KR101423585B1 - Method for determination of sunscreen component - Google Patents

Abstract

More particularly, the present invention relates to a method for analyzing an ultraviolet screening component, and more particularly, to a method for analyzing an ultraviolet screening component, comprising: extracting an ultraviolet screening component by adding a mixed solvent containing tetrahydrofuran, methanol and distilled water to a cosmetic composition containing an ultraviolet screening component; Introducing the ultraviolet blocking component extracted in the above-described step (a) into a reversed phase nonpolar column as a stationary phase; And analyzing an ultraviolet shielding component using liquid chromatography using the mixed solvent as a mobile phase.

The method for analyzing ultraviolet shielding component of the present invention is an analytical method based on liquid chromatography (HPLC), and it is possible to rapidly analyze ultraviolet shielding components with a high degree of separation, and furthermore to analyze ultraviolet shielding components more economically and effectively It can be usefully used for quality control of ultraviolet shielding components contained in cosmetic compositions.

Description

[0001] The present invention relates to a method for determining a sunscreen component,

The present invention relates to a method for simultaneously analyzing ultraviolet blocking components having different chemical properties, and more particularly, to a method for simultaneously and simultaneously detecting hydrophilic and lipophilic ultraviolet blocking components contained in a cosmetic composition using liquid chromatography (HPLC) And more particularly to an analytical method for accurately analyzing a sample.

Recently, as the incidence of skin cancer and photoaging due to ultraviolet rays increases due to destruction of the ozone layer, there is an increasing need for an excellent ultraviolet shielding component for protecting human skin from harmful effects of ultraviolet rays.

Chemical sunscreen ingredients that are frequently used today include compounds that absorb or reflect ultraviolet light to minimize the deleterious effects of ultraviolet light on the skin. Of these, butyl methoxydibenzoylmethane is known to be a very useful lipophilic property and a very useful UV-A blocking agent. It is also known as Ethylhexyl Methoxycinnamate (EMC), Ethylhexyl Salicylate (Ethylhexyl Salicylate, EHS), Phenylbenzimidazole Sulfonic Acid, etc. are widely used as a blocking component for UV-B ultraviolet rays. These ultraviolet shielding components can be classified into lipophilic component and hydrophilic component depending on their characteristics, and these components are frequently mixed and used.

Conventionally, thin layer chromatography (TLC), liquid chromatography (HPLC), gas chromatography (GC), etc. have been used as methods for analyzing ultraviolet shielding components having different characteristics included in such a cosmetic composition. However, when these conventional methods are used, it is inappropriate to simultaneously analyze ultraviolet shielding components having strong lipophilic properties and ultraviolet shielding components having high hydrophilic properties.

Therefore, if the method is capable of simultaneously analyzing the lipophilic ultraviolet blocking component and the hydrophilic ultraviolet blocking component contained in the cosmetic composition, it is expected to be usefully used in related fields.

Accordingly, one aspect of the present invention is to provide a simultaneous analysis method capable of rapidly and accurately analyzing ultraviolet shielding components having different properties of hydrophilic and lipophilic properties simultaneously.

According to one aspect of the present invention, there is provided a cosmetic composition comprising: a cosmetic composition containing an ultraviolet shielding component; a step of extracting an ultraviolet shielding component by adding a mixed solvent containing tetrahydrofuran, methanol and distilled water; Introducing the lipophilic and hydrophilic UV blocking component extracted above into a reversed phase nonpolar column as a stationary phase; And analyzing an ultraviolet shielding component using liquid chromatography using the mixed solvent as a mobile phase.

Preferably, the mixed solvent is mixed with tetrahydrofuran and methanol in a volume ratio of 9: 1 to 19: 1 based on the volume of distilled water 10.

The length of the reversed phase nonpolar column is preferably more than 7.5 cm and less than 25 cm.

The ultraviolet shielding component preferably includes a lipophilic ultraviolet shielding component and a hydrophilic ultraviolet shielding component.

The ultraviolet blocking component may be selected from the group consisting of Butyl Methoxydibenzoylmethane (BM), Ethylhexyl Methoxycinnamate (EMC), Ethylhexyl Salicylate (EHS) and Phenylbenzimidazole Sulfonic acid, PSA).

Preferably, the cosmetic composition is selected from the group consisting of creams, lotions, solid cream, and foundations.

The reversed-phase non-polar column is preferably filled with at least one selected from the group consisting of octadecylsilane (C18), dodecylsilane (C12) and octasilane (C8).

The mixed solvent is preferably used in an amount of 0.25 to 10 parts by weight per 100 parts by weight of the cosmetic composition.

It is preferable that the analysis method includes a step of confirming the analysis result through a detector having a wavelength adjusted to a range of 300 nm to 320 nm.

The method for analyzing ultraviolet shielding component of the present invention is an analytical method based on liquid chromatography (HPLC), and it is possible to rapidly analyze ultraviolet shielding components with a high degree of separation, and furthermore to analyze ultraviolet shielding components more economically and effectively It can be usefully used for quality control of ultraviolet shielding components contained in cosmetic compositions.

1 is a chromatogram of a standard solution prepared by dissolving 4 kinds of ultraviolet blocking components (BM, EMC, EHS, and PSA) in tetrahydrofuran: methanol: distilled water = 9: 1: 10 (volume ratio).
FIG. 2 is a graph showing the calibration curves obtained by using the concentrations of the ultraviolet blocking components and the signal intensity.
FIG. 3 shows a chromatogram of ultraviolet blocking components in a creamy water-type cream.
Figure 4 shows chromatograms of UV-blocking ingredients in the oil-in-water lotion.
FIG. 5 shows a chromatogram of ultraviolet blocking components in a lotion in the form of water.
FIG. 6 shows a chromatogram of the UV-blocking components in a solid cream in the form of water.
Figure 7 shows chromatograms of UV-blocking ingredients in an oil-in-water type foundation.
FIG. 8 shows a chromatogram of ultraviolet blocking components in a water-based foundation.

Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings. However, the embodiments of the present invention can be modified into various other forms, and the scope of the present invention is not limited to the embodiments described below.

More particularly, the present invention relates to a simultaneous analysis method for rapidly and accurately analyzing hydrophilic and lipophilic UV blocking components present in a cosmetic composition using liquid chromatography (HPLC) .

The present invention relates to a cosmetic composition containing an ultraviolet shielding component, which comprises extracting an ultraviolet shielding component by adding a mixed solvent containing tetrahydrofuran, methanol and distilled water to the cosmetic composition, Introducing the ultraviolet blocking component extracted in the above-described step (a) into a reversed phase nonpolar column as a stationary phase; And analyzing the ultraviolet blocking component using liquid chromatography using the mixed solvent as a mobile phase.

The cosmetic composition to which the analytical method of the present invention can be applied is not particularly limited, and the present invention can be particularly usefully applied to a case where components having different characteristics such as a hydrophilic ultraviolet blocking component and an oleophilic ultraviolet blocking component are mixed.

First, the present invention performs a step of extracting an ultraviolet shielding component by adding a mixed solvent containing tetrahydrofuran, methanol and distilled water to a cosmetic composition containing an ultraviolet shielding component.

In the extracting step, the mixed solvent is preferably used in an amount of 0.25 to 10 parts by weight, more preferably 0.5 to 7.5 parts by weight, per 100 parts by weight of the cosmetic composition to be analyzed.

When the mixed solvent is used in an amount of less than 0.25 part by weight per 100 parts by weight of the cosmetic composition, there is a problem that the ultraviolet shielding function of the ultraviolet shielding component is insufficient, and the mixed solvent is used in an amount exceeding 10 parts by weight per 100 parts by weight of the cosmetic composition , There is an unexplained problem in considering the composition limit of the KFDA of the ultraviolet screening component.

The mixed solvent is preferably mixed with tetrahydrofuran and methanol at a volume ratio of 8: 1 to 25: 1, more preferably 9: 1 to 19: 1, based on the volume of distilled water 10.

When tetrahydrofuran and methanol are contained in excess of the above range on the basis of distilled water or when the distilled water is contained in the range below the above range, there is a problem in that the non-polarity becomes strong, so that there is a problem of overlapping of peaks, and tetrahydrofuran and methanol are mixed with distilled water The analysis time is excessively long when the distilled water is contained in the range below the above range or the distilled water is included in the range exceeding the above range.

On the other hand, when the tetrahydrofuran content exceeds the above range or the methanol content is less than the above range in relation to the mixing ratio of tetrahydrofuran and methanol, there is a problem that the non-polarity becomes strong, If it is included below the above range or exceeds the above range, the analysis time becomes excessively long, which results in poor analytical efficiency, which is uneconomical.

When the extraction is completed as described above, the ultraviolet blocking component extracted from the ultraviolet blocking component is added to the reversed phase nonpolar column.

The reversed phase nonpolar column used in the liquid chromatography (HPLC) analysis of the present invention is preferably filled with at least one selected from the group consisting of octadecylsilane (C18), dodecylsilane (C12) and octasilane (C8) It is more preferable to use a column packed with octadecylsilane (C18).

The octadecylsilane (C ₁₈ ) column is packed with 18 chains of non-polar carbon in the column. The polar component does not bond with the non-polar column functionalities and dissolves quickly, while the non-polar component binds to the non- . According to this principle, it is possible to separate each of the different components of the mixture by the polarity difference of the components.

When the step of injecting the extracted ultraviolet blocking component into the reversed phase nonpolar column is completed as described above, ultraviolet blocking components are analyzed using liquid chromatography using the mixed solvent as a mobile phase.

That is, the mobile phase used in the liquid chromatography (HPLC) analysis of the present invention preferably has the same composition as the above-mentioned mixed solvent. In order to simultaneously transport lipophilic and hydrophilic UV blocking components, tetrahydrofuran, methanol And a mixed solution of distilled water are preferably used.

The length of the reversed-phase nonpolar column used in the analysis method of the present invention is related to the analysis time. It is preferably more than 7.5 cm, more preferably less than 25 cm, more preferably 10 cm to 20 cm, desirable.

When the column length of the stationary phase is 7.5 cm or less, there is a problem that peaks are overlapped. When the column length is 25 cm or more, the analysis time is excessively long, In the case of lengths falling within the scope of the present invention, particularly when a C18 column of about 15 cm is used, it has the most suitable separation.

The ultraviolet shielding component to be analyzed according to the present invention preferably contains a lipophilic ultraviolet shielding component and a hydrophilic ultraviolet shielding component. In such a case, separation is not easy by other methods, but according to the assay method of the present invention, Each UV blocking component can be clearly separated.

Specific ultraviolet shielding components to which the present invention can be applied include but are not limited to butyl methoxydibenzoylmethane (BM), ethylhexyl methoxycinnamate (EMC), ethyl (EHS), and phenylbenzimidazole sulfonic acid (PSA), which are known to those skilled in the art.

