KR100897519B1 - Simultaneous screening method for Sunscreen Agents - Google Patents

Abstract

The present invention relates to simultaneous analysis of sunscreen ingredients of different chemical properties, and more particularly, to simultaneous analysis of hydrophilic and lipophilic sunscreen ingredients in cosmetics using liquid chromatography (HPLC) at the same time. will be.

Sunscreen, Liquid Chromatography (HPLC), Ethylhexyl Methoxycinnamate (OMC), Isoamyl p-Methoxycinnamate (IMC), Ethylhexyl Salicylate (Ethylhexyl Salicylate) , OS), Ethylhexyl Triazone (OT), Methylene Bis-Benzotriazolyl Tetramethylbutylphenol, Tinosorb M, Bisethylhexyloxyphenol Methoxyphenyl Methoxyphenyl Triazine, Tinosorb S)

Description

Simultaneous analysis of sunscreen ingredients {Simultaneous screening method for Sunscreen Agents}

The present invention relates to the simultaneous analysis of sunscreen ingredients of different chemical properties, and more particularly, to a simultaneous analysis method for simultaneously and accurately analyzing hydrophilic and lipophilic sunscreen ingredients present in cosmetics using liquid chromatography (HPLC). will be.

As the frequency of skin cancer and photoaging caused by ultraviolet rays increases, the need for good sunscreen ingredients to prevent harmful effects of ultraviolet rays on human skin is increasing. Chemical sunscreen ingredients that are widely used in recent years are compounds that absorb or reflect ultraviolet rays to minimize the harmful effects of ultraviolet rays on the skin. Of these, methylene bis-benzoxazolyl tetramethylbutylphenol (Tinosorb M) and bisethylhexyloxyphenol Methoxyphenyl Triazine (Tinosorb S) are very useful with strong lipophilic properties. Known as a UV-A sunscreen ingredient, Ethylhexyl Methoxycinnamate (OMC), Isoamyl p-Methoxycinnamate (IMC), Ethylhexyl Salicylate, OS) and ethylhexyl triazone (OT) are widely used as UV-B sunscreen ingredients.

Thin layer chromatography (TLC), liquid chromatography (HPLC) and gas chromatography (GC) have been used to analyze sunscreen ingredients in cosmetics. However, these methods have not been reported for the simultaneous analysis of UV-A sunscreen components having strong lipophilic properties with UV-B sunscreen components having hydrophilic properties.

Accordingly, the present inventors propose a simultaneous analysis method based on liquid chromatography (HPLC) of lipophilic and hydrophilic sunscreen ingredients in cosmetics. This method is suitable for quality control of sunscreen ingredients in cosmetics because it can be analyzed quickly with high separation and can be analyzed more economically and effectively.

The present invention seeks to provide an optimal liquid chromatography (HPLC) analysis method for simultaneously and accurately analyzing two groups of sunscreen ingredients having different chemical properties in cosmetics.

The present invention relates to the simultaneous analysis of sunscreen ingredients of different chemical properties, and more particularly, to a simultaneous analysis method for simultaneously and accurately analyzing hydrophilic and lipophilic sunscreen ingredients present in cosmetics using liquid chromatography (HPLC). will be.

Hereinafter, the present invention will be described in detail.

Simultaneous analysis of the sunscreen component according to the present invention consists of the following steps.

1) extracting a lipophilic and hydrophilic sunscreen component by adding a mixed solvent of dimethylformamide and methanol in a volume ratio of 1: 0.9 to 1.2 to the cosmetic containing a lipophilic and hydrophilic sunscreen component;

2) injecting the lipophilic and hydrophilic sunscreen components extracted in step 1) into a reversed phase nonpolar column filled with octadecylsilane (C18), dodecylsilane (C12) or octasilane (C8) having a nonpolarity as a stationary phase; ; And

3) Qualitative and quantitative analysis of lipophilic and hydrophilic UV blocking components by liquid chromatography using a mixed solvent of water and ethanol or ethanol as a mobile phase

The lipophilic sunscreen component is methylene bis-Benzotriazolyl Tetramethylbutylphenol (Tinosorb M) or bisethylhexyloxyphenol Methoxyphenyl Triazine, Tinosorb S Sunscreen ingredients include Ethylhexyl Methoxycinnamate (OMC), Isoamyl p-Methoxycinnamate (IMC), Ethylhexyl Salicylate (OS) or Ethyl hexyltria As the zone (Ethylhexyl Triazone, OT), the following structure is shown.

