Method for rapidly and simultaneously detecting vitriol content and glycerol content in cosmetics

Abstract

The invention provides a method for rapidly and simultaneously detecting the content of glassine and glycerol in cosmetics. The method comprises the following steps: step 1, preparing a glycerol standard substance and a glassine standard substance into standard solutions with different concentrations; 2, injecting the standard solutions prepared in the step 1 into a high performance liquid chromatograph, measuring peak areas of the standard solutions with different concentrations, and drawing a standard curve to obtain a linear equation of the standard curve; step 3, pre-treating a sample, diluting the treated sample, preparing into a sample extraction liquid, filtering, injecting the filtered sample extraction liquid into a high performance liquid chromatograph, and measuring the peak area of a substance to be measured in the filtered sample extraction liquid; and 4, substituting the peak area of the substance to be detected in the filtered sample extract into the linear equation of the standard curve, and solving the corresponding concentration and content. The detection method can be used for rapidly detecting the content of glycerol and glassine in cosmetics, and has important practical significance and wide application prospects.

Description

Technical Field

[0001] The present invention relates to the technical field of cosmetic ingredients, and particularly relates to a method for rapidly and simultaneously detecting the contents of hydroxyprolisane and glycerol in cosmetics. Background Art

[0002] In today's cosmetic market, consumers have increasingly higher requirements for the quality and efficacy of products. The ingredient contents in cosmetics are directly related to the performance and safety of products. Among them, glycerol and hydroxyprolisane are two common and important ingredients.

[0003] Glycerol has good moisturizing properties and can absorb moisture in the air to keep the skin hydrated. It is widely used in various cosmetics such as lotions, creams, and toners. Accurately determining the content of glycerol in cosmetics is crucial for ensuring the moisturizing effect of products. However, currently, traditional detection methods are often complex in operation, time-consuming, and require professional equipment and technicians. This not only increases the detection cost but also is difficult to meet the need for rapid detection, which is not conducive to quality control during the production process and market supervision.

[0004] As a popular anti-wrinkle ingredient, hydroxyprolisane has the effects of promoting collagen synthesis and enhancing skin elasticity. With the increasing demand of consumers for anti-aging products, cosmetics containing hydroxyprolisane are becoming more and more popular. However, due to the relatively complex structure of hydroxyprolisane, accurate detection of its content also faces many challenges. Existing detection methods usually have problems such as low precision, cumbersome steps, and long analysis time, and cannot provide accurate content information for production enterprises and regulatory departments in a timely manner.

[0005] In addition, with the rapid development of the cosmetic industry, market competition is becoming increasingly fierce. Production enterprises need to rapidly and accurately detect the ingredient contents in cosmetics to ensure product quality, meet consumer needs, and at the same time improve production efficiency and market competitiveness. Regulatory departments also need efficient detection means to strengthen the supervision of the cosmetic market and protect the legitimate rights and interests of consumers.

[0006] In summary, there is currently a lack of a rapid, accurate, and simple method for detecting the contents of glycerol and hydroxyprolisane in cosmetics. Therefore, developing a technology for rapidly detecting the contents of glycerol and hydroxyprolisane in cosmetics has important practical significance and broad application prospects. Summary of the Invention

[0007] Object of the Invention:

[0008] The object of the present invention is to provide a method for rapidly and simultaneously detecting the contents of hydroxyprolisane and glycerol in cosmetics, and to solve the problem that the existing technology uses gas chromatography to determine the content of glycerol but cannot simultaneously determine the content of hydroxyprolisane.