In the case of the ultraviolet shielding component, the compounding limit of the KFDA is limited to 0.5 to 10 wt%, and in the case of the specific ultraviolet shielding component mentioned above, the range of the content is limited to butylmethoxydibenzoylmethane 0.5 to 5.0% by weight of ethylhexylmethoxycinnamate, 0.5 to 7.5% by weight of ethylhexylmethoxycinnamate, 0.5 to 5% by weight of ethylhexylsalicylate, and 0.5 to 4% by weight of phenylbenzimidazosulfonic acid.

The analysis method of the present invention can be used to effectively and specifically detect the ultraviolet shielding component present in the composition for external application for skin, and can be widely applied to the quality control of the ultraviolet shielding ingredients contained in the cosmetic composition.

The cosmetic composition is preferably a formulation selected from the group consisting of creams, lotions, solid creams and foundations, but is not particularly limited thereto, and various forms of cosmetic compositions widely applicable in the art may be included.

Meanwhile, the analysis of the ultraviolet blocking component of the present invention can be confirmed through a detector, and the wavelength can be confirmed by setting the wavelength within the range of 300 nm to 320 nm.

The analytical method according to the present invention has excellent sensitivity, reproducibility, accuracy and the like as can be seen in the following examples, can shorten the analysis time, and further has effects such as low cost and simplicity. Can be effectively and widely applied in the quality control of the ultraviolet shielding ingredients contained in the cosmetic composition.

Hereinafter, the present invention will be described more specifically by way of specific examples. The following examples are provided to aid understanding of the present invention, and the scope of the present invention is not limited thereto.

Example

1. Optimal column  Experiment for selection

The liquid chromatography used in the present invention used a reversed phase non-polar column C18 as a stationary phase. In this experiment, ultraviolet blocking components such as butyl methoxydibenzoylmethane (BM), ethylhexylmethoxycinnamate (EMC ), Ethylhexyl salicylate (EHS), and phenylbenzimidazolesulfonic acid (PSA).

In this case, the butylmethoxydibenzoylmethane (BM), ethylhexylmethoxycinnamate (EMC), and ethylhexylsalicylate (EHS) are lipophilic compounds having a nonpolar property, However, the hydrophilic phenylbenzimidazolesulfonic acid (PSA) having a polar nature is rapidly eluted due to the small binding capacity with the non-polar functional group in the fixed phase under such conditions, causing interference with other polar components in the sample As a result, there is a problem that accurate analysis is difficult due to low separation.

Since the four ultraviolet blocking components have a large chemical property difference, the length of the fixed C18 column which separates the components to set the analytical conditions free from a proper retention time and matrix interference is 25 cm, 15 cm and 7.5 cm, and it was confirmed that the most suitable separation was obtained when 15 cm C18 column was used.

2. For improved separation Mobile phase  Experiment of condition setting

(1) Preparing the experiment

Liquid chromatography separates each component according to the polarity difference by the interaction of the stationary phase column, the mobile phase and the component to be analyzed. Accordingly, not only the kind of the substance packed in the column but also the polarity of the moving phase is a very important factor for setting the analysis conditions. For example, if a non-polar column is used, the polarity of the mobile phase will elute the components quickly, and the non-polar mobile phase will slowly elute the components so that the polarity difference in the mobile phase will allow separation of the components in the mixture.

Analysis of lipophilic butylmethoxydibenzoylmethane (BM), ethylhexylmethoxycinnamate (EMC) and ethylhexylsalicylate (EHS) simultaneously with hydrophilic phenylbenzimidazolesulfonic acid (PSA) Methanol, acetonitrile and tetrahydrofuran as the mobile phase.

(2) Sintering

As a result, when methanol was used, the retention time was too slow, the analysis time was excessively long, and asymmetric trailing phenomenon was observed in the peak shape, making it difficult to obtain accurate analysis results. Even when acetonitrile, which is somewhat less polar than methanol, was used as the organic solvent, it was confirmed that the trailing phenomenon of the peak was observed in the same manner as in the case of using methanol, which is not suitable. Although tetrahydrofuran, which is more non-polar than methanol and acetonitrile, was used as an organic solvent, it was possible to rapidly analyze the above four ultraviolet shielding components within 10 minutes, but it was found that the components were synergistically generated and the components eluted excessively There was a problem.

Therefore, according to the present invention, the four ultraviolet blocking components were analyzed by liquid chromatography by setting the mobile phase conditions as shown in Table 1 below. Specifically, the ultraviolet blocking components extracted with a solution of tetrahydrofuran, methanol and distilled water in a ratio of 9: 1: 10 were injected into liquid chromatography and subjected to column chromatography using C18 (length: 15.0 cm, inner diameter: 4.6 mm, particle 3.5 μm) After separation, the mobile phase was made to have the same composition as the above-mentioned extraction solvent.

column Phenomenex C18 (4.0 mM? 150 mM, 3.5?) Mobile phase Tetrahydrofuran: methanol: distilled water = 9: 1: 10 Flow rate 1.3 mL / min Temperature Room temperature Dose 10ul Detection wavelength 315 nm

At this time, the flow rate of the mobile phase was 1.3 mL / min, and the sample injection amount was 10 μl. Analysis was performed at room temperature and the result was detected at 315 nm using a UV detector. All experiments below were carried out under the conditions of Table 1 above.

3. Verification of analysis method of ultraviolet blocking component according to the present invention

In order to verify the method of analyzing the ultraviolet screening component according to the present invention, the analysis of the above four ultraviolet screening components (BM, EMC, EHS and PSA) was performed on specificity, linearity, Repeatability, Intermediate precision, System stability and Accuracy were evaluated as follows.