In order to extract the lipophilic and hydrophilic sunscreen ingredients present in the cosmetics in step 1), a mixed solvent having a polar difference, that is, dimethylformamide and methanol is mixed in a volume ratio of 1: 0.9 to 1.2. Most preferably, a mixed solvent in which dimethylformamide and methanol are mixed in a volume ratio of 1: 1. Methylenebisbenzotriazolyltetramethylbutylphenol (Tinosorb M) and bisethylhexyloxyphenol methoxyphenyltriazine (Tinosorb S), which are lipophilic sunscreen components, are dissolved in dimethylformamide and ethyl is a hydrophilic sunscreen component. Hexylmethoxycinnamate (OMC), isoamyl-p-methoxycinnamate (IMC), ethylhexyl salicylate (OS) and ethylhexyltriazone (OT) are dissolved in methanol.

The cosmetics are selected from the group consisting of lotions, essences, foundations, powders, lipsticks or twin pacts containing lipophilic and hydrophilic sunscreen ingredients.

The column used in step 2) is preferably a reverse phase nonpolar column filled with octadecylsilane (C18), dodecylsilane (C12) or octasilane (C8) having a nonpolarity in the fixed phase. When using a C12 or C8 column, the separation of the sunscreen components of different chemical properties is reduced, so the C18 column is most preferred for accurate analysis.

The length of the C18 column is related to the analysis time, and there are 25 cm, 10 cm, and 7.5 cm, and the 7.5 cm column is most suitable in consideration of rapidity.

As the mobile phase in step 3), ethanol and water having a polarity difference are used to simultaneously move the lipophilic and hydrophilic sunscreen components.

In case of using methanol or acetonitrile instead of ethanol, some ultraviolet components overlap and there is a problem that accurate analysis is difficult.

The hydrophilic sunscreen ingredients are first separated with a mixed solvent of ethanol and water mixed in a volume ratio of 1: 3 to 9, which is an optimum ratio with respect to time, and the lipophilic sunscreen ingredients are separated under 100% ethanol condition without water. The method is preferred.

As a result of quantifying the sunscreen ingredients in the cosmetic using simultaneous analysis of sunscreen ingredients with different chemical properties according to the present invention, all 6 sunscreen ingredients in the calibration curve were R ² in the concentration range of 5 to 200 ㎍ / ml. Good linearity of = 0.999 or more is shown. In addition, the simultaneous analysis method of the sunscreen ingredients according to the present invention has the effects of excellent sensitivity, reproducibility, accuracy, shorten the analysis time, low cost and simplicity, and can be effectively and widely applied for quality control of sunscreen ingredients in cosmetics. have.

As described above, the simultaneous analysis of UV blocking components of the present invention has the effects of reproducibility, accuracy, shortening between analyzers, low cost and simplicity. Therefore, the simultaneous analysis method of the sunscreen ingredients of different chemical properties of the present invention can effectively detect the sunscreen ingredients present in the external composition of the skin, it can be widely applied to the quality control of sunscreen ingredients in cosmetics. In addition, the lipophilic and hydrophilic properties of the sunscreen compound can be analyzed at the same time, and will be effectively applied to the new sunscreen ingredients in the future.

Hereinafter, the configuration and effects of the present invention will be described in more detail with reference to Examples and Test Examples. However, these experimental examples and examples are provided only for the purpose of illustration to help the understanding of the present invention is not limited to the scope and scope of the present invention by the following examples and experimental examples.

Example 1 Selection of Optimum Conditions (Column and Mobile Phase)

In order to accurately analyze the six sunscreen components having different chemical properties (Tinosorb M, Tinosorb S, OMC, IMC, OS, OT) with a high degree of separation, the following experiment was performed.

1. Optimal column  Experiment for selection

The most commonly used type of column as a fixed phase in liquid chromatography is C18, a reverse phase nonpolar column, which is filled with 18 non-polar carbon chains inside the column, and since the polar component does not bind with the nonpolar column functional group, Elution and the nonpolar component elutes slowly in combination with the nonpolar functional group. According to this principle, the difference in polarity of the components allows the separation of the individual components in the mixture.