[0009] Technical solution of the present invention:

[0010] A method for rapidly and simultaneously detecting the contents of hydroxyprolisilane and glycerin in cosmetics, comprising the following steps:

[0011] Step 1: Dissolve glycerin standard and hydroxyprolisilane standard in an extraction solution, and dilute and prepare standard solutions with different concentrations;

[0012] Step 2: Inject the standard solutions with different concentrations prepared in Step 1 into a high performance liquid chromatograph respectively. Under the same chromatographic conditions, measure the peak areas of the standard solutions with different concentrations, and use the concentration of the standard solution as the abscissa and the corresponding peak area as the ordinate to plot a standard curve and obtain its linear equation;

[0013] Step 3: Pretreat the sample, then dilute the treated sample with an extraction solution to prepare a sample extraction solution, filter it, inject the filtered sample extraction solution into a high performance liquid chromatograph, and perform under the chromatographic conditions of Step 2 to measure the peak area of the substance to be detected in the filtered sample extraction solution;

[0014] Step 4: Substitute the peak area of the substance to be detected in the filtered sample extraction solution into the linear equation of the standard curve plotted in Step 2 to obtain the corresponding concentration and content.

[0015] Further, the concentration of the standard solution in Step 1 is 100-500 mg / L.

[0016] Furthermore, the concentrations of the standard solutions are 100 mg / L, 200 mg / L, 300 mg / L, 400 mg / L, and 500 mg / L in sequence.

[0017] Further, the extraction solution is an aqueous acetonitrile solution of 30-70%.

[0018] Further, the chromatographic conditions in Step 2 include a chromatographic column, an injection volume, a column temperature, a mobile phase, and a mobile phase flow rate.

[0019] Furthermore, the chromatographic column used in the chromatographic conditions is an amino column, and the specifications of the amino column are 3.0×100 mm and the particle size is 3.5 μm.

[0020] Furthermore, the injection volume in the chromatographic conditions is 20-40 μL.

[0021] Furthermore, the mobile phase used in the chromatographic conditions is an aqueous acetonitrile solution of 85-95%.

[0022] Furthermore, the mobile phase flow rate in the chromatographic conditions is 0.5-1.5 mL / min.

[0023] Further, the column temperature in the chromatographic conditions is 30 - 40 °C.

[0024] Further, the sample pretreatment in step 3 includes the following steps:

[0025] S1: Weigh an appropriate amount of the sample into a medium-speed filter paper, fold and fix it, place the filter paper wrapped with the sample in a Soxhlet extraction tube, and connect the lower end of the Soxhlet extraction tube to a round-bottom flask;

[0026] S2: Add an extraction solution to the Soxhlet extraction tube in step S2. Connect a condenser reflux tube to the upper end of the Soxhlet extraction tube, turn on the condenser reflux, turn on the heating mantle, adjust the heating temperature to obtain a sample extraction solution, and repeatedly extract the sample extraction solution;

[0027] S3: After extracting in step S2 for 2 - 4 h, turn off the heating. Wait for the round-bottom flask to cool to room temperature, turn off the cooling water, remove the Soxhlet extraction device, transfer all the sample extraction solution in the round-bottom flask to a rotary evaporation flask, concentrate it to a certain volume, and the sample pretreatment is completed.

[0028] Further, the extraction solution added in step 2 is 50 - 100 times the mass of the sample.

[0029] Further, the heating temperature in step S2 is 50 - 70 °C.

[0030] Further, the extraction times in step S2 are 6 - 10 times / h.

[0031] Further, the extraction solution is a 50% acetonitrile aqueous solution; in the chromatographic conditions, the amino column has a specification of 3.0 × 100 mm, a particle size of 3.5 μm, the mobile phase is a 90% acetonitrile aqueous solution, the column temperature is 35 °C, the flow rate of the mobile phase is 1 mL / min, and the injection volume is 20 μL. Description of the Drawings

[0032] Figure 1 : Standard curve of glycerol-protinex;

[0033] Figure 2 : Liquid chromatogram of the sample in Example 1;

[0034] Figure 3 : Liquid chromatogram of the sample in Example 2.

[0035] Beneficial Effects:

[0036] 1. The HPLC-refractive index detection method can quickly and simultaneously and accurately quantify protinex and glycerol in cosmetics;

[0037] 2. The operation is simple, the calculation process is simple, the content can be directly calculated on the instrument through the standard curve, the calculation is simple, the error is small, the accuracy is high, the repeatability is strong, and the precision is high. Specific Embodiments

[0038] The present invention will be described below in conjunction with specific implementation embodiments. It should be noted that the following examples are examples of the present invention and are only used to illustrate the present invention, rather than to limit the present invention. Without departing from the gist or scope of the present invention, other combinations and various improvements within the concept of the present invention can be made.

