RU2431656C1 - Toilet soap with antimicrobial properties - Google Patents

Abstract

FIELD: chemistry. ^ SUBSTANCE: soap contains the following in wt %: soap base 70-80, antimicrobial agent 1-10, antioxidant 0.2-0.5, polyvinylpyrrolidone 0.1-1.0, functional additives 2.5-5.0 and water - the rest. The antimicrobial agent is nanoparticles of bentonite powder intercalated with Ag+ and/or Cu2+ ions. The powder is obtained by modifying bentonite with aqueous solutions of silver nitrate or copper sulphate, where said bentonite is first enriched with Na+ cations during treatment thereof with aqueous solution of an inorganic sodium salt followed by purification. The particle size of the bentonite powder is not greater than 150 nm. ^ EFFECT: prolonged antimicrobial skin protection by reducing negative effect on the skin. ^ 7 cl, 7 ex

Description

The field of technology.

The invention relates to the field of production of hygiene products, namely to toilet soap with antimicrobial properties, which can be used for both medical and domestic purposes.

Currently, toilet soaps are widely used, which contain an antimicrobial additive that gives the soap disinfectant properties.

The prior art.

Known compositions of toilet soap with antimicrobial properties [RU No. 2147607, publ. 2000, No. 2163255, publ. 2001], containing a soap fat base and functional additives, including an antimicrobial based on triclosan (3,4,4'-trichloro-2'-hydroxydiphenyl ether),

So, the antibacterial toilet soap according to patent No. 2163255 contains soap chips, an antioxidant, titanium dioxide, perfume fragrance, dye, as well as triclosan and oil extracts of medicinal herbs.

This soap has foaming properties and provides disinfecting and deodorizing effects.

However, modern studies have found that triclosan suppresses not only pathogenic microflora, but also protective resident microflora, which can lead to negative side effects when using soap. The presence of phenolic and aromatic halogenated groups in triclosan has an irritating and allergenic effect on the skin.

Currently, in the field of cosmetology and hygiene, considerable attention is paid to the creation of preparations, including for washing the body, the composition of which is based on the use of natural components of inorganic origin, biologically compatible with human skin.

For these purposes, in the composition of the developed means of hygiene and cosmetics are widely used:

metals or metal compounds, such as silver, copper, zinc, lead, chromium, etc., which exhibit effective antimicrobial properties to a wide range of gram-negative and gram-positive bacteria ((Krasilnikov A.P. Handbook of antiseptics. - Minsk: Higher school, 1995 , 91, 109; Reference book of medicines used in medical practice in the USSR / under the editorship of M.A. Klyuyev. - M .: Medicine, 1989),

components based on layered minerals, such as bentonites, the presence of which to the composition of the soap helps to improve the cleansing and degreasing effects on the skin.

In US patent No. 7285521, publ. 2007, a toilet soap was proposed containing a soap base (64-80 wt.%), Bentonite powder with a particle size of 8 to 15 microns in an amount of at least 16 wt.% And functional additives, including moisturizers, such as glycerin, lanolin, or others.

The sorbing effect of bentonite powder in this soap composition improves skin cleansing and degreasing. However, this technical solution does not confirm the antimicrobial effect of soap on the skin.

In the application US 2009/0286706, publ. November 19, 2009, a soap composition is proposed containing a soap base, an antibacterial agent based on zinc oxide powder, foaming in the form of lauric acid salt, and smectite clay.

The antimicrobial effect of soap on the skin is provided through the use of zinc oxide in its composition. However, the advisability of using this antibacterial agent is limited by the conditions of the costly part of its production and the negative effect on the skin - increased dryness.

In the technical solution according to the application WO 2006/097238, publ. 09/21/2006, which is selected as the closest analogue of the claimed invention, a toilet soap with antimicrobial properties is proposed, containing a soap base, antimicrobial agents, antioxidant, functional additives and water.

The composition of the soap uses montmorillonite powder (Na ⁺ bentonite form) in an amount of 5 to 30 wt.%, Which gives the soap adsorbing properties. As an antimicrobial agent in this solution, a mixture of 3,4,4'-trichlorocarbanilide (TCC) and 3,4,4'-trichloro-2'-hydroxydiphenyl ether (TCN) is used in an amount of not more than 2 wt.%.