Methylenebisbenzotriazolyltetramethylbutylphenol (Tinosorb M) and bisethylhexyloxyphenolmethoxyphenyltriazine (Tinosorb S) are lipophilic compounds with nonpolar properties and are separated only in reverse phase conditions without water. Under these conditions, however, polar hydrophilic ethylhexylmethoxycinnamate (OMC), isoamyl-p-methoxycinnamate (IMC), ethylhexylsalicylate (OS) and ethylhexyltriazone (OT) Due to the reduced binding capacity with the non-polar functional groups of the stationary phase, it is rapidly eluted, causing interference with other polar components in the sample. As a result, accurate analysis is difficult due to low separation.

The six UV blocking components are so satisfactory that the difference in chemical properties is sufficient to increase the length of the column which is a stationary phase that separates the components when setting the appropriate retention time and analysis conditions without the interference of the matrix. Hard to find In this case, the functional phase of the column of the stationary column was used as a non-polar cyan column (column with CN functional groups) than the C18 column having 18 carbon atoms, but in this case, the separation degree of the six UV blocking components is C18 column. Although better, the analysis time exceeded 30 minutes and was not suitable for the efficiency of the analysis. In the case of using an amine column (column with NH ₂ functional groups), which is a polar column, the polarity is a polar component, and the nonpolar component is a lipophilic methylenebisbenzotriazolyl having a strong nonpolar property according to the principle that the binding ability is strong. Tetramethylbutylphenol (Tinosorb M) and bisethylhexyloxyphenolmethoxyphenyltriazine (Tinosorb S) were released without binding to the polar amine column, making it difficult to detect these components in liquid chromatography. Eventually a C18 nonpolar column was chosen as the stationary phase for proper separation, and a short column of 7.5 cm was selected for the sake of speed.

2. to improve separation Mobile phase  Conditional setting experiment

Liquid chromatography has the principle of separating the components according to the polarity difference by the interaction of the stationary column with the mobile phase and the analyte. Therefore, the polarity of the mobile phase as well as the type of material packed in the column is the main factor in setting the analysis conditions. Therefore, in the case of using a nonpolar column, the mobile phase having a high polarity elutes the components quickly and the mobile phase having a nonpolar polarity elutes the components slowly. Thus, the polarity difference of the mobile phases allows the components in the mixture to be separated without overlap.

The lipophilic methylenebisbenzotriazolyltetramethylbutylphenol (Tinosorb M) and bisethylhexyloxyphenol methoxyphenyltriazine (Tinosorb S) were converted into hydrophilic ethylhexylmethoxycinnamate (OMC) and isoamyl-p-meth Several organic solvents suitable as mobile phases were used in the experiments for simultaneous analysis with oxycinnamate (IMC), ethylhexylsalicylate (OS) and ethylhexyltriazone (OT). When methanol is used as the first mobile phase, the residence time of methylenebisbenzotriazolyltetramethylbutylphenol (Tinosorb M) and bisethylhexyloxyphenol methoxyphenyl triazine (Tinosorb S) is too slow, and the analysis time is long. As a result, asymmetrical tailings were observed in the shape of peaks, making it difficult to derive accurate analysis results.

In the case of using acetonitrile, which is slightly less polar than the second methanol, as the organic solvent, the tailing of the peak was observed as in the case of using methanol, and thus it was found to be inadequate.

When the non-polar ethanol was used as the organic solvent than the third methanol and acetonitrile, the six sunscreens were analyzed with satisfactory separation and peak shape within 10 minutes.

Acetone, hexane, acetic acid, etc., which are more polar solvents than ethanol, have a problem of eluting the above six kinds of UV-blocking components overlapping with each other. If chloroform or water, which is a more polar solvent than methanol, is eluted, It was too slow and the analysis time was too long.

Therefore, it was confirmed that ethanol is the most suitable organic solvent among mobile phases in the simultaneous analysis of the six UV blocking components, and thus the mobile phase conditions as set forth in Table 1 were set. The ratio of water and ethanol for each time period is set in consideration of the polarity difference between the stationary phase, the mobile phase and the components in which the peaks of the six UV blocking components do not overlap and can be optimally separated. That is, the hydrophilic sunscreen components are separated without peak overlap between the components using water as a polar solvent to have a proper retention time in the nonpolar column, and the lipophilic sunscreen components are mobile phase without water so as to quickly elute from the nonpolar column. Analytical conditions for separation under conditions (100% ethanol conditions) were set.