(1) specificity ( Specificity )

In order to investigate whether the analyte can be accurately measured in the presence of impurities, degradation products and compound components predicted for coexistence, a comparison was made between the blank test solution and the standard solution to observe whether there was interference in the two chromatograms.

The standard solution was prepared by dissolving 4 kinds of ultraviolet blocking ingredients (BM, EMC, EHS, and PSA) in tetrahydrofuran: methanol: distilled water = 9: 1: 10 (volume ratio).

The lotion and cream prepared in the formulations of the following Tables 2 and 3 were dissolved in tetrahydrofuran: methanol: distilled water = 9 (oil: in water) lotion formulation and O / : 1: 10 (volume ratio).

This experiment related to the blank test solution is an experiment to confirm whether other peaks do not occur when applied to cosmetic formulations, and it is also possible to judge whether overlapping peaks occur through analysis values. If the peak is higher than the peak analyzed by the standard solution, it can be interpreted that another overlapping peak may occur. In the case of a peak smaller than the standard solution, it can be interpreted that the component is lost in the extraction step or the content is lower than the content by other disturbing components.

1) lotion formulation

After the water phase and the oil phase were dissolved by heating at 80 ° C, the oil phase was slowly added to the water phase, and the mixture was emulsified at 5,000RPM for 5 minutes using a homomixer and cooled.

division ingredient Content (% by weight) Awards Purified water to 100 Triethanolamine 2.10 Glyceryl stearate 0.80 FAGE -100 stearate 0.90 Polysorbate 60 1.20 Sorbitan stearate 0.50 Cetearyl alcohol 0.80 glycerin 8.00 Butylene glycol 5.00 Methylparaben 0.20 Phenoxyethanol 0.15 Paid C12-15 alkyl benzoate 5.00 Hexyl laurate 3.00 Cyclopentasiloxane 3.00 Spices 0.10

2) Cream formulation

After the water phase and the oil phase were dissolved by heating at 80 ° C, the oil phase was slowly added to the aqueous phase, emulsified at 5,000RPM for 5 minutes using a homomixer, and cooled to produce an oil-in-water cream.

division ingredient Content (% by weight) Awards Purified water to 100 Triethanolamine 2.10 Glyceryl stearate 0.80 FAGE -100 stearate 0.90 Polysorbate 60 1.20 Sorbitan stearate 0.50 Cetearyl alcohol 3.50 glycerin 8.00 Butylene glycol 5.00 Methylparaben 0.20 Phenoxyethanol 0.15 Paid C12-15 alkyl benzoate 5.00 Hexyl laurate 11.00 Cyclopentasiloxane 3.00 Spices 0.10

The retention positions of the peaks of the four ultraviolet shielding components are checked from the standard solution, and it is confirmed that these components do not overlap with each other, and other cosmetic ingredients among the O / W lotion and the O / It was observed whether or not the matrix of the formulations had an influence. The peak retention times of the four ultraviolet blocking components are shown in Table 4 below.

PSA BM EMC EHS Peak hold time
(minute) 0.833 10,000 11.358 13.775

As a result of comparing the chromatograms of the standard solution and the blank test solution, it was confirmed in FIG. 1 that there is no other specific peak in the positions of the four ultraviolet blocking components.

Also, it was confirmed that the peaks of the four ultraviolet blocking components can be analyzed simultaneously without overlapping.

(2) Linearity ( Linearity )

A standard solution (tetrahydrofuran: methanol: distilled water = 9: 1: 10 (volume ratio)) was prepared as shown in Table 5 to examine the linearity of the quantitative concentration range at the time of testing the contents of the four ultraviolet blocking components. A calibration curve was created using the concentration of each of the components and the intensity of the signal, and the results are shown in FIG.

Flask ID
(Standard solution) Concentration (mg / L) flask
Size (mL) From
Flask * volume
(mL) PSA BM EMC EHS A 400 500 750 500 100 B 200 250 375 250 50 A 25 C 100 125 187.5 125 50 B 25 D 50 62.5 93.75 62.5 50 C 25 E 25 31.25 46.875 31.25 50 D 25

* From Flask means that 25 ml is taken from the standard solution in the column and placed in 50 ml flask.

The four ultraviolet screening components were suitable for the linearity item with R2 greater than 0.999 in the test concentration range. R2 is closer to 1, which means a better value. In general, when R2 is 0.995 or more, R2 can be used as reliable data.

(3) Repeatability ( Repeatability )

The standard deviation and the relative standard deviation of peak area and retention time were calculated six times in succession using the standard solution prepared in accordance with Table 5 above. The repeatability results for each UV blocking component are shown in Table 6 below.

PSA BM EMS EHS Number of injections Peak area
(Area) stay
Time (minutes) Peak area
(Area) stay
Time (minutes) Peak area
(Area) stay
Time (minutes) Peak area
(Area) stay
Time (minutes) One 1662482.866 0.833 718736.578 10,000 3678914.922 11.358 405410.000 13.775 2 1671641.129 0.833 720467.944 10,000 3703298.806 11.358 405723.000 13.767 3 1683200.286 0.833 729860.140 10,000 3731870.860 11.358 410418.000 13.767 4 1693189.690 0.825 732876.251 9.992 3755558.249 11.350 411748.750 13.758 5 1675973.176 0.833 725390.743 10,000 3714729.757 11.358 406674.750 13.767 6 1679339.935 0.825 727510.694 9.992 3740992.306 11.358 410343.500 13.767 Average 1677637.847 0.830 725807.058 9.997 3720894.150 11.357 408386.333 13.767 Standard Deviation 10431.710 0.0041 5440.119 0.0041 27697.925 0.0033 2762.080 0.0054 Relative standard
Deviation (≤1%) 0.622 0.498 0.750 0.041 0.744 0.029 0.676 0.039

Repeatability was measured by injecting the standard solution six times. As a result, the relative standard deviation of the peak area and retention time was less than 1%, which satisfied the criterion.