As additional functional additives in the invention it is proposed to use perfume, moisturizers, for example glycerin, lanolin or other additives. The basis of toilet soap is traditionally obtained by saponification of fats, including such as edible fats, palm oil, coconut oil, sunflower oil, etc.

When using soap, the risks of inflammatory processes are reduced.

However, the use of an antibacterial agent based on these organic compounds containing phenolic and aromatic halogenated groups, as already noted above, is impractical, in view of their irritating and allergenic effects on the skin. The presence of a mineral in the composition of the soap (Na bentonite ⁺ form) containing alkali metal cations (Na ⁺ , K ⁺ ) leads to an increase in pH (soap alkalinity), which adversely affects the skin.

To improve the cosmetic properties of soap, its formulation contains a significant amount of moisturizing, emollient additives and antioxidants, which increases the cost of soap.

However, in the analysis of the prior art established fame antimicrobial agent created on the basis of inorganic components (see patent RU No. 2330673. Publ. 2008). This solution proposes an antimicrobial agent based on nanoparticles of bentonite powder intercalated with Ag ⁺ or / and Cu ^{2+ ions} , which were obtained by modifying with solutions of inorganic salts of silver nitrate or copper sulfate of bentonite, previously enriched with Na ⁺ cations by treating it with an aqueous solution of inorganic salt sodium followed by purification.

The antimicrobial agent is obtained from mineral, environmentally friendly components and can be used as additives to various drugs, including medical and cosmetic purposes.

However, this decision does not provide for the development of soap formulations with antimicrobial properties.

Disclosure of the invention.

The objective of the invention was to create a soap with antimicrobial properties, providing a technical result for obtaining the antimicrobial effect of a prolonged action while reducing the risk of negative side effects.

The objective of the invention was to create a soap with antimicrobial properties, providing a technical result for antimicrobial skin protection through the use of components that are biologically compatible with human skin, which reduce the risk of negative dermatological manifestations.

To solve the technical problem, a toilet soap containing a soap base, an antimicrobial agent, an antioxidant, functional additives and water is proposed, in which, according to the claimed invention, the soap additionally contains polyvinylpyrrolidone and, as an antimicrobial agent, nanoparticles of bentonite powder intercalated with Ag ⁺ or ions / and Cu ²⁺ ions, which is obtained by modification of water solutions of silver nitrate or copper sulfate, bentonite, pre-enriched cations Na ^+, by treating it with water th solution of an inorganic salt of sodium and subsequent cleaning, the soap has the following component ratio, wt.%:

soap base 70.0-80.0 bentonite powder intercalated by ions of Ag ⁺ or Cu ²⁺ or a mixture of these powders with a ratio of 1: (0.5-4) 1.0-10.0 polyvinylpyrrolidone 0.1-1.0 antioxidant 0.2-0.5 functional additives 2.5-5.0 water the rest, while the particle size of the bentonite powder is not more than 150 nm

According to the invention, the quantitative content of metals in the composition of soap is 0.02-0.8 wt.%.

According to the invention, as functional additives, titanium dioxide, glycerin, citric acid and other additives are used with the following content in the composition of soap, wt.%:

titanium dioxide 0.1-0.5 glycerol 2.0-2.5 citric acid 0.1-0.5 other additives 0.3-1.5

According to the invention, Antal P-2 is used as an antioxidant.

According to the invention, perfume composition and / or cosmetic cream are preferably used as other additives.

According to the invention, soap chips are used as the base.

According to the invention, polyvinylpyrrolidone with a molecular weight of 12 · 10 ³ -40 · 10 ^{3 is used} .

The inventive soap (in the presence of an antimicrobial agent and a biopolymer biologically compatible with the skin) provides antimicrobial protection of the skin with prolonged action while reducing its negative impact.

In the preparation of the soap composition, silver and copper cations intercalated into bentonite nanoparticles are released and bind to the functional groups (-C = O) of polyvinylpyrrolidone with the formation of silver and copper nanoclusters stabilized by polyvinylpyrrolidone and having an antimicrobial prolonged effect on the skin when using soap .

Other ingredients that make up the soap of the invention are traditionally used components to balance the detergent and cosmetic properties of the soap.

In the analysis of the prior art, no technical solutions with a combination of features corresponding to the claimed technical solution and implementing the above result were identified.

