3-Propanediol 9 Luviquat a) Phenoxyethanol a) 0.10 Passed Clear Hold*** b) Phenylpropanol b) 0.30 1,2-Octanediol 1,3-Propanediol 10 Luviquat a) Phenoxyethanol a) 0.40 Passed Clear Hold*** b) Phenylpropanol b) 0.10 1,2-Octanediol 1,3-Propanediol 11 Luviquat a) Phenoxyethanol a) 0.1 Passed Almost Hold*** c) 1,2-Pentanediol c) 0.45 clear, very 1,2-Octanediol slightly 1,2-Decanediol cloudy 12 Luviquat a) Phenoxyethanol a) 0.45 Passed Almost Hold*** c) 1,2-Pentanediol c) 0.25 clear 1,2-Octanediol 1,2-Decanediol 13 Luviskol a) Phenoxyethanol a) 0.15 Passed Clear K85/ b) Phenylpropanol b) 0.35 K90**** 1,2-Octanediol 1,3-Propanediol 14 Luviskol a) Phenoxyethanol a) 0.45 Passed Clear K85/ b) Phenylpropanol b) 0.25 K90**** 1,2-Octanediol 1,3-Propanediol 15 Luviskol a) Phenoxyethanol a) 0.50 Passed Clear/almost K85/ c) 1,2-Pentanediol c) 0.15 clear K90**** 1,2-Octanediol 1,2-Decanediol 16 Luviskol d) Phenoxyethanol d) 0.75 Passed Clear K 85**** Ethylhexylglyceryl e) 0.1 e) Ethanol 17 Luviskol d) Phenoxyethanol d) 1.00 Passed Clear K 85**** Ethylhexylglyceryl e) 0.1 e) Ethanol 18 Luviskol d) Phenoxyethanol d) 1.10 passed Clear K90***** Ethylhexylglyceryl e) 0.25 e) Isopropanol * = Copolymer of vinylpyrrolidone, methacrylamide and vinylimidazole 20% strength aqueous solution ** = Polyurethane -39, 20% strength aqueous solution ***= Polyquaternium -46, 20% strength aqueous solution ****= Polyvinylpyrrolidone, 20% strength aqueous solution
(12) Furthermore, comparative experiments with polymer solutions according to comparative examples 1 to 14 were carried out, which comprise either only the phenoxyethanol a), ethanol e) or isopropanol e) on its own or the preservative mixtures b) and c) as stabilizer(s). Compared to the corresponding examples according to the invention, up to more than 10-fold the amount of preservative was used. In this regard, reference is made to table 2 below.
(13) TABLE-US-00002 TABLE 2 Concentration of Polymer in the individual Appearance Compar- aqueous components in the Germ of the ative polymer Preservative or polymer solution loading stabilized example solution preservative mixture (% by weight) test solution 1 Luviset c) 2-Phenoxyethanol c) 1.15 Not Very Clear * passed slightly cloudy 2 Luviset b) Phenylpropanol b) 0.65 Not Slightly Clear * 1,2-Octanediol passed cloudy 1,3-Propanediol 3 Luviset c) 1,2-Pentanediol c) 0.75 Not cloudy/phase Clear * 1,2-Octanediol passed separation 1,2-Decanediol 4 Luvigel b) 2-Phenoyxethanol c) 1.50 Not Almost Star ** passed clear 5 Luvigel d) Phenylpropanol c) 0.95 Not Almost Star ** 1,2-Octanediol passed clear 1,3-Propanediol 6 Luvigel c) 1,2-Pentanediol d) 1.25 Not Minimal Star ** 1,2-Octanediol passed cloudy 1,2-Decanediol 7 Luviquat c) Phenoxyethanol c) 1.15 Not Almost Hold*** passed clear/very slightly cloudy 8 Luviquat d) Phenylpropanol b) 0.6 Not Almost Hold*** 1,2-Octanediol passed clear/very 1,3-Propanediol slightly cloudy 9 Luviquat c) 1,2-Pentanediol c) 0.75 Not Cloudy/phase Hold*** 1,2-Octanediol passed separation 1,2-Decanediol 10 Luviskol d) Phenylpropanol b) 0.65 Not Slightly K85**** 1,2-Octanediol passed cloudy 1,3-Propanediol 11 Luviskol c) Phenoxyethanol d) 1.25 Not Almost K90***** passed clear 12 Luviskol c) 1,2-Pentanediol c) 0.65 Not Cloudy K90***** 1,2-Octanediol passed 1,2-Decanediol 13 Luviskol e) Ethanol e) 3.00 Not Almost K90***** passed clear 14 Luviskol d) Phenoxyethanol d) 1.25 Not Almost K90***** Ethylhexylglyceryl passed clear * = Copolymer of vinylpyrrolidone, methacrylamide and vinylimidazole 20% strength aqueous solution ** = Polyurethane -39, 20% strength aqueous solution ***= Polyquaternium -46, 20% strength aqueous solution ****= Polyvinylpyrrolidone, 20% strength aqueous solution *****= Polyvinylpyrrolidone, 20% strength aqueous solution
(14) As can be seen by reference to comparative examples 1 to 14, the polymer solutions stabilized with phenoxyethanol, ethanol or isopropanol on its own or the preservative mixtures b) and c) have overall not passed the germ loading test. After 7, 14 and 28 days, freedom from germs was found with regard to the tested strains Pseudomonas aeruginosa (ATCC 9027), Staphylococcus aureus (ATCC 6638) and Candida albicans (ATCC 10231). However a colonization with Aspergillus brasiliensis (ATCC 16404) was established. Moreover, the aqueous comparison polymer solutions exhibited a cloudy, yellowish coloration, and they are unacceptably odor-intensive. Moreover, the preservative mixtures b) and c) are extremely expensive and therefore not very economical compared to the boosting preservative mixtures according to the invention.