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GB/T 37544-2019 English PDF

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GB/T 37544-2019: Determination of 6 kinds of phenolic antibacterial agent including o-cymen-5-ol in cosmetics - High performance liquid chromatography
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Standard similar to GB/T 37544-2019

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Basic data

Standard ID GB/T 37544-2019 (GB/T37544-2019)
Description (Translated English) Determination of 6 kinds of phenolic antibacterial agent including o-cymen-5-ol in cosmetics - High performance liquid chromatography
Sector / Industry National Standard (Recommended)
Classification of Chinese Standard Y42
Classification of International Standard 71.100.70
Word Count Estimation 10,114
Date of Issue 2019-06-04
Date of Implementation 2020-01-01
Issuing agency(ies) State Administration for Market Regulation, China National Standardization Administration

GB/T 37544-2019: Determination of 6 kinds of phenolic antibacterial agent including o-cymen-5-ol in cosmetics - High performance liquid chromatography


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Determination of 6 kinds of phenolic antibacterial agent including o-cymen-5-ol in cosmetics--High performance liquid chromatography ICS 71.100.70 Y42 National Standards of People's Republic of China 6 kinds of phenols such as o-cymene-5-ol in cosmetics Determination of antibacterial agents by high performance liquid chromatography Determinationof6kindsofphenolicantibacterialagent including 2019-06-04 release 2020-01-01 implementation State Administration of Market Supervision Published by China National Standardization Administration

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard was proposed by the China Light Industry Federation. This standard is under the jurisdiction of the National Technical Committee for Standardization of Flavors, Fragrances, and Cosmetics (SAC/TC257). This standard was drafted. Jiangsu Provincial Product Quality Supervision and Inspection Institute, Suzhou World Spectrum Testing Technology Co., Ltd., Infinite (China) Co., Ltd., Shanghai Daily Chemical Industry Research Institute, Guangzhou Huaxin Detection Technology Co., Ltd. (East) Commodity Co., Ltd., Guangzhou Institute of Quality Supervision and Inspection, Suzhou Institute of Quality Inspection and Scientific Research, Jiangsu Food and Drug Supervision, Inspection and Research Institute Academy. The main drafters of this standard. Zhang Xiaoqiang, Lu Jian, Huang Jinfeng, Sun Hongmei, Xun Zhiqing, Li Xiaomin, Dai Dan, Liao Huayong, Shen Min, Zhang Lihua, Dai Jieling, Zhang Zheng, Zou Jie, Yang Anwen, Yuan Liwen, Peng Yurui, Li Hai, Zhao Chunxiao, Wang Changjie, Kang Wei, Wu Zhongping, Yang Yang, Qu Mei, Sun Shanshan, Cao Qianwen, Ye Zhuhong, Shi Bing, Ye Jiarong, Wang Chenxia, Liu Xiangmei, Chen Yiguang, Wu Yanping, Hou Xiangyi, Wu Yuchen, Guo Xindong.

Introduction

The tested substances of this standard. phenol, 4-tert-butylphenol, 2,4,6-trichlorophenol and pentachlorophenol are China's "Cosmetic Safety Technical Specifications" (2015 edition). Prohibited substances are substances that cannot be added to cosmetics as raw materials for cosmetic production, that is, components. "Cosmetic Safety Technical Specification (2015 edition) '' stipulates. If it is technically impossible to prevent prohibited substances from being brought into cosmetics as impurities, a safety risk assessment should be performed to ensure that Under normal, reasonable and foreseeable conditions of use shall not cause harm to human health. At present, China has not stipulated the limit values of these substances. The formulation of this standard only provides detection methods for the determination of these substances in cosmetics. 6 kinds of phenols such as o-cymene-5-ol in cosmetics Determination of antibacterial agents by high performance liquid chromatography

1 Scope

This standard specifies phenol, p-chloro-m-cresol, o-cymene-5-ol, 4-tert-butylphenol, 2,4,6-trichlorophenol, and pentachlorobenzene in cosmetics. Principles, methods and reagents of high-performance liquid chromatography for the determination of 6 phenol antibacterial agents, reagents and materials, equipment, test procedures, calculation of results, recovery Rate and precision, tolerance, etc. This standard applies to phenol, p-chloro-cresol, o-cymene-5-ol, 4-tert-butylphenol, 2,4,6-trichlorophenol, and pentachlorobenzene in cosmetics. Determination of 6 phenol antibacterial agents. The detection limit and limit of quantitation of the methods of this standard. phenols in water preparations, emulsions, creams, powder cosmetics, p-chloro-m-cresol, o-cymene-5- The method detection limit of alcohol, 4-tert-butylphenol, 2,4,6-trichlorophenol and pentachlorophenol is 2.5mg/kg, and the method limit of quantification is 8.5mg/kg. The detection limits of phenol, p-chloro-cresol, o-cymene-5-ol, 4-tert-butylphenol, 2,4,6-trichlorophenol and pentachlorophenol in cosmetics are. 5.0mg/kg, the method limit of quantification was 17.0mg/kg.

