Method for detecting acid yellow 73 and solvent orange 16 in makeup cosmetics

Abstract

The invention discloses a method for detecting acid yellow 73 and solvent orange 16 in makeup cosmetics, which comprises the following steps: step 1, adding a drying agent and a dispersing agent into a sample to be detected to obtain a sample mixture, transferring the sample mixture into a solid-phase extraction hollow tube with a sieve plate and C18 powder, and performing solid-phase extraction on the solid-phase extraction hollow tube; placing another sieve plate above the sample mixture, pressing the sieve plate, adding an eluent and an extraction agent into a solid-phase extraction hollow pipe for elution to obtain an eluent, carrying out centrifugal treatment on the eluent, taking lower-layer liquid, blow-drying the lower-layer liquid with nitrogen, dissolving the lower-layer liquid with a constant-volume solvent, and filtering the lower-layer liquid with a filter membrane to obtain a to-be-detected extracting solution; and 2, simultaneously determining the contents of the acid yellow 73 and the solvent orange 16 in the to-be-detected extracting solution by using a high performance liquid chromatography-diode array detector. The method has the advantages of high specificity, low organic solvent consumption, easiness in popularization and application and the like.

Description

Technical Field

[0001] The invention relates to a method for detecting acid yellow 73 and solvent orange 16 in color cosmetics. Background Art

[0002] With the popularization and rejuvenation of the cosmetics market and the opening up of the male cosmetics market, the user population is becoming more and more extensive. Colorants in cosmetics refer to substances that use the principle of absorbing or reflecting visible light to make cosmetics, the body or its parts appear colored. Their role in the product is mainly evaluated from the perspective of beauty color science and psychology. They are mainly used in cosmetic products, namely lipstick, rouge, eye shadow, mascara, nail polish, etc.

[0003] According to the source, colorants can be divided into two categories: natural and synthetic. Organic synthetic colorants are widely used in cosmetics such as lipstick, rouge, and nail polish due to their strong hiding power and coloring power. However, many synthetic colorants come from coal tar products and are azo compounds. They have certain safety risks, photosensitivity, reproductive developmental toxicity, and even a few may induce cancer. Therefore, the safety of colorant ingredients has been increasingly valued by consumers and regulatory authorities. All countries have conducted risk assessments and made corresponding regulations and restrictions, such as the European Parliament and the Council of the European Union Cosmetics Regulation (EC) 1223 / 2009 and Chapter 21 of the United States Code of Federal Regulations. Table 6 of China's "Technical Specifications for Safety of Cosmetics" (2015 Edition) lists 157 colorants that are allowed to be used, and clarifies their scope of use (various cosmetics, cosmetics other than eye cosmetics, cosmetics that are specifically used for non-contact with mucous membranes, and cosmetics that are specifically used for temporary contact with the skin), other restrictions and requirements, and labeling regulations. For example, for Acid Yellow 73, its limit in cosmetics is 6%, but it is prohibited in hair dye products, and the impurity resorcinol content contained in it shall not exceed 0.5%, the content of phthalic acid shall not exceed 1%, and the content of 2-(2,4-dihydroxybenzoyl)benzoic acid shall not exceed 0.5%; for another example, although Solvent Orange 16 can be used in various cosmetics, when used in lipstick, the colorant is only allowed to be in the free (acid) form, and the limit is 1%.

[0004] In view of the fact that some colorants are harmful to human health, improving the quality of color cosmetics is conducive to ensuring the safety of consumers and promoting the healthy development of the industry. In recent years, the research on the detection methods of colorants in cosmetics has received increasing attention, but the permitted colorants covered by the current standards only account for 1 / 3 of the "Technical Specifications for Cosmetic Safety", and there are still many gaps in the determination technology of colorants. The main detection methods are high performance liquid chromatography and liquid chromatography-mass spectrometry, while others such as micellar electrokinetic chromatography, thin layer chromatography, and ultraviolet spectrophotometry have been basically eliminated due to their high detection limits and poor specificity.