TABLE 1

Therefore, six different sunscreen ingredients with different chemical properties were analyzed directly by liquid chromatography. Specifically, the sunscreen components extracted with a 1: 1 mixture of dimethylformamide and methanol were injected into the liquid chromatography, separated by a column of C18 (length: 7.5 cm, inner diameter: 4.6 mm, particles 3.5 μm), and moved. As a phase, using ethanol and water was carried out as shown in Table 2. At this time, the flow rate of the mobile phase was 1 mL / min, the sample injection amount is 10 μl, it was detected at 310 nm using a UV detector. The temperature of the other columns and the samples was analyzed at room temperature. Hereinafter, all experiments were performed under the conditions of Table 2 below.

TABLE 2

[ Example  2] Simultaneous analysis of six UV blocking components

Six kinds of sunscreen ingredients in cosmetics [methylenebisbenzotriazolyltetramethylbutylphenol (Tinosorb M, hereinafter referred to as 'TM'), bisethylhexyloxyphenol methoxyphenyltriazine (Tinosorb S, hereinafter referred to as 'TS') Specificity to verify the simultaneous analysis of ethylhexylmethoxycinnamate (OMC), isoamyl-p-methoxycinnamate (IMC), ethylhexylsalicylate (OS) and ethylhexyltriazone (OT)]. (Specificity, Linearity, Repeatability, Intermediate precision, System stability and Accuracy) were performed as follows.

1. Specificity

In order to determine whether the analyte can be accurately measured in the presence of impurities, degradation products, and compound components predicted to coexist, the test solution and the standard solution were compared and analyzed to see if there was no interference in the two chromatograms.

A standard solution was prepared by dissolving a total of six sunscreen components [TM, TS, OMC, IMC, OS and OT] in dimethylformamide: methanol = 1: 1 (volume ratio).

The blank test solution was prepared by dissolving the lotion and cream (including all other cosmetic ingredients) prepared in O / W lotion formulation and O / W cream formulation in dimethylformamide: methanol = 1: 1 (volume ratio). Prepared.

The retention positions of the peaks of the six sunscreen ingredients are confirmed from the standard solution, and the six sunscreen ingredients come out without overlap with each other. It was confirmed whether there is an overlap with the matrix effect of the formulation, the peak retention time of the six sunscreen components are shown in Table 3 below.

TABLE 3

In comparison with the chromatogram of the standard solution and the blank test solution it can be seen in Figure 2 that there are no other unusual peaks in the position of the six sunscreen components. In addition, it was confirmed that the peaks of the six UV-blocking components are separated without overlap, so that simultaneous analysis is possible.

2. Linearity

In order to determine the linearity of the quantitative concentration range in the experiment of the content of the six types of UV-blocking components, a standard solution (used solvent dimethylformamide: methanol = 1: 1 by volume) was prepared as shown in Table 4 below. The calibration curve was prepared using the concentration and signal intensity of each of them (FIG. 3).

TABLE 4

In the test concentration range of the six UV-blocking components, R ² is 0.999 or more, and the linearity item is suitable.

3. Repeatability

The standard solution C prepared in Table 4 was measured six times in succession to calculate the standard deviation and relative standard deviation of the peak area and retention time. The repeatability results of isoamyl-p-methoxycinnamate (IMC) and ethylhexylmethoxycinnamate (OMC) are shown in Table 5 below.

TABLE 5

Repeatability was measured by six injections of the standard solution C. As a result, the relative standard deviation of the peak area and the retention time was less than 1%, which satisfies the criteria.

4. In the lab  Precision Intermediate precision )

Different test days, testers, and test equipment were used to measure the content of UV-blocking components in the same sample. In vitro precision results of isoamyl-p-methoxycinnamate (IMC) and ethylhexylmethoxycinnamate (OMC) are shown in Table 6.

TABLE 6

Relative standard deviation results for the content of sunscreen components in the same sample were less than 2% and met the criteria.

