Method of determining stability of cosmetic product emulsion

FIELD: medicine.

SUBSTANCE: invention relates to chemical-pharmaceutical industry and represents method of determining cosmetic product emulsion stability, characterised by the following: selection and preparation of samples are carried out and centrifuged and it differs by the fact that at the first stage carried out are microscopic observation of centrifuged material and calculation of number of micelle n on site 1 cm2 at 10, or 40, or 100-multiple magnification with the following comparison with the number of micelles n0 in sample, which is not subjected to preparation, considering emulsion conditionally stable at and at the second stage samples with conditionally stable emulsion, are subjected by accelerated aging during a month by placing of examined samples in thermostat and keeping at temperature 40-42°C and relative humidity 65±2%, periodically carrying out microscopic observation of samples on 1 cm2 site at 10, or 40, or 100-multiple magnification and statistic processing of experimental data with construction of mathematical model of forecast and solution of equation of form where n' - is number of micelles, pieces./cm2; τ is time of accelerated aging, days; design factors of exponential equation, obtained in processing experimental data, at τ → given time of storing, with calculation of possible emulsion state, in case of value emulsion is considered stable and suitable for durative storage, and in case of it is considered unsuitable for durative storing.

EFFECT: invention ensures increased effectiveness of determination of emulsion stability.

2 ex, 2 tbl, 6 dwg

 

The invention relates to the field of fat and cosmetic industries, and in particular to a method of determining the stability of the emulsion.

There is a method of determining the stability of the water-carbon emulsion (U.S. Pat. RF 2189026, EN), including continuous measurement of changes in weight gravimetric detector, part of which is immersed in this mixture. The method consists of a first stage of heating or cooling the emulsion to a predetermined temperature and a second stage during which the emulsion is maintained at this temperature, record the curve changes the specified weight of the detector in time, providing the definition of collected solid mass, and the speed of separation of the mixture into two phases by determining the slope of this curve, and the stability of the emulsion is determined by comparison with a reference emulsions, the stability of which is known.

The disadvantages of this method is that the determination of the stability of the emulsion based only on quantitative measurement of the process of separation of liquid and solid is not miscible phases using the liquid, which is supported homogeneous; the method requires an additional device for measuring the separation of the emulsion into several liquid and/or solid phases, which leads to complexity of the process of determining the stability of the emulsion; the method of ensuring Ecevit global analysis of the whole sample volume, bypassing measuring its microstructure and touching only the quantitative measurement of the phase separation process; the determination of stability and is determined by the presence of the aqueous phase in the organic substance.

In contrast to the method of determining the stability of the water-hydrocarbon emulsion, the inventive method of determining the stability of the emulsion on the basis of the analysis of the microstructure does not depend on the temperature, keeping the emulsion at the time of the study, and from time to time, during which the emulsion is subjected to changes.

The closest in technical essence is a way of determining the stability of the emulsion (GOST 29188.3-91 Method of determining the stability of the emulsion. Cosmetic products).

The method consists in the fact that the two tubes is filled with2/3the volume of the studied emulsion and weighed, the result is recorded to the second decimal point. The difference in mass of the test tubes with the emulsion should not exceed 0.2 g Tube placed in a water bath or thermostat and incubated for 20 min at a temperature of 42-45°C - thick emulsion, at a temperature of 22-25°C - liquid emulsion. The tubes are taken out, dried them on the outside and set in sockets of a centrifuge. Centrifugation should be performed within 5 min at a frequency of rotation

100-1. Take out the test tube and determine the stability of the emulsion. If that is are in one test tube and observe the separation of the emulsion, then repeat the test with new portions of the emulsion.

When determining the stability of liquid emulsions, if you do not see a clear stratification, the contents of the tube gently poured on a sheet of white construction paper and note the presence or absence of delamination of the emulsion.

The emulsion is considered stable if after centrifugation the tubes see allocation of not more than droplets of the aqueous phase or layer of oil phase is not more than 0.5 cm

This method is based on the observation of the beginning of the separation of emulsions of fat and water phase that is determined at the time of inspection cosmetics. The determination is performed visually and may be biased. This method also does not allow one to predict the safety of a product within a certain period of storage. The disadvantage of this method is the lack of clear objective criteria to determine the stability and the inability to predict the stability of the emulsion over time.

The task of the invention is to develop a method that improves the accuracy of determination due to the fixation process of breaking emulsions using instrumental methods, and the development of a method for predicting shelf life of the cosmetic product on the basis of the analysis of the microstructure.