The relative standard deviation of the results was less than 1%.

(4) precision in laboratory Intermediate precision )

The contents of the UV blocking components were measured on the same sample on the test day and the test taker. The in-vitro precision results for each UV blocking component are shown in Table 7 below.

Measurement date Tester content(%) Sample # 1 Sample # 2 Sample # 3 PSA July 26, 2012 KJH 1.793 1.794 1.832 July 27, 2012 PDK 1.799 1.771 1.748 statistics Average 1.789 Standard Deviation 0.028 Relative standard deviation (≤2%) 1.572 BM July 26, 2012 KJH 2.189 2.188 2.214 July 27, 2012 PDK 2.195 2.141 2.113 statistics Average 2.173 Standard Deviation 0.038 Relative standard deviation (≤2%) 1.747 EMS July 26, 2012 KJH 3.812 3.795 3.874 July 27, 2012 PDK 3.831 3.757 3.706 statistics Average 3.796 Standard Deviation 0.058 Relative standard deviation (≤2%) 1.539 EHS July 26, 2012 KJH 4.090 4.060 4.169 July 27, 2012 PDK 4.117 4.037 3.977 statistics Average 4.075 Standard Deviation 0.067 Relative standard deviation (≤2%) 1.633

* KJH and PDK are initials of the experimenter

The relative standard deviation results for the content of UV-blocking ingredients in the same sample were less than 2% and met the criteria.

(5) System stability system stability )

To determine the stability of the liquid chromatography system over time and to determine whether the standard liquid was stable within a predetermined time, the standard liquid prepared in Table 4 was added to the liquid at a predetermined cycle, that is, 24 hours after the preparation, 48 hours after the production Respectively. The system stability results of each ultraviolet blocking component are shown in Table 8 below.

PSA BM EMS EHS Injection time Peak area
(Area) stay
Time (minutes) Peak area
(Area) stay
Time (minutes) Peak area
(Area) stay
Time (minutes) Peak area
(Area) stay
Time (minutes) During manufacture 1662482.866 0.833 718736.578 10 3678914.922 11.358 405410 13.775 24 hours 1668491.938 0.833 719082.869 10 3694786.631 11.358 405770 13.767 48 hours 1669496.592 0.833 717132.153 10 3700854.097 11.367 405576 13.775 Average 1666823.799 0.833 718317.200 10,000 3691518.550 11.361 405585.333 13.772 Standard Deviation 3792.770 0.000 1040.784 0.000 11328.818 0.005 180.181 0.005 Relative standard
Deviation (≤2%) 0.228 0.000 0.145 0.000 0.307 0.046 0.044 0.034

When the standard solution was injected after 24 hours and 48 hours, respectively, the relative standard deviation of the peak area and the retention time was less than 2%, and it was confirmed that the system stability against the standard solution and the analytical method was appropriate. Respectively.

(6) Accuracy ( Accuracy )

The cream formulations were prepared in the same manner as in the conventional cream production method, and the recovery rates were calculated using the content of the ultraviolet blocking ingredients contained in the preparation and the content calculated through analysis.

division ingredient Content (% by weight) Awards Purified water to 100 Phenylbenzimidazolesulfonic acid 3.50 Triethanolamine 2.10 Glyceryl stearate 0.80 FAGE -100 stearate 0.90 Polysorbate 60 1.20 Sorbitan stearate 0.50 Cetearyl alcohol 3.50 glycerin 8.00 Butylene glycol 5.00 Methylparaben 0.20 Phenoxyethanol 0.15 Paid Butyl methoxydibenzoylmethane 3.00 To a solution of < RTI ID = 0.0 & 7.00 To a solution of < RTI ID = 4.50 C12-15 alkyl benzoate 5.00 Hexyl laurate 11.00 Cyclopentasiloxane 3.00 Spices 0.10

The accuracy results for each UV blocking component are shown in Table 10 below.

Analysis item sample Sample volume (g) density Peak area (AREA) Measurement concentration
(mg / L) Recovery rate (mg / L) Injection 1 Injection 2 Injection 3 (%) PSA One 1.0051 348.22 5725978.714 5892510.078 5743478.941 356.46 102.37 2 0.9973 350.95 5754136.000 5655168.554 5541878.012 350.75 99.94 3 0.9994 350.21 5846926.824 5516529.250 5587392.482 350.01 99.94 BM One 1.0051 301.14 1887340.250 1933039.750 1844079.500 300.47 99.78 2 0.9973 298.18 1871782.500 1861685.250 1820785.250 296.93 99.58 3 0.9994 300.81 1931255.000 1818357.000 1849360.500 298.69 99.29 EMS One 1.0051 702.67 13205312.000 13518288.750 12905381.500 704.89 100.32 2 0.9973 695.76 13101443.500 13040423.500 12752001.250 697.23 100.21 3 0.9994 701.90 13523330.750 12703317.000 12881447.000 699.59 99.67 EHS One 1.0051 451.72 1280015.250 1304509.000 1245229.500 454.38 100.59 2 0.9973 447.27 1264431.250 1258586.500 1231784.500 448.97 100.38 3 0.9994 451.22 1302101.500 1222967.500 1241368.000 449.42 99.60

4. Analysis of ultraviolet shielding component using the present invention

(1) Analytical instruments ( HPLC ) Condition

A UV-2075/2070 Ubite detector was connected to Jasco HPLC 2000 Series liquid chromatography of Jasco for the analysis of UV blocking components using the present invention.