[0039] Unless otherwise specified, the chemical reagents used in the present invention are all ordinary commercially available analytical pure. Example 1:

[0040] A method for detecting the content of hydroxyproline and glycerol in cosmetics, comprising the following steps:

[0041] Step 1: Weigh 10 g of glycerol standard and 10 g of hydroxyproline standard respectively, and dilute and prepare standard solutions with concentrations of 100 mg / L, 200 mg / L, 300 mg / L, 400 mg / L, and 500 mg / L using 50% acetonitrile aqueous solution;

[0042] Step 2: Under the conditions that the amino column has a specification of 3.0×100 mm, a particle size of 3.5 μm, the mobile phase is 90% acetonitrile aqueous solution, the column temperature is 35°C, and the flow rate of the mobile phase is 1 mL / min, inject 20 μL of the standard solutions with concentrations of 100 mg / L, 200 mg / L, 300 mg / L, 400 mg / L, and 500 mg / L prepared in Step 1 into the high-performance liquid chromatograph respectively, measure the peak areas of the standard solutions with different concentrations, and use the concentration of the standard solution as the abscissa and the corresponding peak area as the ordinate to plot a standard curve, and obtain its linear equation as Figure 1 , the standard curve of the glycerol standard is y = 67.423x - 4185.9, the correlation coefficient R2 = 0.996, and the standard curve of the hydroxyproline standard is y = 98.272x - 4058, the correlation coefficient R2 = 0.9988;

[0043] Step 3: Pretreat 2.5 g of Sample 1, then put the treated Sample 1 into a 50 ml volumetric flask, then add 50% acetonitrile aqueous solution to dilute and make up the volume, then filter the sample extract after volume making through a 0.45 μm microporous filter membrane, and take 20 μL of the filtered sample extract and inject it into the high-performance liquid chromatograph for testing under the same chromatographic conditions as in Step 2;

[0044] Step 4: According to as Figure 2For the chromatogram shown, substitute the peak areas of glycerol and hydroxyproline measured in the filtered sample extract into the linear equation of the standard curve plotted in Step 2 to obtain a glycerol concentration of 956.9 mg / L in the filtered sample extract, a glycerol content of 19.14% in Sample 1, a hydroxyproline concentration of 192.5 mg / L in the filtered sample extract, and a hydroxyproline content of 3.85% in Sample 1;

[0045] Pretreatment steps for Sample 1:

[0046] S1: Weigh 2.5 g of Sample 1 into a medium-speed filter paper, fold and fix it. Place the filter paper wrapped with Sample 1 in a Soxhlet extraction thimble, and connect the lower end of the Soxhlet extraction thimble to a 250 mL round-bottom flask;

[0047] S2: Add 150 mL of 50% acetonitrile aqueous solution to the Soxhlet extraction thimble in Step S2. Connect a condenser reflux tube to the upper end of the Soxhlet extraction thimble, turn on the condenser reflux, turn on the heating mantle, and adjust the heating temperature to 60 °C to obtain a sample extract. Extract the sample extract repeatedly 6 times / h;

[0048] S3: After Soxhlet extraction in Step S2 for 3 h, turn off the heating. Wait for the round-bottom flask to cool to room temperature, turn off the cooling water, remove the Soxhlet extraction device, transfer all the sample extract in the round-bottom flask to a rotary evaporation flask, and concentrate it to 40 mL. The pretreatment of Sample 1 is completed.