The above analysis of the prior art indicates that the claimed technical solution meets the criteria of "novelty", "inventive step".

The claimed invention can be industrially implemented to obtain soap with antimicrobial properties, which reduces the risk of negative dermatological manifestations.

The implementation of the invention.

The invention is illustrated by the choice of raw materials for the implementation of the invention, examples of its implementation, test results.

To implement the invention using:

soap chips, preferably from sodium salts of natural and / or synthetic fatty acids, traditionally used for the manufacture of various toilet soaps;

polyvinylpyrrolidone (PVP) with a molecular weight (m) of 12 · 10 ³ -40 · 10 ³ , a water-soluble biopolymer used in medicine and cosmetics, including as a modifier of the viscosity of aqueous solutions and a foam stabilizer in detergents. Preferred is the use of polyvinylpyrrolidone (VFS 42-1791-88), m. M 20 · 10 ³ -30 · 10 ³ ;

titanium dioxide, which is used in the manufacture of soap as a pigment filler and is a barrier to UV radiation;

glycerin used in cosmetics, including in the manufacture of soap as a functional additive softens the skin and protects it from drying out;

antioxidant Antal P-2, traditionally used in the composition of soap as a stabilizer to prevent the oxidation of products and plasticizer to improve the rheological properties of the soap mass;

citric acid, traditionally used in the composition of soaps to regulate the indicator (pH) and as an amplifier of antioxidant properties;

other functional additives traditionally used as part of soap: perfumes (perfume compositions), cosmetic cream to improve the operational properties of soaps, including organoleptic ones;

an antimicrobial component created on the basis of inorganic components (see patent RU No. 2330673).

This component is obtained by a two-stage process. At the first stage, montmorillonite (Na ⁺ bentonite form) is treated with an aqueous solution of sodium chloride (NaCl), bentonite is kept in this solution for 10-24 hours, it is decanted several times with rinsing with deionized water to pH = 7 to remove chlorine, then dried. In the second stage, the resulting semi-finished product (bentonite enriched in sodium ions) is treated with an aqueous solution of silver nitrate (AgNO ₃ ) or copper sulfate (CuSO ₄ ). As a result of ion substitution reactions, cations (Na ⁺ ) are replaced by substitution metal cations (Ag ⁺ or Cu ²⁺ ), and then the sodium salts of the intercalated product are purified, filtered, dried and ground.

For the manufacture of 100 g of bentonite intercalated by ions of Ag ⁺ , Cu ²⁺ (according to the claimed invention), used:

the initial raw material component is bentonite of the Na ⁺ form (montmorillonite) in an amount of 110 g; 10% aqueous solution of sodium chloride and 15% aqueous solutions of inorganic salts, respectively, of silver nitrate (AgNO ₃ ) and copper sulfate (CuSO ₄ ).

Activation (enrichment) of bentonite by sodium ions and intercalation of the obtained bentonite semi-finished product (after its enrichment with sodium ions) by silver and copper ions was carried out at a ratio of bentonite: solution, as 1:10 (v.h.).

The resulting antimicrobial agents were evaluated by particle size and analyzed by determining the quantitative content of silver and copper in them.

The particle size of the obtained bentonite powders intercalated with silver or copper ions was controlled using an electron microscope. As a result, it was found that nanoparticles of bentonite powder have a size of not more than 150 nm.

The quantitative content of silver and copper in the obtained products was determined using titrimetric analysis using indicators that fix the point of titration equivalence. Depending on the initial raw material product, the amount of activating and intercalating (modifying) reagents in the modified bentonite powder contains from 2 to 8 wt. % metals (silver, copper).

The indicated amount of the aforementioned metals in bentonite powders is optimal. An increase in the amount of metals leads to an increase in the costly part of obtaining an antimicrobial agent, and when they decrease in the intercalated bentonite powder, its antimicrobial activity decreases.

In the manufacture of soap according to the invention using a traditional process:

the components (ingredients) specified according to the invention are introduced into the soap shavings, the resulting soap mass is mixed until a homogeneous state;

the soap mass is subjected to additional mechanical processing (sawing), followed by molding, cutting the obtained pieces, stamping the soap, wrapping it in packaging.

When developing a soap formulation, the amount of components was determined by the developer experimentally from the conditions of ensuring effective antimicrobial protection of the skin, the balance of washing and cosmetic properties of soap.