The column was a Phenomenex Bondclone 10u C18 column (3.9 mm x 15.0 cm) and the data was processed using Jasco's Browin Software Operation program.

(2) UV blocking agent

For the analysis of the ultraviolet shielding component using the present invention, four types of ultraviolet shielding components as shown in Table 11 were analyzed.

Ingredients product name INCI Abbreviation manufacturer Lipophilic Butyl methoxydibenzoylmethane Parsol 1789 Butyl Methoxydibenzoylmethane BM DSM Nutritional Products Ltd. Ethyl hexylmethoxycinnamate Parsol MCX Ethylhexyl
Methoxy
Cinnamate, EMC Ethylhexyl salicylate Parsol EHS Ethyl
Hexyl
Salicylate, EHS Hydrophilic Phenylbenzimidazolesulfonic acid Parsol HS Phenyl
Benzimidazole
Sulfonic Acid PSA

(3) Analysis of ultraviolet screening components

Example  One: Wastewater  Analysis of sunscreen ingredients in form cream

In order to confirm the method of analyzing the ultraviolet shielding component of the present invention in the cream of the water in the form of water, the lotion was prepared in the composition shown in Table 12 below. The oil phase and water phase were dissolved by heating at 80 ° C, The mixture was emulsified at 5,000 RPM for 5 minutes using a mixer and cooled to prepare a cream in the form of water.

division ingredient Content (% by weight) Paid Butyl methoxydibenzoylmethane 3.00 To a solution of < RTI ID = 0.0 & 7.00 To a solution of < RTI ID = 4.50 C12-15 alkyl benzoate 5.00 Hexyl laurate 5.00 Three tilipies / piperazine-10/1 dimethicone 3.50 Cyclopentasiloxane 3.00 Spices 0.10 Awards Purified water to 100 Phenylbenzimidazolesulfonic acid 3.50 Triethanolamine 2.10 Butylene glycol 5.00 glycerin 8.00 Methylparaben 0.20 Phenoxyethanol 0.15

1.003 g of the prepared cream in water was precisely weighed, dispersed in 50 ml of mobile phase, and further added with mobile phase to make 100 ml, which was then used as a sample solution for filtration.

30.1 mg of butyl methoxydibenzoylmethane (BM), 70 mg of ethylhexyl methoxycinnamate (EMC), 44.9 mg of ethylhexyl salicylate (EHS), 40 mg of phenylbenzimidazole Sulfonic Acid, PSA) were added to each well and dispersed in 50 ml of mobile phase. The mobile phase was further added to make 100 ml, which was then filtered and used as a standard solution.

Test solution and standard solution 10ul each was taken and tested according to the liquid chromatographic method under the conditions of Table 1 to determine the peak areas A _T and A _S of ultraviolet components. The test solution means a product prepared by diluting a cosmetic formulation in a mobile phase, and the standard solution means that four kinds of ultraviolet blocking components are diluted in a mobile phase.

[formula]

= Amount of UV blocking ingredient (mg) × Ar / As

FIG. 3 shows the chromatogram of the ultraviolet blocking components in the creamy water using the above analysis method. The results are shown in Table 13 below.

Ingredients Analytical amount (%) Content in product (%) Content relative to analytical amount (%) Butyl methoxydibenzoylmethane 3.48 3.52 101.0 Ethyl hexylmethoxycinnamate 3.01 3.00 99.5 Ethylhexyl salicylate 7.00 6.99 99.9 Phenylbenzimidazolesulfonic acid 4.49 4.48 99.8

As shown in Table 11, it was confirmed that the content of the ultraviolet blocking components in the cream formulation was within 100 ± 2% of the analytical amount.

Example  2: Oil oil  Simultaneous analysis of UV-blocking agents in lotions of the form

In order to confirm the method of analyzing the ultraviolet blocking component of the present invention in a lotion for underwater lotion, a lotion was prepared in the composition shown in the following Table 14, and the water phase and the oil phase were respectively dissolved by heating at 80 DEG C and then the oil phase was slowly added to the aqueous phase. And emulsified at 5,000RPM for 5 minutes and cooled to prepare a lotion in the form of an oil-in-water oil.

division ingredient Content (% by weight) Paid Butyl methoxydibenzoylmethane 3.00 To a solution of < RTI ID = 0.0 & 7.00 To a solution of < RTI ID = 4.50 C12-15 alkyl benzoate 6.00 Hexyl laurate 15.00 Three tilipies / piperazine-10/1 dimethicone 3.50 Cyclopentasiloxane 3.00 Spices 0.10 Awards Purified water to 100 Phenylbenzimidazolesulfonic acid 3.50 Triethanolamine 2.10 Butylene glycol 5.00 glycerin 8.00 Methylparaben 0.20 Phenoxyethanol 0.15

0.9939 g of the prepared oil-in-water lotion was precisely weighed, dispersed in 50 ml of mobile phase, and further added with mobile phase to make 100 ml, which was then used as a sample solution for filtration.

A standard solution was prepared in the same manner as in Example 1 and tested according to a liquid chromatographic method to determine peak areas A _T and A _S of ultraviolet components.