[0005] The current detection methods have disadvantages such as poor specificity, high consumption of organic solvents, and difficulty in popularization and application. Summary of the invention

[0006] The technical problem to be solved by the present invention is to overcome the above-mentioned defects of the prior art and provide a method for detecting Acid Yellow 73 and Solvent Orange 16 in color cosmetics.

[0007] The present invention solves the above technical problems through the following technical solutions:

[0008] A method for detecting acid yellow 73 and solvent orange 16 in color cosmetics, comprising the following steps:

[0009] Step 1: Add a desiccant and a dispersant to the sample to be tested, grind and mix to obtain a sample mixture, and transfer the sample mixture to a plate with a sieve plate and C 18 The powder is placed in an empty tube for solid phase extraction, and then another sieve plate is placed on the sample mixture and pressed tightly. Then, the eluent and the extractant are added to the empty tube for solid phase extraction for elution. The eluent is centrifuged, the lower layer of liquid is taken out and dried with nitrogen, and then dissolved with a constant volume solvent, and filtered through a filter membrane to obtain an extract to be tested;

[0010] Step 2: using high performance liquid chromatography-diode array detector to simultaneously determine the contents of acid yellow 73 and solvent orange 16 in the extract to be tested.

[0011] Furthermore, in step 1, the desiccant is anhydrous sodium sulfate; the dispersant is C 18 powder.

[0012] Furthermore, in step 1, both sieve plates are made of polypropylene.

[0013] Furthermore, in step 1, the eluent is 50% acetonitrile solution.

[0014] Furthermore, in step 1, the extractant is 1-butyl-3-methylimidazolium hexafluorophosphate.

[0015] Furthermore, in step 1, the step of centrifuging the eluate comprises: centrifuging at a speed of 5000 r / min for 5 minutes.

[0016] Furthermore, in step 1, the constant volume solvent is 30% acetonitrile-70% ammonium acetate.

[0017] Furthermore, in step 1, the filter membrane is a polytetrafluoroethylene filter membrane.

[0018] Furthermore, in step 2, a series of standard solutions of Acid Yellow 73 and Solvent Orange 16 with concentration gradients are first prepared, and the standard solutions are detected by high performance liquid chromatography-diode array detector, and a chromatographic peak area-concentration standard correspondence is established according to the detection results; the chromatographic peak areas of Acid Yellow 73 and Solvent Orange 16 in the extract to be detected are simultaneously determined by high performance liquid chromatography-diode array detector, and then the contents of Acid Yellow 73 and Solvent Orange 16 in the extract to be detected are obtained according to the chromatographic peak area-concentration standard correspondence.

[0019] Furthermore, in step 2, when using high performance liquid chromatography-diode array detector, the chromatographic conditions are:

[0020] C 18 Column, 4.6 mm × 250 mm, 5 μm;

[0021] The mobile phase was 30% acetonitrile-70% 0.05 mol / L ammonium acetate;

[0022] Flow rate 1.0mL / min, column temperature 40℃, injection volume 10μL

[0023] The detection wavelength of the diode array detector is 492 nm.

[0024] The beneficial effects of the present invention are as follows: the present invention adopts the pretreatment technology of ionic liquid-matrix dispersed solid phase extraction, and uses high performance liquid chromatography-diode array detector to simultaneously determine the colorants acid yellow 73 and solvent orange 16 in color cosmetics, and has the advantages of strong method specificity, low organic solvent consumption, and easy promotion and application. DETAILED DESCRIPTION

[0025] A preferred embodiment is given below to clearly and completely illustrate the present invention.