The technical result is to increase the attachment performance of the method for determining the stability of the emulsion and the development of a method for predicting the duration of stability of the emulsion over time based on the analysis of the microstructure with the prospect of determining the timing storage of cosmetics based on the emulsion.

The problem is solved due to the fact that in the method of determining the stability of the emulsion cosmetic products, characterized by the fact that carry out sampling and preparation of samples, centrifuged, at the first stage is conducted microscopic observation of the centrifuged material and counting the number of micelles n on-site one cm2at 10, or 40, or 100-fold increase with subsequent comparison with the number of micelles of n0in the sample, not thrown preparation, considering the emulsion is conditionally stable under n×100/n0≥50, and the second stage samples with a relatively stable emulsion is subjected to accelerated aging in a month by putting the samples in thermostat and keeping at a temperature of 40-42°C and a relative humidity of 65±2%, periodically conducting microscopic observation of the samples at site 1 cm2at 10, or 40, or 100-fold increase, and carry out statistical processing of the experimental data with the mathematical model prediction and solution of equations of the form

where n' is the number of micelles, PCs/cm2;

τ - time, accelerated aging, days:

a, a1- estimated coefficients of the exponential equation, obtained by processing the experimental the data

when τ → set the retention period, with the expectation of a possible state of the emulsion when the value of n'×100/n0≥50 emulsion is considered stable and suitable for a given storage time, and when n'×100/n0≤50 is considered not suitable for this storage time.

As you know, emulsion water in oil and oil in water is presented in the form of micelles. Their size, the possibility of combining determine their stability during storage and the ability to merge them into larger micelles.

It is experimentally proven that curve determine the ratio of the number of micelles from time to time on a certain area of the microscope characterizes the stability of the emulsion over time.

The method of determining the stability of the emulsion is carried out in several stages: at the first stage of sample preparation of the emulsion, centrifugation, microscopy and determination of stability by comparing the number of micelles in the sample of the emulsion held training from the original sample, and the second stage is conducted accelerated aging of the sample under certain conditions, microscope patterns in certain time intervals, counting the number of micelles in a certain space and the mathematical processing of the data, and then identify possible periods of storage.

A sample of the cream is subjected to the accelerated starane is in thermostat at a humidity of 65±2% and a temperature of 40-42°C. Periodically taking a sample of seasoned emulsion to assess its stability by the claimed method with parallel making the determination of stability by the standard method until the bundle.

For analysis of the microstructure of 1-2 g of cream evenly spread over the surface of glass slides and covered with a cover glass to prevent evaporation. The thickness should allow clearance nanomicelles patterns. A glass slide is placed under the microscope, with fotonica, and spend the microscope structure of the emulsion at ×10, 40, 100-fold increase with fixation of the image. The obtained photo-allocate space in 1 cm2and do count the number of micelles. These operations are repeated in a time of accelerated aging, and temporal characteristics of accelerated aging lead in the table indicating the relation between the number of micelles from the time of accelerated aging.

The results build the curve describing the dependence of the number of micelles on the designated area on time. The graph presented on figure 1, where n is the number of micelles, PCs/cm; τ - time, accelerated aging, days.

From the obtained graph according to the number of micelles from the retention time has an exponential dependence. To obtain a mathematical model related to the spine of the number of micelles on the designated space time graph is approximated by the exponential function of the form n=a exp(a 1τ), as shown in figure 2, where a, a1- estimated coefficients of the exponential equation, obtained by processing the experimental data.

The equation n=a exp(a1τ) verified describes the experimental and calculated data. Based on the obtained data, all curves adequately describe the experimental data with a confidence interval of 95%.

With increasing time the number of micelles decreases and, as is known from the experimental data, the emulsion loses stability when destroyed more than 50% of the micelles. Therefore, using the mathematical model, rebuilding its coordinates according to the inverse of time, we get an equation of the form n=f(1/τ), τ→∞. This model will have the form shown in figure 3, and the equation describing the resulting curve is an expression of the form.

This graph and the equation can be used to determine and predict the shelf life of cosmetic products.

Knowing the equation of the formsolved it to determine 1/τ when the value of n is equal to 50% of the original and the received time of use as possible shelf life of cosmetic products. This graph and the equation can be used to determine and predict the timing of XP is in cosmetic products.

To confirm the claimed technical solution, experiments were carried out according to previously described method under the conditions shown in table 1.

Table 1
The conditions of the experiment
The conditions of the experimentExamples of the claimed methodThe performance of the prototypeThe original sample without preparation
123
The temperature of the water bath, °C42424242no
Aging time before centrifugation, min20202020no
The rotational speed of the centrifuge, with-1100100100no
The time of centrifugation, min5555no
The magnification, times1040100no1040100
Square platforms, 1 cm2111no111
The number of micelles, PCs/cm2423318no5643,821
Stability7575,375,7stable
n×100/n0≥50 (stable)

In accordance with the conditions shown in table 1, experiments analysis of cosmetic cream based on the emulsion.