The chromatogram of the ultraviolet blocking components in the lotion of the underwater using the above analysis method is shown in FIG. 4. The content of the chromatogram is shown in Table 15 below.

Ingredients Analytical amount (%) Content in product (%) Content relative to analytical amount (%) Butyl methoxydibenzoylmethane 3.48 3.52 101.1 Ethyl hexylmethoxycinnamate 3.01 3.00 99.6 Ethylhexyl salicylate 7.00 7.00 100.0 Phenylbenzimidazolesulfonic acid 4.49 4.48 99.7

As shown in Table 13, it was confirmed that the content of the ultraviolet shielding components in the lotion formulation in the oil-in-water type was within 100 ± 2% of the analytical amount.

Example  3: Wastewater  Simultaneous analysis of UV-blocking agents in lotions of the form

In order to confirm the method of analyzing the ultraviolet screening component of the present invention in a lotion with a water-in-oil form, a lotion was prepared according to the composition shown in Table 16 below, and the water phase and water phase were dissolved by heating at 80 ° C, The mixture was emulsified at 5,000 RPM for 5 minutes using a mixer and cooled to prepare a lotion in the form of water.

division ingredient Content (% by weight) Paid Butyl methoxydibenzoylmethane 3.00 To a solution of < RTI ID = 0.0 & 7.00 To a solution of < RTI ID = 4.50 C12-15 alkyl benzoate 6.00 Hexyl laurate 15.00 Three tilipies / piperazine-10/1 dimethicone 3.50 Cyclopentasiloxane 3.00 Spices 0.10 Awards Purified water to 100 Phenylbenzimidazolesulfonic acid 3.50 Triethanolamine 2.10 Butylene glycol 5.00 glycerin 8.00 Methylparaben 0.20 Phenoxyethanol 0.15

1.0132 g of the prepared lotion in the form of water was precisely weighed and dispersed in 50 ml of mobile phase, and then the mobile phase was further added to make 100 ml, which was then filtered to be used as a sample solution.

A standard solution was prepared in the same manner as in Example 1 and tested according to a liquid chromatographic method to determine peak areas A _T and A _S of ultraviolet components.

FIG. 5 shows chromatograms of ultraviolet blocking components of the lotion in the form of water using the above analysis method. The results are shown in Table 17 below.

Ingredients Analytical amount (%) Content in product (%) Content relative to analytical amount (%) Butyl methoxydibenzoylmethane 3.48 3.47 99.6 Ethyl hexylmethoxycinnamate 3.01 3.05 101.2 Ethylhexyl salicylate 7.00 7.06 100.8 Phenylbenzimidazolesulfonic acid 4.49 4.58 101.9

As shown in Table 17, it was confirmed that the contents of ultraviolet blocking components in the lotion formulation in the water-in-oil form showed a consistent result within 100 ± 2% of the analytical amount.

Example  4: Wastewater  Simultaneous analysis of UV blocking components in solid cream of the type

In order to confirm the method of analyzing the ultraviolet shielding component of the present invention in a creamy water-type solid cream, a cream was prepared according to the composition shown in Table 18 below. The oil phase and water phase were dissolved by heating at 80 ° C, And emulsified at 5,000 RPM for 5 minutes using a homomixer and cooled to produce a solid cream in the form of water.

division ingredient Content (% by weight) Paid Butyl methoxydibenzoylmethane 3.00 To a solution of < RTI ID = 0.0 & 7.00 To a solution of < RTI ID = 4.50 C12-15 alkyl benzoate 6.00 Ozokerite 10.00 Three tilipies / piperazine-10/1 dimethicone 3.50 Cyclopentasiloxane 8.00 Spices 0.10 Awards Purified water to 100 Phenylbenzimidazolesulfonic acid 3.50 Triethanolamine 2.10 Butylene glycol 5.00 glycerin 8.00 Methylparaben 0.20 Phenoxyethanol 0.15

1.0101 g of solid cream in the form of water was added to accurately disperse 50 ml of the mobile phase, and then the mobile phase was further added to make 100 ml, which was then filtered to be used as a sample solution.

A standard solution was prepared in the same manner as in Example 1 and tested according to a liquid chromatographic method to determine peak areas A _T and A _S of ultraviolet components.

FIG. 6 shows chromatograms of the ultraviolet blocking components in the water-in-oil type solid cream using the above analysis method. The results are shown in Table 19 below.

Ingredients Analytical amount (%) Content in product (%) Content relative to analytical amount (%) Butyl methoxydibenzoylmethane 3.48 3.50 100.7 Ethyl hexylmethoxycinnamate 3.01 3.06 101.5 Ethylhexyl salicylate 7.00 7.10 101.4 Phenylbenzimidazolesulfonic acid 4.49 4.57 101.8

As shown in Table 19, it was confirmed that the content of the ultraviolet blocking components in the water-in-oil type solid cream formulation was within 100 ± 2% of the analytical amount.