The combination of components specified in the invention and their amount is optimal for obtaining a solid soap with antimicrobial properties and corresponding to dermatological requirements.

The use of polyvinylpyrrolidone (PVP) in the soap at a given amount and molecular weight is optimal for the formation of stable nanoclusters of antimicrobial action in the soap composition and to give the soap mass optimal viscosity during homogenization.

When used for the manufacture of soap, PVP with a molecular weight of more than 40 · 10 ³ or / and with an amount of more than 1.0 wt.%, The viscosity of the soap mass increases sharply, which affects the homogenization process.

Use of PVP with m.m. less than 12 · 10 ³ worsens the stabilizing effect of this drug on foaming with a decrease in the formation of active antimicrobial nanoclusters in solution.

A decrease in the amount of PVP in the soap composition of less than 0.1 wt.% Worsens its stabilizing effect and the antimicrobial properties of the soap.

Used according to the invention, an antibacterial agent based on nanoparticles of bentonite powder intercalated with silver and / or copper ions, given the amount specified in the invention in the soap formulation, provides a pronounced antimicrobial effect without adverse dermatological effects. A decrease in the amount of this agent in soap worsens its antimicrobial effect, and an increase leads to an increase in cost.

The ratio of the mixture of used bentonite powders intercalated with silver ions (Ag ⁺ ) and copper ions (Cu ²⁺ ), which is specified according to the invention, is economically most expedient and optimal in terms of the antimicrobial properties of the soap.

The specified particle size of the bentonite powder is most appropriate according to the conditions of the process of its introduction into the soap mass and to ensure the prolonged action of the antimicrobial effect when using soap.

The qualitative and quantitative composition of other ingredients included in the composition of the soap of the invention and providing its washing and cosmetic properties is optimized based on traditional developments used for the manufacture of solid soaps (see, for example, Safeguard soap manufactured by Procter & Gamble, a also patent RU No. 2147607, developer of the Cosmetic Association “Freedom” OJSC). The compositions of these soaps also contain an antibacterial agent based on triclosan, the use of which, as noted above, worsens the dermatological properties of soaps.

Below are examples of the implementation of the invention, in accordance with which, using laboratory equipment, soap samples were obtained.

The quantitative content of ingredients (components) in each example is calculated to obtain 500 g of soap.

Example 1

Soap shavings 74%; antimicrobial agent based on bentonite powder intercalated with Ag ⁺ ions, 2.5%; polyvinylpyrrolidone, m.m. 20 · 10 ³ -30 · 10 ³ 0.3%; antioxidant (Antal P-2) 0.3%; glycyrin 2%; citric acid 0.1%; titanium dioxide 0.1%, perfumery composition (fantasy direction with a floral scent) 0.5%; water is the rest.

Example 2. The same as in example 1, but bentonite powder intercalated with Cu ^{2+ ions} in an amount of 2.5 wt.% Was used as an antimicrobial agent.

Example 3. The same as in example 1, but as an antimicrobial agent used bentonite powder intercalated with Cu ^{2+ ions} in an amount of 5.0 wt.%.

Example 4. The same as in example 1, but as an antimicrobial agent, a mixture of bentonite powders intercalated with Ag ⁺ and Cu ^{2+ ions was used} , with a ratio of 1: 1 in the mixture and 2.5% by weight. .

Example 5. The same as in example 1, but as an antimicrobial agent, a mixture of bentonite powders intercalated with Ag ⁺ and Cu ^{2+ ions was used} , with a ratio of 1: 5 in the mixture and 2.5% by weight. .

Example 6. The same as in example 1, but in the presence of low molecular weight polyvinylnirrolidone with m.m. 8 · 10 ³ -10 · 10 ³ (this HHGP is used in medicines to detoxify and improve blood rheological properties) 1.0 wt. .%.

Example 7 (control). The same as in example 1, but as an antimicrobial agent used triclosan in an amount of 3 wt.%.

According to examples 1-7, soap samples weighing 110 g were obtained. For each example, 4 soap samples were obtained (taking into account technological losses during manufacture).

Evaluation of the antimicrobial properties of the soap was carried out using microbiological studies in relation to gram-negative (Escherichia coli) and gram-positive (Staphilococcus aureus) bacteria by the method of dilution of soap (according to examples 1-7) in liquid nutrient media.

