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GB/T 42425-2023: PDF in English (GBT 42425-2023)

GB/T 42425-2023 GB NATIONAL STANDARD OF THE PEOPLE'S REPUBLIC OF CHINA ICS 71.100.70 CCS Y 42 Determination of capryloyl salicylic acid, phenylethyl resorcinol, ferulic acid in cosmetics - High performance liquid chromatography ISSUED ON: MARCH 17, 2023 IMPLEMENTED ON: OCTOBER 1, 2023 Issued by: State Administration for Market Regulation; Standardization Administration of PRC. Table of Contents Foreword ... 3 1 Scope ... 4 2 Normative references ... 4 3 Terms and definitions ... 4 4 Principles ... 5 5 Reagents and materials ... 5 6 Instruments and equipment ... 5 7 Test steps ... 6 8 Result calculation ... 8 9 Recovery rate ... 8 10 Precision ... 8 Appendix A (Informative) Information on capryloyl salicylic acid, phenylethyl resorcinol, and ferulic acid standard substances ... 9 Appendix B (Informative) High-performance liquid chromatogram and DAD spectrogram of capryloyl salicylic acid, phenylethyl resorcinol and ferulic acid ... 10 Determination of capryloyl salicylic acid, phenylethyl resorcinol, ferulic acid in cosmetics - High performance liquid chromatography WARNING -- The personnel using this document shall have practical experience in formal laboratory work. This document does not indicate all possible safety issues. The user is responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated by relevant national regulations. 1 Scope This document describes the high-performance liquid chromatography method for the determination of capryloyl salicylic acid, phenylethyl resorcinol, and ferulic acid in cosmetics, including principles, reagents and materials, instruments and equipment, test steps, test data processing, recovery rate, precision, etc. This document is applicable to the determination of capryloyl salicylic acid, phenylethyl resorcinol, and ferulic acid in water, lotion, and cream cosmetics. In this document, the method detection limit and quantification limit of capryloyl salicylic acid, phenylethyl resorcinol, and ferulic acid are 3.3 mg/kg and 10 mg/kg, respectively. 2 Normative references The following documents contain the provisions which, through normative reference in this document, constitute the essential provisions of this document. For the dated referenced documents, only the versions with the indicated dates are applicable to this document; for the undated referenced documents, only the latest version (including all the amendments) is applicable to this document. GB/T 6682 Water for analytical laboratory use - Specification and test methods 3 Terms and definitions There are no terms and definitions that need to be defined in this document. 4 Principles The sample is vortex-oscillated with methanol solution, treated through ultrasonic extraction, centrifugal precipitation, separation and filtration, separated by reversed- phase high-performance liquid chromatography, detected by a diode array detector, and quantified by external standard method. 5 Reagents and materials Unless otherwise specified, only analytically pure reagents are used. 5.1 Water: Grade 1 specified in GB/T 6682. 5.2 Acetonitrile (chromatographically pure). 5.3 Methanol. 5.4 Capryloyl salicylic acid, phenylethyl resorcinol, and ferulic acid: The content is not less than 95%. See Table A.1 in Appendix A for the English name, INCI name (International Name of Cosmetic Ingredients), CAS number, molecular formula, relative molecular mass, and chemical structural formula. 5.5 Sea sand, chemically pure. 5.6 Sodium decanesulfonate. 5.7 Phosphoric acid. 5.8 Standard stock solution of capryloyl salicylic acid, phenylethyl resorcinol, and ferulic acid: Accurately weigh 25.0 mg of each of capryloyl salicylic acid, phenylethyl resorcinol, and ferulic acid (5.4) in a 25 mL volumetric flask, and dilute to the mark with methanol (5.3). A standard stock solution with a mass concentration of 1000 μg/mL is obtained; it is stored in a -18 °C refrigerator, and the validity period is 6 months. 5.9 Polytetrafluoroethylene (PTFE) filter membrane: The pore size is 0.22 μm. 6 Instruments and equipment 6.1 High-performance liquid chromatograph (diode array detector). 6.2 Analytical balance: The sense quantity is 0.1 mg and 0.001 g. 6.3 Volumetric flask: 10 mL, 25 mL, and 100 mL. 6.4 Graduated centrifuge test tube with a stopper: 10 mL. 6.5 Ultrasonic oscillator: The power is not less than 180 W. 6.6 Centrifuge: The rotation speed is not less than 10000 r/min. 6.7 Vortex oscillator. 6.8 Pipette or pipettor: 1 mL, 5 mL, and 10 mL. 7 Test steps 7.1 Sample treatment For water cosmetics, take 1 g of the sample (accurate to 0.001 g) into a graduated centrifuge tube with a stopper, add 7 mL of methanol (5.3), vortex-oscillate for 1 minute, extract with ultrasonic for 20 minutes, and cool to room temperature; make up the volume to 10 mL with methanol (5.3), centrifuge at 10000 r/min for 10 min, and filter the supernatant through a 0.22 μm filter membrane (5.9) for later testing. For facial masks (the mask liquid taken from facial masks), lotions, and cream cosmetics, take 1 g of the sample (accurate to 0.001 g) into a graduated centrifuge tube with a stopper, add methanol (5.3) to make up the volume to 10 mL, vortex-oscillate for 1 minute, and conduct ultrasonic extraction for 20 min; after cooling to room temperature, add 0.5 g~1.0 g of sea sand (5.5), vortex for 1 min, centrifuge at 10000 r/min for 10 min, and filter the supernatant through a 0.22 μm filter membrane (5.9) for later testing. Do two experiments in parallel. 7.2 Determination conditions The reference conditions for high-performance liquid chromatography determination are as follows: a) Chromatographic column specifications: C18 chromatographic column, 250 mm×4.6 mm (particle size of 5 μm); or, a chromatographic column with equivalent performance; b) Mobile phase: 5 mmol/L sodium decanesulfonate solution (containing 0.1% phosphoric acid) (A): acetonitrile (B), and the gradient elution procedure is shown in Table 1; c) Column temperature: 35 ℃; d) Mobile phase flow rate: 1.0 mL/min; ......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.

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