[0049] Example 2:

[0050] The difference from Example 1 is that: replace "2.5 g of Sample 1" in Step 3 with "2.5 g of Sample 2". Pretreatment steps for Sample 2:

[0051] S1: Weigh 2.5 g of Sample 2 into a medium-speed filter paper, fold and fix it. Place the filter paper wrapped with Sample 2 in a Soxhlet extraction thimble, and connect the lower end of the Soxhlet extraction thimble to a 250 mL round-bottom flask;

[0052] S2: Add 150 mL of 50% acetonitrile aqueous solution to the Soxhlet extraction thimble in Step S2. Connect a condenser reflux tube to the upper end of the Soxhlet extraction thimble, turn on the condenser reflux, turn on the heating mantle, and adjust the heating temperature to 60 °C to obtain a sample extract. Extract the sample extract repeatedly 10 times / h;

[0053] S3: After Soxhlet extraction in Step S2 for 2 h, turn off the heating. Wait for the round-bottom flask to cool to room temperature, turn off the cooling water, remove the Soxhlet extraction device, transfer all the sample extract in the round-bottom flask to a rotary evaporation flask, and concentrate it to 40 mL. The pretreatment of Sample 2 is completed;

[0054] In Step 4, "According to Figure 2Modify the following: "According to the chromatogram shown, substitute the peak areas of glycerol and hydroxyproline measured in the filtered sample extract into the linear equation of the standard curve plotted in step 2, and the concentration of glycerol in the filtered sample extract is found to be 956.9 mg / L, the content of glycerol in sample 1 is 19.14%, the concentration of hydroxyproline in the filtered sample extract is 192.5 mg / L, and the content of hydroxyproline in sample 1 is 3.85%" to "According to the chromatogram as shown in Figure 3 substitute the peak areas of glycerol and hydroxyproline measured in the filtered sample extract into the linear equation of the standard curve plotted in step 2, and the concentration of glycerol in the filtered sample extract is found to be 695.7 mg / L, the content of glycerol in sample 2 is 13.90%, the concentration of hydroxyproline in the filtered sample extract is 119.3 mg / L, and the content of hydroxyproline in sample 2 is 2.39%."

[0055] Conduct a methodological investigation on the method for rapidly and simultaneously detecting the contents of hydroxyproline and glycerol in cosmetics provided by the present invention:

[0056] 1. Repeatability investigation: Measure sample 1 multiple times using the detection method provided in Example 1, and the calculation results are shown in Table 1:

[0057] Table 1:

[0058] Number of tests 1 2 3 4 5 RSD Glycerol content (%) 19.14 19.15 19.14 19.14 19.16 0.047％ Pro-Xylane content (%) 3.86 3.85 3.85 3.84 3.84 0.220％

[0059] As can be seen from Table 1, the relative standard deviation RSD of the detection method provided in Example 1 is less than 2%, indicating that the experimental results can accurately reflect the true situation of the sample, and the method has good feasibility and reproducibility.

[0060] 2. Precision investigation: Use the detection method provided in Example 1 for sample 1, conduct 5 repeated tests using different instruments, with an injection volume of 20 μL each time, and measure the peak areas of each time. The results are shown in Table 2:

[0061] Table 2:

[0062]

[0063]

[0064] As can be seen from Table 2, the relative standard deviation RSD of the detection method provided in Example 1 is less than 2%, indicating that the experimental results can accurately reflect the true situation of the sample, and the method has good precision.

[0065] From the above data, it can be seen that a method for rapidly and simultaneously detecting the contents of hydroxyproline and glycerol in cosmetics according to the present invention can accurately quantify hydroxyproline and glycerol in cosmetics rapidly and simultaneously. The operation is simple and the calculation process is simple. The content of the sample can be directly read on the instrument through the standard curve without going through a large number of cumbersome calculation processes, reducing errors and improving accuracy.

[0066] The present invention can also have various other embodiments. Without departing from the spirit and essence of the present invention, those skilled in the art can make various corresponding changes and deformations according to the present invention, but these corresponding changes and deformations should all fall within the protection scope of the appended claims of the present invention.