5. System stability

In order to determine the stability of the liquid chromatography system and whether the standard solution dissolved in the 1: 1 mixture of dimethylformamide and methanol is stable within a certain time, the standard solution C prepared in Table 4 was subjected to a constant cycle ( At the time of manufacture, after 24 hours, after 48 hours). The system stability results of isoamyl-p-methoxycinnamate (IMC) and ethylhexylmethoxycinnamate (OMC) are shown in Table 7 below.

TABLE 7

When preparing the standard solution, when the sample was injected after 24 hours and after 48 hours, the relative standard deviation result of the peak area and retention time was less than 2%. .

6. Accuracy

In the same formulation, a sample that accurately knows the content of the sunscreen ingredients was calculated through the content and analysis of the sunscreen ingredients prepared by preparing the cream formulation in the same manner as the conventional cream preparation method using the ingredients and contents of Table 8 below. The recovery was determined by the content. The accuracy results of isoamyl-p-methoxycinnamate (IMC) and ethylhexylmethoxycinnamate (OMC) are shown in Table 9 below.

TABLE 8

TABLE 9

[ Example  3] Simultaneous Analysis of 6 UV Protection Components

The following experiment was conducted to simultaneously analyze the sunscreen ingredients present in the cosmetics.

1. Analyzer ( HPLC ) Condition

The liquid chromatography used in the experiment is Waters's Alliance 2695, to which a 2996 photodiode array UV detector (PDA) is connected. The column used a Waters symmetry C18 column (4.6 mm x 7.5 cm, 3.5 μm), and data processing was performed using Waters' Empower II program.

2. Standard

Standard products used for the simultaneous analysis of six different sunscreen components are shown in Table 10 below.

TABLE 10

3. Simultaneous Analysis of UV Protection Components in Lotion

To confirm the simultaneous analysis of the sunscreen ingredients in the lotion lotion was prepared in the composition shown in Table 11 below, each oil phase and water phase was completely dissolved at 70 ℃ and emulsified at 7,000rpm for 5 minutes to prepare a lotion.

TABLE 11

0.2 g of the lotion prepared above was precisely weighed, 50 mL of dimethylformamide was added to disperse, and 50 mL of methanol was added to make a total of 100 mL, and then filtered and used as a sample solution.

40 mg isoamyl-p-methoxycinnamate (IMC), 140 mg ethylhexylmethoxycinnamate (OMC), 90 mg ethylhexylsalicylate (OS) and bisethylhexyloxyphenolmethoxyphenyltriazine (TS) ) Weigh 60 mg, add 50 mL of dimethylformamide to disperse, add 50 mL of methanol to make 100 mL, add 10 mL correctly, and add 90 mL of a mixture of dimethylformamide and methanol (1: 1, v / v). After adjusting 100 mL was used as a standard solution. 10 parts of the sample solution and the standard solution were taken and tested according to the liquid chromatograph method under the conditions of Table 2 to determine the peak areas A _T and A _S of the ultraviolet components.

[formula]

The chromatogram of the sunscreen ingredients in the lotion using the above method is shown in FIG. 4, and the results of the content measurement are shown in Table 12 below.

TABLE 12

As shown in Table 12, the content of the sunscreen ingredients in the lotion formulation is shown to match within 100 ± 2% of the indicated amount.

4. Simultaneous analysis of sunscreen ingredients in creams

Cream was prepared by the composition of Table 13 to confirm the simultaneous analysis of the sunscreen ingredients in the cream, each of the oil phase and water phase was completely dissolved at 70 ℃ and emulsified at 7,000 rpm for 5 minutes to prepare a cream.

TABLE 13

0.2 g of the prepared cream was precisely weighed, 50 mL of dimethylformamide was added and dispersed, and 50 mL of methanol was added to make a total of 100 mL, followed by filtration to use as a sample solution.

40 mg of isoamyl-p-methoxycinnamate (IMC), 100 mg of ethylhexylmethoxycinnamate (OMC), 20 mg of methylenebisbenzotriazolyltetramethylbutylphenol (TM) and bisethylhexyloxyphenolmethoxyphenyl Weigh 60 mg of triazine (TS), add 50 mL of dimethylformamide to disperse, add 50 mL of methanol to make 100 mL, and take 10 mL correctly. Mixture of dimethylformamide and methanol (1: 1, v / v) ) 90mL was added and a total of 100mL was used as a standard solution. 10 parts of the sample solution and the standard solution were taken and tested according to the liquid chromatograph method under the conditions of Table 2 to determine the peak areas A _T and A _S of the ultraviolet components.