Selected samples of the cream and placed in two test tubes, filling them with2/3the volume of the studied emulsion, and weighed, the result is recorded to the second decimal point. The difference in mass of the test tubes with the emulsion should not exceed 0.2 g Tube placed in a water bath or thermostat and incubated for 20 min at a temperature of 42-45°C - thick emulsion, at a temperature of 22-25°C - liquid emulsion. The tubes are taken out, dried them on the outside and set in sockets of a centrifuge. Centrifugation should be performed within 5 min at a frequency of rotation

100-1. Take out the test tube and determine the stability of the emulsion, conducting microscopic observation of the sample subjected to processing, and source at site 1 cm2with magnification ×10, 40, 100 times. Is visual counting of micelles and comparing the results. The emulsion loses stability when destroyed 50% of the micelles. Samples of both on offer, and the way the prototype showed stability.

The second stage consists of determining the probable time storage of cosmetic emulsions. The proposed method R is alzueta the following examples of specific performance.

Example 1

In the present example describes the use of 1 of the method of the invention for determining the stability of the emulsion cosmetic product.

This method is as follows.

A sample of emulsion cosmetic cream. It is subjected to accelerated aging in a thermostat at a humidity of 65±2% and a temperature of 42°C, With periodic sampling to assess its stability according to standard procedures until the bundle. After certain time intervals of 1 g of the sample are distributed uniformly on the surface of glass slides and covered with cover glass. A glass slide is placed under the microscope, having

fotonica, and spend the microscope structure of the emulsion at ×10-fold increase with fixation of the image. The obtained image is allocated space in 1 cm2and do count the number of micelles.

These operations are repeated in a time of accelerated aging of the emulsion in a thermostat at 40°C and relative humidity of 65%. Determination of micellar structure is carried out by previously described methods by plotting the forward and backward according to the number of micelles of time and the definition of expected shelf life, which is 530±10 days.

Example 2

This example analyzes other conditions of the experiment,when the microscope structure of the emulsion is carried out at ×40-fold increase with fixation of the image, and on the resulting photographic image is allocated space in 1 cm2and it is counting the number of micelles. The data are recorded in table 2.

Table 2
The change in the number of micelles in time
Time accelerated aging, days32031
The number of micelles, PCs/cm412920

Microscopic examination of the microstructure of the emulsion analyzed cream cosmetic type oil-in-water is shown in figure 4.

All other operations are performed analogously to example 1.

A plot of the change in the number of micelles in time investigated cosmetics shown in figure 5.

The equation n=45,2514×exp(-0,0252×τ)describing the obtained curve, verified describes the experimental and calculated data. Based on the obtained data, all curves adequately describe the experimental data with a confidence interval of 95%. An inverse relationship is presented in figure 6.

As can be seen from the plot of the change in the number of micelles in the time studied cosmetics with increasing time the number of micelles decreases, which can be quantitatively determined by rebuilding its coordinates according to the inverse time.

The experimental data found that accelerated aging in the above-described conditions within 30 days corresponds to the storage of the product in regulated conditions within one year. Therefore, calculating the calculated value of n' with τ=30 days

n'=21,

get n'×100/n0=21×100/56=37,5.

From the data obtained it follows that this emulsion product may be stored for years without loss of quality.

The method of determining the stability of the emulsion cosmetic products, characterized by the fact that carry out sampling and preparation of samples, centrifuged, characterized in that the first stage is conducted microscopic observation of the centrifuged material and counting the number of micelles n on the space of 1 cm2at 10, or 40, or 100-fold increase with subsequent comparison with the number of micelles of n0in the sample not subjected to the preparation, considering the emulsion conditionally stable whenand at the second stage samples with conditionally stable emulsion is subjected to accelerated aging in a month by putting the samples in thermostat and keeping at a temperature of 40-42°C and a relative humidity of 6±2%, periodically conducting microscopic observation of the samples at site 1 cm2at 10, or 40, or 100-fold increase and statistical processing of the experimental data with the mathematical model prediction and solution of equations of the form

where n' is the number of micelles, PCs/cm2;
τ - time, accelerated aging, days;
- estimated coefficients of the exponential equation, obtained by processing the experimental data,
when τ → set the retention period, with the expectation of a possible state of the emulsion when the value ofthe emulsion is considered stable and suitable for long-term storage, and inconsider not suitable for long term storage.



 

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