Example  5: Oil oil  Simultaneous analysis of UV blocking agents in form foundations

In order to confirm the method of analyzing the ultraviolet shielding component of the present invention in an oil-in-water type foundation, a foundation was prepared according to the composition shown in the following Table 20. The water phase and the oil phase were dissolved by heating at 80 ° C, The emulsion was emulsified at 5,000 RPM for 5 minutes using a mixer and cooled to prepare an oil-in-water type foundation.

division ingredient Content (% by weight) Awards Purified water to 100 Phenylbenzimidazolesulfonic acid 3.50 Triethanolamine 2.10 Glyceryl stearate 0.80 FAGE -100 stearate 0.90 Polysorbate 60 1.20 Sorbitan stearate 0.50 Cetearyl alcohol 3.50 glycerin 8.00 Butylene glycol 5.00 Titanium dioxide 8.00 Red iron oxide 0.30 Yellow iron oxide 0.80 Black iron oxide 0.10 Methylparaben 0.20 Phenoxyethanol 0.15 Paid Butyl methoxydibenzoylmethane 3.00 To a solution of < RTI ID = 0.0 & 7.00 To a solution of < RTI ID = 4.50 C12-15 alkyl benzoate 5.00 Hexyl laurate 9.00 Cyclopentasiloxane 3.00 Spices 0.10

1.0191 g of the prepared oil-in-water type foundation was precisely weighed and dispersed in 50 ml of mobile phase, and then further mobile phase was added to make 100 ml, which was then used as a sample solution for filtration.

A standard solution was prepared in the same manner as in Example 1 and tested according to a liquid chromatographic method to determine peak areas A _T and A _S of ultraviolet components.

7 shows chromatograms of ultraviolet blocking components in an oil-in-water type foundation using the above analysis method. The results of the content measurement are shown in Table 21 below.

Ingredients Analytical amount (%) Content in product (%) Content relative to analytical amount (%) Butyl methoxydibenzoylmethane 3.48 3.50 100.7 Ethyl hexylmethoxycinnamate 3.01 3.06 101.5 Ethylhexyl salicylate 7.00 7.10 101.4 Phenylbenzimidazolesulfonic acid 4.49 4.57 101.8

As shown in Table 21, it was confirmed that the content of the ultraviolet shielding components in the oil-in-water type foundation formulation was within 100 ± 2% of the analytical amount.

Example  6: Wastewater  Form Foundation  Simultaneous analysis of UV blocking ingredients

In order to confirm the assay method of the ultraviolet shielding component of the present invention in a water-in-oil type foundation, a foundation was prepared according to the composition shown in the following Table 22. The oil phase and water phase were each dissolved by heating at 80 DEG C, the aqueous phase was slowly added to the oil phase, Was emulsified at 5,000RPM for 5 minutes and cooled to prepare a foundation in the form of water.

division ingredient Content (% by weight) Paid Butyl methoxydibenzoylmethane 3.00 To a solution of < RTI ID = 0.0 & 7.00 To a solution of < RTI ID = 4.50 C12-15 alkyl benzoate 5.00 Hexyl laurate 5.00 Three tilipies / piperazine-10/1 dimethicone 3.50 Cyclopentasiloxane 3.00 Titanium dioxide 8.00 Red iron oxide 0.30 Yellow iron oxide 0.80 Black iron oxide 0.10 Spices 0.10 Awards Purified water to 100 Phenylbenzimidazolesulfonic acid 3.50 Triethanolamine 2.10 Butylene glycol 5.00 glycerin 8.00 Methylparaben 0.20 Phenoxyethanol 0.15

1.0098 g of the above-prepared water-in-oil type foundation was precisely weighed and dispersed by adding 50 ml of mobile phase, and further added with mobile phase to make 100 ml, which was then filtered to be used as a sample solution.

A standard solution was prepared in the same manner as in Example 1 and tested according to a liquid chromatographic method to determine peak areas A _T and A _S of ultraviolet components.

8 shows chromatograms of ultraviolet blocking components in a water-in-oil type foundation using the above analysis method. The results are shown in Table 23 below.

Ingredients Analytical amount (%) Content in product (%) Content relative to analytical amount (%) Butyl methoxydibenzoylmethane 3.48 3.51 100.7 Ethyl hexylmethoxycinnamate 3.01 3.06 101.8 Ethylhexyl salicylate 7.00 7.11 101.6 Phenylbenzimidazolesulfonic acid 4.49 4.58 101.9

As shown in Table 22, it was confirmed that the content of ultraviolet blocking components in the water-in-oil type foundation formulation was within 100 ± 2% of the analytical amount.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, It will be obvious to those of ordinary skill in the art.

Claims (9)

Butyl methoxydibenzoylmethane (BM), ethylhexyl methoxycinnamate (EMC), ethylhexyl salicylate (EHS), and phenylbenzimidazole sulfonic acid (PSA) Adding a mixed solvent containing tetrahydrofuran, methanol and distilled water to a cosmetic composition containing an ultraviolet shielding component containing the ultraviolet shielding component;
Introducing the ultraviolet blocking component extracted in the reversed phase nonpolar column packed with at least one member selected from the group consisting of octadecylsilane (C18), dodecylsilane (C12) and octasilane (C8) as the stationary phase; And
Analyzing the ultraviolet blocking component using liquid chromatography using the mixed solvent as a mobile phase
/ RTI > of the UV-blocking component.
The method according to claim 1, wherein the mixed solvent is a mixture of tetrahydrofuran and methanol in a volume ratio of 9: 1 to 19: 1, based on 10 volumes of distilled water.
The method of claim 1, wherein the length of the reversed phase non-polar column is greater than 7.5 cm and less than 25 cm.
delete delete The method of claim 1, wherein the cosmetic composition is selected from the group consisting of creams, lotions, solid creams and foundations.
delete The method according to claim 1, wherein the mixed solvent in the step of extracting the ultraviolet shielding component is used in an amount of 0.25 to 10.00 parts by weight per 100 parts by weight of the cosmetic composition.
The method of claim 1, wherein the analyzing method comprises confirming the analysis result through a detector having a wavelength adjusted to a range of 300 nm to 320 nm.

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