[formula]

The chromatogram of the sunscreen ingredients in the cream using the above assay is shown in FIG. 5, and the results of the content measurement are shown in Table 14 below.

TABLE 14

As shown in Table 14, the content of the sunscreen ingredients in the cream formulation is consistent with the results within 100 ± 2% of the indicated amount.

5. Simultaneous Analysis of UV Protection Components in Foundation

In order to confirm the simultaneous analysis method of UV-blocking components in the foundation, it was prepared in the composition shown in Table 15 below. After the oil phase 2 was added, and then completely dissolved at 80 ℃ water phase was prepared by emulsifying at 7,000 rpm for 5 minutes.

TABLE 15

0.2 g of the foundation prepared above was precisely weighed, 50 mL of dimethylformamide was added to disperse, and 50 mL of methanol was added to make a total of 100 mL, and then filtered and used as a sample solution.

Weigh 40 mg of isoamyl-p-methoxycinnamate (IMC) and 100 mg of ethylhexylmethoxycinnamate (OMC), add 50 mL of dimethylformamide to disperse it, add 50 mL of methanol to make a total of 100 mL. 10 mL was correctly taken and 90 mL of a mixture of dimethylformamide and methanol (1: 1, v / v) was added to make a total of 100 mL, which was then used as a standard solution. 10 parts of the sample solution and the standard solution were taken and tested according to the liquid chromatograph method under the conditions of Table 2 to determine the peak areas A _T and A _S of the ultraviolet components.

[formula]

The chromatogram of the sunscreen ingredients in the cream using the assay was shown in FIG. 6, and the content measurement results are shown in Table 16 below.

TABLE 16

As shown in Table 16, the content of the sunscreen ingredients in the foundation formulation is consistent with the results within 100 ± 2% of the displayed amount.

6. Simultaneous Analysis of UV Protection Components in Makeup Base

In order to confirm the simultaneous analysis method of UV-blocking ingredients in the make-up base, it was prepared in the composition shown in Table 17 below. After the oil phase 2 was added, and then completely dissolved at 80 ℃ water phase was prepared by emulsifying 5 minutes at 7,000rpm.

TABLE 17

0.2 g of the makeup base prepared above was precisely weighed, 50 mL of dimethylformamide was added to disperse, 50 mL of methanol was added to make a total of 100 mL, and then used as a sample solution by filtration.

Weigh 140 mg of ethylhexylmethoxycinnamate (OMC), add 50 mL of dimethylformamide, disperse, add 50 mL of methanol to make 100 mL, and take 10 mL correctly. Mixture of dimethylformamide and methanol (1: 1, v / v) 90mL was added to adjust the total 100mL was used as a standard solution. 10 parts of the sample solution and the standard solution were taken and tested according to the liquid chromatograph method under the conditions of Table 2 to determine the peak areas A _T and A _S of the ultraviolet components.

[formula]

The chromatogram of analyzing the sunscreen ingredients in the makeup base using the analysis method is shown in FIG. 7, and the content measurement results are shown in Table 18 below.

TABLE 18

As shown in Table 18, the content of the sunscreen ingredients in the make-up base formulation shows a result within 100 ± 2% of the indicated amount.

7. Simultaneous Analysis of UV Protection Components in Powders

In order to confirm the simultaneous analysis of UV blocking ingredients in the powder was prepared in the composition shown in Table 19. First, the powder phase was mixed at 1200rpm, 5 minutes at room temperature, the oil phase was added and further mixed at 1200rpm for 5 minutes Prepare a powder. The powder thus prepared was pulverized into fine particles using a grinder, and then filtered through a 50 mesh filter net to prepare a powder formulation.

TABLE 19

0.2 g of the powder prepared above was precisely weighed, 50 mL of dimethylformamide was added to disperse, and 50 mL of methanol was added to make a total of 100 mL, which was then filtered and used as a sample solution.