[0026] A method for detecting acid yellow 73 and solvent orange 16 in color cosmetics, comprising the following steps:

[0027] Step 1: Weigh 0.2 g of the cosmetic sample to be tested and place it in a mortar, then add 0.2 g of anhydrous sodium sulfate and 0.5 g of C which also serves as a dispersant. 18 The powder was ground and mixed evenly to obtain a sample mixture; the sample mixture was then transferred to a polypropylene frit plate with a pore size of 20 μm and 0.5 g C 18The powder was placed in an empty solid phase extraction tube, and then another polypropylene sieve plate with a pore size of 20 μm was placed above the sample mixture and pressed to exclude the air in the tube; then, 4 mL of 50% acetonitrile and 200 μL of 1-butyl-3-methylimidazolium hexafluorophosphate were mixed and added to the solid phase extraction tube for elution, and the flow rate was controlled below 1 mL / min to obtain an eluent, which was placed in a centrifuge tube; centrifuged at 5000 r / min for 5 min, the lower layer of liquid was taken out and dried with nitrogen, and then dissolved with 1.0 mL of 30% acetonitrile-70% 0.05 mol / L ammonium acetate, and filtered through a 0.22 μm polytetrafluoroethylene filter membrane to obtain an extract to be detected.

[0028] Step 2: using high performance liquid chromatography-diode array detector to simultaneously determine the contents of acid yellow 73 and solvent orange 16 in the extract to be tested.

[0029] In step 2, a series of standard solutions of Acid Yellow 73 and Solvent Orange 16 with concentration gradients are first prepared, and the standard solutions are detected by high performance liquid chromatography-diode array detector, and a chromatographic peak area-concentration standard correspondence relationship is established according to the detection results; the chromatographic peak areas of Acid Yellow 73 and Solvent Orange 16 in the extract to be detected are simultaneously determined by high performance liquid chromatography-diode array detector, and then the contents of Acid Yellow 73 and Solvent Orange 16 in the extract to be detected are obtained according to the chromatographic peak area-concentration standard correspondence relationship.

[0030] In step 2, when using high performance liquid chromatography-diode array detector, the chromatographic conditions are:

[0031] C 18 Column, 4.6 mm × 250 mm, 5 μm;

[0032] The mobile phase was 30% acetonitrile-70% 0.05 mol / L ammonium acetate;

[0033] The flow rate was 1.0 mL / min, the column temperature was 40 °C, the injection volume was 10 μL, and the detection wavelength was 492 nm.

[0034] Using this detection method, the concentrations of Acid Yellow 73 and Solvent Orange 16 in the range of 0.5 μg / mL-50 μg / mL showed a linear relationship with the chromatographic peak area (see Table 1).

[0035] Table 1 Linear data

[0036]

[0037] In Table 1, the R 2 The R of Solvent Orange 16 is 0.9996. 2 is 0.9998.

[0038] Using this detection method, the detection concentrations of Acid Yellow 73 and Solvent Orange 16 were determined to be 0.25 and 0.2 μg / mL, respectively, and the minimum quantitative concentrations were 1.0 and 0.8 μg / mL, respectively, based on the standard deviation of three and ten times the blank samples combined with the blank matrix sample spike. Based on the extraction of 0.2 g sample to 1.0 mL, the detection limits were 1.25 and 1.0 mg / kg, respectively, and the quantitative lower limits were set at 5.0 and 4.0 mg / kg, respectively.

[0039] Using this detection method, sample extracts with different Acid Yellow 73 and Solvent Orange 16 contents were continuously sampled and measured 6 times, and samples with different pigment contents were extracted and measured 6 times according to the determined determination method. The calculated relative standard deviations RSD were all less than 10%, indicating good precision and repeatability.

[0040] Using this detection method, the sample extracts with different Acid Yellow 73 and Solvent Orange 16 contents were measured at 0h, 1h, 3h, 6h, 12h, and 24h after sample preparation. The results showed that there was no significant difference in the values ​​and the stability was good within 24h. The sample extracts with different pigment contents were stored in a refrigerator at 4℃ after sample preparation and measured at 0d, 1d, 2d, 3d, 5d, and 7d. The results showed that there was no significant difference in the values ​​and the stability was good within 1 week.

[0041] The present invention adopts the pretreatment technology of ionic liquid-matrix dispersed solid phase extraction and uses high performance liquid chromatography-diode array detector to simultaneously determine the colorants acid yellow 73 and solvent orange 16 in color cosmetics. The method has the advantages of strong method specificity, low organic solvent consumption, and easy promotion and application.