The microbial load was 10 ⁷ CFU / ml.

The antimicrobial effect was controlled by subsequent seeding of each dilution on solid nutrient media.

As a result of studies, it was found that when using soap compositions, the antimicrobial effect in relation to:

gram-positive bacteria (S. aureus) takes place for soap in example 1, 3 and 7 within 24 hours .; according to example 4 for 20 hours .; according to example 2, 5 and 6 for 15 hours .;

gram-negative bacteria (E. coli) - for soap according to examples 1 and 4 - within 20 hours .; for example 3-24 hours .; according to examples 2, 5 and 7 for 18 hours.

From microbiological studies it follows that the most effective antimicrobial properties in relation to these microorganisms are soap compositions according to examples 1, 3, 4 and 7.

The decrease in the effectiveness of the antimicrobial activity against bacteria (S. aureus) of the soap in example 2 indicates the advisability of increasing the concentration in the composition of the soap of an antibacterial agent based on bentonite powder intercalated by copper ions, which is confirmed by microbiological studies of the soap sample in example 3.

The decrease in the antimicrobial activity of the soap according to example 5 indicates the inappropriateness of changing the weight ratio of the mixture of the antimicrobial agents indicated in the invention.

The decrease in the antimicrobial activity of the soap sample according to example 6 indicates the inappropriateness of the use of PVP with m.m. less than 12 · 10 ³ . Use of PVP with m.m. less than 12 · 10 ³ worsens the stabilizing effect of this drug on foaming with a decrease in the formation of active antimicrobial nanoclusters in solution.

Evaluation of consumer properties of soap samples (examples 1-7) was carried out by their dermatological effect on the skin of the hands of the subjects with frequent use for 8 days. For testing, 14 people were invited (every two people used the same type of soap samples in examples 1-7).

The tests established:

the soap of examples 1-5 does not have an irritating and allergic effect on the skin during the entire test period;

the soap of example 7 caused an irritating effect on the skin of the subjects on the 3rd and 5th day of its use;

the soap of example 6 does not have an irritating and allergic effect on the skin, but this soap has an increased dissolution rate. The soap test period was reduced to 4 days.

Thus, on the basis of the data obtained, it was found that the soap according to the invention, in accordance with examples 1-4, is most effective in antimicrobial protection of the skin and does not have a side dermatological effect, which indicates the optimal choice of components and their amount for soap composition according to invention.

According to its technical characteristics (organoleptic and physicochemical), the obtained soap according to examples 1-4 corresponds to standard requirements.

Claims (7)

1. Toilet soap containing a soap base, antimicrobial agent, antioxidant, functional additives and water, characterized in that the soap additionally contains gulivinyl pyrrolidone, and as an antimicrobial agent - nanoparticles of bentonite powder intercalated with Ag ⁺ or / ions and Cu ^{2+ ions} , which is obtained by modification of water solutions of silver nitrate or copper sulfate, bentonite, pre-enriched cations Na ^+, by treating it with an aqueous solution of an inorganic salt of sodium and subsequent cleaning, the soap s an following component ratio, wt.%:
soap base 70.0-80.0 bentonite powder intercalated by ions of Ag ⁺ or Cu ²⁺ , or a mixture of these powders with a ratio of 1: (0.5-4) 1.0-10.0 polyvinylpyrrolidone 0.1-1.0 antioxidant 0.2-0.5 functional additives 2.5-5.0 water rest
while the particle size of the bentonite powder is not more than 150 nm. 2. Soap according to claim 1, characterized in that the quantitative content of metals in the composition of soap is 0.02-0.8 wt.%. 3. Soap according to claim 1, characterized in that titanium dioxide, glycerin, citric acid and other additives are used as functional additives at their next content in the composition of soap, wt.%:
titanium dioxide 0.1-0.5 glycerol 2.0-2.5 citric acid 0.1-0.5 other additives 0.3-1.5 4. Soap according to claim 1, characterized in that "Antal P-2" is used as an antioxidant. 5. Soap according to claim 1, characterized in that the perfume composition and / or cosmetic cream are preferably used as other additives. 6. Soap according to claim 1, characterized in that soap chips are used as the base. 7. The soap according to claim 1, characterized in that the use of polyvinylpyrrolidone with a molecular weight of 12 · 10 ³ -40 · 10 ³ .