Weigh 20 mg of ethylhexylmethoxycinnamate (OMC), add 50 mL of dimethylformamide, disperse, add 50 mL of methanol to make 100 mL, and take 10 mL correctly. Mixture of dimethylformamide and methanol (1: 1, v / v) 90mL was added to adjust the total 100mL was used as a standard solution. Each sample and 10 standard solutions were taken and tested according to the liquid check chromatography method under the conditions of Table 2 to determine peak areas A _T and A _S of ultraviolet components.

[formula]

The chromatogram of analyzing the sunscreen ingredients in the powder using the above method is shown in FIG. 8, and the results of the content measurement are shown in Table 20 below.

TABLE 20

As shown in Table 20, the content of the sunscreen ingredients in the powder formulation is consistent with the results within 100 ± 2% of the indicated amount.

8. Simultaneous Analysis of UV Protection Components in Twin Pact

In order to confirm the simultaneous analysis method of the sunscreen ingredients in the Twin Pact, the composition of Table 21 was prepared. First, the powder phase was mixed at 1200 rpm for 5 minutes at room temperature, and then the oil phase was added, and the mixture was further mixed at 1200 rpm for 5 minutes. To make powder. The powder thus prepared was pulverized into fine particles using a grinder, and then compressed into a compact using a press.

TABLE 21

0.2 g of the twin pact prepared above was precisely weighed and dispersed by adding 50 mL of dimethylformamide, and then 50 mL of methanol was added to make a total of 100 mL, and then filtered and used as a sample solution.

Weigh 120 mg of ethylhexylmethoxycinnamate (OMC) and 40 mg of bisethylhexyloxyphenolmethoxyphenyltriazine (TS), add 50 mL of dimethylformamide to disperse, add 50 mL of methanol to make a total of 100 mL. 10 mL was correctly taken and 90 mL of a mixture of dimethylformamide and methanol (1: 1, v / v) was added to make a total of 100 mL, which was then used as a standard solution. 10 parts of the sample solution and the standard solution were taken and tested according to the liquid chromatograph method under the conditions of Table 2 to determine the peak areas A _T and A _S of the ultraviolet components.

[formula]

The chromatogram of the sunscreen components of the twin pact was analyzed by using the above method, and is shown in FIG.

Table 22

As shown in Table 22, the content of the sunscreen ingredients in the twin-fact formulation shows a result within 100 ± 2% of the indicated amount.

9. Simultaneous Analysis of Sunscreen Ingredients at Sun Balm

To confirm the simultaneous analysis method of the sunscreen ingredients in the sun balm was prepared in the composition of Table 22, the oil phase was completely dissolved at 80 ℃ and the pigment part was added and dispersed for 10 minutes at 7,000rpm (based on the laboratory TK mixer) It was prepared by adding a flavoring agent through a degassing process.

TABLE 23

0.2 g of the prepared sun chestnut was precisely weighed and dispersed by adding 50 mL of dimethylformamide, and then 50 mL of methanol was added to make a total of 100 mL, and then filtered and used as a sample solution.

Weigh 140 mg of ethylhexylmethoxycinnamate (OMC) and 40 mg of isoamyl-p-methoxycinnamate (IMC), add 50 mL of dimethylformamide to disperse, add 50 mL of methanol to make a total of 100 mL. Take exactly mL and add 90 mL of dimethylformamide and methanol mixture (1: 1, v / v) to adjust the total 100 mL to use as a standard solution. 10 parts of the sample solution and the standard solution were taken and tested according to the liquid chromatograph method under the conditions of Table 2 to determine the peak areas A _T and A _S of the ultraviolet components.

[formula]

The chromatogram of the sunscreen ingredients in sun chestnut was analyzed in FIG. 10 using the above method, and the content measurement results are shown in Table 24 below.

TABLE 24

As shown in Table 24, the content of the sunscreen ingredients in the sun balm formulation is showing a result within 100 ± 2% of the indicated amount.

11. Simultaneous analysis of sunscreen ingredients in lipstick

To confirm the simultaneous analysis of the sunscreen ingredients in the lipstick was prepared in the composition shown in Table 25, Part 1 was dissolved by heating at 90 degrees or more, and then stirred with a homogenizer to make a mixture, Part 2 was added thereto and dispersed. After adjusting the temperature of the mixture to about 75 ~ 80 ℃ and gradually added part 3 while homogeneously mixing with homogenizer was prepared through degassing, fragrance and cooling process.