Claims

1. A method for rapidly and simultaneously detecting the content of hydroxybenzoic acid and glycerol in cosmetics, characterized in that: The following steps are involved: Step 1: Dissolve the glycerol standard and the bosacene standard in the extract and dilute to prepare standard solutions of different concentrations; Step 2: inject the standard solutions of different concentrations prepared in step 1 into a high performance liquid chromatograph respectively, measure the peak areas of the standard solutions of different concentrations under the same chromatographic conditions, and draw a standard curve with the concentration of the standard solution as the abscissa and the corresponding peak area as the ordinate to obtain its linear equation; Step 3: pre-treat the sample, then dilute the treated sample with an extract to prepare a sample extract, filter, inject the filtered sample extract into a high performance liquid chromatograph, perform chromatography under the conditions of step 2, and measure the peak area of ​​the substance to be tested in the filtered sample extract; Step 4: Substitute the peak area of ​​the substance to be tested in the filtered sample extract into the linear equation of the standard curve drawn in step 2 to calculate the corresponding concentration and content.

2. The method for rapidly and simultaneously detecting the content of hydroxybenzoic acid and glycerin in cosmetics according to claim 1, characterized in that: The concentration of the standard solution in step 1 is 100-500 mg / L.

3. The method for rapid and simultaneous detection of hydroxybenzoic acid and glycerol content in cosmetics according to claim 1, characterized in that: The extract is a 30-70% acetonitrile aqueous solution.

4. The method for rapid and simultaneous detection of hydroxybenzoic acid and glycerol content in cosmetics according to claim 1, characterized in that: The chromatographic conditions of step 2 include chromatographic column, injection volume, column temperature, mobile phase, and mobile phase flow rate.

5. The method for rapid and simultaneous detection of hydroxybenzoic acid and glycerol content in cosmetics according to claim 4, characterized in that: The chromatographic column used in the chromatographic conditions is an amino column, the specification of the amino column is 3.0×100 mm, and the particle size is 3.5 μm; The injection volume in the chromatographic conditions is 20-40 μL; The mobile phase used in the chromatographic conditions is 85-95% acetonitrile aqueous solution; The mobile phase flow rate in the chromatographic conditions is 0.5-1.5 mL / min; The column temperature in the chromatographic conditions is 30-40°C.

6. The method for rapid and simultaneous detection of hydroxybenzoic acid and glycerol content in cosmetics according to claim 1, characterized in that: The sample pretreatment in step 3 comprises the following steps: S1: Weigh an appropriate amount of sample into medium-speed filter paper, fold and fix it, place the filter paper containing the sample into a pull-through tube, and connect the lower end of the pull-through tube to a round-bottom flask; S2: Add the extracting liquid to the extraction tube in step S2, connect the upper end of the extraction tube to the condensation reflux tube, turn on the condensation reflux, turn on the heating jacket, adjust the heating temperature, obtain the sample extract, and repeatedly extract the sample extract; S3: After 2-4 hours of extraction in step S2, turn off the heating, wait for the round-bottom flask to cool to room temperature, turn off the condensing water, remove the extraction device, transfer all the sample extract in the round-bottom flask to the rotary evaporator, and concentrate it to a certain volume. The sample pretreatment is completed.

7. The method for rapid and simultaneous detection of hydroxybenzoic acid and glycerol content in cosmetics according to claim 6, characterized in that: The extract added in step 2 is 50-100 times the mass of the sample.

8. The method for rapid and simultaneous detection of hydroxybenzoic acid and glycerol content in cosmetics according to claim 6, characterized in that: The heating temperature in step S2 is 50-70°C.

9. The method for rapid and simultaneous detection of hydroxybenzoic acid and glycerol content in cosmetics according to claim 6, characterized in that: The extraction frequency in step S2 is 6-10 times / h.

10. The method for rapid and simultaneous detection of hydroxybenzoic acid and glycerol content in cosmetics according to claim 1, characterized in that: The extract is a 50% acetonitrile aqueous solution; the chromatographic conditions use an amino column with a specification of 3.0×100 mm, a particle size of 3.5 μm, a mobile phase of 90% acetonitrile aqueous solution, a column temperature of 35° C., a mobile phase flow rate of 1 mL / min, and an injection volume of 20 μL.

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