[0042] Although the specific embodiments of the present invention are described above, it should be understood by those skilled in the art that this is only for illustration and the protection scope of the present invention is defined by the appended claims. Those skilled in the art may make various changes or modifications to these embodiments without departing from the principles and essence of the present invention, but these changes and modifications all fall within the protection scope of the present invention.

Claims

1. A method for detecting acid yellow 73 and solvent orange 16 in color cosmetics, characterized in that: It includes the following steps: Step 1: Add a desiccant and a dispersant to the sample to be tested, grind and mix to obtain a sample mixture, and transfer the sample mixture to a plate with a sieve plate and C 18 The powder is placed in an empty tube for solid phase extraction, and then another sieve plate is placed on the sample mixture and pressed tightly. Then, the eluent and the extractant are added to the empty tube for solid phase extraction for elution. The eluent is centrifuged, the lower layer of liquid is taken out and dried with nitrogen, and then dissolved with a constant volume solvent, and filtered through a filter membrane to obtain an extract to be tested; Step 2: using high performance liquid chromatography-diode array detector to simultaneously determine the contents of acid yellow 73 and solvent orange 16 in the extract to be tested.

2. The method for detecting Acid Yellow 73 and Solvent Orange 16 in color cosmetics according to claim 1, characterized in that: In step 1, the desiccant is anhydrous sodium sulfate; the dispersant is C 18 powder.

3. The method for detecting Acid Yellow 73 and Solvent Orange 16 in color cosmetics according to claim 1, characterized in that: In step 1, both sieve plates are made of polypropylene.

4. The method for detecting Acid Yellow 73 and Solvent Orange 16 in color cosmetics according to claim 1, characterized in that: In step 1, the eluent is 50% acetonitrile solution.

5. The method for detecting Acid Yellow 73 and Solvent Orange 16 in color cosmetics according to claim 1, characterized in that: In step 1, the extractant is 1-butyl-3-methylimidazolium hexafluorophosphate.

6. The method for detecting Acid Yellow 73 and Solvent Orange 16 in color cosmetics according to claim 1, characterized in that: In step 1, the step of centrifuging the eluate comprises: centrifuging at a speed of 5000 r / min for 5 minutes.

7. The method for detecting Acid Yellow 73 and Solvent Orange 16 in color cosmetics according to claim 1, characterized in that: In step 1, the constant volume solvent is a 30% acetonitrile-70% ammonium acetate mixed solution.

8. The method for detecting Acid Yellow 73 and Solvent Orange 16 in color cosmetics according to claim 1, characterized in that: In step 1, the filter membrane is a polytetrafluoroethylene filter membrane.

9. The method for detecting Acid Yellow 73 and Solvent Orange 16 in color cosmetics according to claim 1, characterized in that: In step 2, a series of standard solutions of Acid Yellow 73 and Solvent Orange 16 with concentration gradients are first prepared, and the standard solutions are detected by high performance liquid chromatography-diode array detector, and a chromatographic peak area-concentration standard correspondence relationship is established according to the detection results; the chromatographic peak areas of Acid Yellow 73 and Solvent Orange 16 in the extract to be detected are simultaneously determined by high performance liquid chromatography-diode array detector, and then the contents of Acid Yellow 73 and Solvent Orange 16 in the extract to be detected are obtained according to the chromatographic peak area-concentration standard correspondence relationship.

10. The method for detecting Acid Yellow 73 and Solvent Orange 16 in color cosmetics according to claim 1, characterized in that: In step 2, when using high performance liquid chromatography-diode array detector, the chromatographic conditions are: C 18 Column, 4.6 mm × 250 mm, 5 μm; The mobile phase was 30% acetonitrile-70% 0.05 mol / L ammonium acetate; Flow rate 1.0 mL / min, column temperature 40 °C, injection volume 10 μL; The detection wavelength of the diode array detector is 492 nm.

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