TABLE 25

0.2 g of the prepared lipstick was precisely weighed and dispersed by adding 50 mL of dimethylformamide, and then 50 mL of methanol was added to make a total of 100 mL, and then used as a sample solution by filtration.

Weigh 40 mg of isoamyl-p-methoxycinnamate (IMC), add 50 mL of dimethylformamide, disperse, add 50 mL of methanol to make 100 mL, and take 10 mL accurately to mix dimethylformamide and methanol (1 : 1, v / v) 90mL was added to adjust the total 100mL was used as a standard solution. 10 parts of the sample solution and the standard solution were taken and tested according to the liquid chromatograph method under the conditions of Table 2 to determine the peak areas A _T and A _S of the ultraviolet components.

[formula]

The chromatogram analyzing the sunscreen ingredients in the lipstick using the above method is shown in FIG. 11, and the results of the content measurement are shown in Table 26 below.

TABLE 26

As shown in Table 26, the content of the sunscreen ingredients in the lipstick formulation shows a result within 100 ± 2% of the indicated amount.

1-6 types of sunscreen ingredients [methylenebisbenzotriazolyltetramethylbutylphenol (Tinosorb M), bisethylhexyloxyphenol methoxyphenyltriazine (Tinosorb S), ethylhexylmethoxycinnamate (OMC), isoamyl -p-methoxycinnamate (IMC), ethylhexylsalicylate (OS) and ethylhexyltriazone (OT)]

2-Chromatogram of standard solution and blank test solution of Example 2

Figure 3-calibration curve for the concentration and signal strength (peak area) of isoamyl-p-methoxycinnamate (IMC)

4-Chromatogram of sunscreen components (IMC, OMC, OS and TS) in the lotion of Example 3

5-Chromatogram of sunscreen ingredients (IMC, OMC, TM and TS) in the cream of Example 3

Figure 6-Chromatogram of sunscreen components (IMC and OMC) in the foundation of Example 3

7-Chromatogram of sunscreen ingredients (OMC) in makeup base of Example 3

8-Chromatogram of sunscreen ingredients (OMC) in powder of Example 3

Figure 9-Chromatogram of sunscreen components (OMC and TS) in the twin facts of Example 3

Figure 10- Chromatogram of sunscreen ingredients (OMC and IMC) at sunbeam of Example 3

11-Chromatogram of sunscreen ingredients (IMC) in lipstick of Example 3

Claims (4)

1) extracting a lipophilic and hydrophilic sunscreen component by adding a mixed solvent of dimethylformamide and methanol in a volume ratio of 1: 0.9 to 1.2 to the cosmetic containing a lipophilic and hydrophilic sunscreen component; 2) injecting the lipophilic and hydrophilic sunscreen components extracted in step 1) into a reversed phase nonpolar column filled with octadecylsilane (C18), dodecylsilane (C12) or octasilane (C8) having a nonpolarity as a stationary phase; ; And 3) separating the hydrophilic UV blocking component by liquid chromatography using a mixed solvent of water and ethanol as a mobile phase, and qualitatively and quantitatively analyzing the lipophilic UV blocking component using ethanol as a mobile phase; Simultaneous analysis of the sunscreen component comprising a. The method of claim 1, The lipophilic sunscreen component is Methylene Bis-Benzotriazolyl Tetramethylbutylphenol or bisethylhexyloxyphenol Methoxyphenyl Triazine, and the hydrophilic sunscreen component is ethylhex UV protection characterized by Ethylhexyl Methoxycinnamate, Isoamyl p-Methoxycinnamate, Ethylhexyl Salicylate or Ethylhexyl Triazone Simultaneous analysis of components. The method of claim 1, The hydrophilic sunscreen component is separated using a solvent mixed with water and ethanol in a volume ratio of 1: 3 to 9 as the mobile phase, and the lipophilic sunscreen component is separated using ethanol as a mobile phase. Simultaneous analysis of. The method of claim 1, The cosmetic is a simultaneous analysis of the sunscreen ingredients, characterized in that selected from the group consisting of lotion, essence, foundation, powder, lipstick or twin facts.

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