2 Normative references

The following documents are essential for the application of this document. For dated references, only the dated version applies to this article Pieces. For undated references, the latest version (including all amendments) applies to this document. GB/T 6682 Analytical laboratory water specifications and test methods

3 Principle

The phenol, p-chloro-cresol, o-cymene-5-ol, 4-tert-butylphenol, 2,4,6-trichlorophenol, and pentachlorophenol in the sample were extracted by the solvent. After centrifugal filtration, it was determined by high-performance liquid chromatography equipped with a diode array detector. The retention time and spectrum were qualitatively determined by external standard method. Confirmed by HPLC-MS/MS.

4 Reagents and materials

4.1 Water. Grade I water specified in GB/T 6682. 4.2 Acetonitrile. chromatographically pure. 4.3 Formic acid. chromatographically pure. 4.4 Ammonium acetate. chromatographically pure. 4.5 Acetonitrile aqueous solution. Accurately measure 70mL of acetonitrile (4.2) and 30mL of water. 4.6 Standard material. purity is not less than 98%. Phenol, p-chloro-cresol, o-cymene-5-ol, 4-tert-butylphenol, 2,4,6-trichlorophenol, Chinese name, INCI name (International Cosmetic Raw Material Name), English name, CAS number, molecular formula, relative molecular weight and For the chemical structural formula, see Appendix A, Table A.1. 4.7 Mixed standard working solution. Weigh the appropriate amount of standard material (4.6) (accurate to 0.1mg) accurately, and prepare the mass with acetonitrile (4.2) Standard stock solution with a concentration of.2000 μg/mL (storage at 4 ° C, protected from light, can be stored for 6 months). Accurately pipette each standard stock solution 500.0 μL in a 10 mL volumetric flask, make up to volume with an acetonitrile aqueous solution (4.5), and mix to obtain a mixed standard stock solution (100.0 μg/mL, 4 ° C, protected from light). Accurately remove an appropriate amount of the standard stock solution, and dilute it gradually with an acetonitrile aqueous solution (4.5) to a mass concentration of 0.10 μg/mL, Series of 0.20 μg/mL, 0.50 μg/mL, 1.00 μg/mL, 2.50 μg/mL, 5.00 μg/mL, 10.0 μg/mL, and 50.0 μg/mL Mix standard working solution (now equipped with current use). 4.8 Microporous filter. organic filter with a pore size of 0.22μm.

5 Equipment

General laboratory equipment, and the following instruments. a) High performance liquid chromatography (HPLC) instrument. equipped with a diode array detector; b) HPLC-triple quadrupole mass spectrometer; c) Analytical balance. Sensitivity 0.001g and 0.0001g; d) vortex oscillator; e) Ultrasonic cleaning instrument. ultrasonic power 250W; f) Centrifuge. The maximum speed is not less than 4000r/min.

6 Test steps

6.1 Sample processing 6.1.1 Liquid, emulsion, cream, powder cosmetics Weigh 0.2g of the sample (accurate to 0.001g) into a 15mL stoppered plastic centrifuge tube, add acetonitrile aqueous solution (4.5) to 5.0mL, and vortex Shake for 2min, sonicate for 10min, centrifuge at 4000r/min for 5min, and take the supernatant through a 0.22μm filter membrane to be determined. 6.1.2 Wax-based cosmetics Weigh 0.1g of the sample (accurate to 0.001g) into a 15mL stoppered plastic centrifuge tube, add 0.5mL tetrahydrofuran, and vortex until Dissolve all, then add acetonitrile aqueous solution (4.5) to 5.0mL, vortex for 2min, sonicate for 10min, centrifuge at 4000r/min for 5min, Take the supernatant through a 0.22 μm filter and wait for the determination. 6.2 Measurement conditions The HPLC reference conditions are as follows. a) Chromatographic column. Column for PAHs, 5μm, 250mm × 4.6mm (inner diameter), or equivalent; b) Mobile phase. acetonitrile-10mmol/L ammonium acetate aqueous solution [adjusted to pH 5.0 with formic acid (4.3)], see Table 1 for gradient elution procedure; c) Flow rate. 1.2mL/min; d) Column temperature. 30 ℃; e) Detection wavelength. 280nm; f) Injection volume. 20 μL. Table 1 Gradient elution procedure Time/min 10mmol/L ammonium acetate aqueous solution (pH5.0) /% acetonitrile /% 0.0 80 20 7.0 70 30 10.0 65 35 20.0 65 35 23.0 10 90 Table 1 (continued) Time/min 10mmol/L ammonium acetate aqueous solution (pH5.0) /% acetonitrile /% 30.0 10 90 31.0 80 20 39.0 80 20 6.3 Standard working curve drawing Measure the serial mixed standard working solution (4.7) according to the measurement conditions (6.2), and take the peak area of the chromatographic peak as the ordinate, and the corresponding solvent The liquid concentration is plotted on the abscissa and a standard working curve is drawn. The HPLC chromatograms of the six reference materials are shown in Appendix B, Figure B.1. 6.4 Sample determination Measure the sample solution according to the measurement conditions (6.2). The test substance in the sample solution is qualitatively determined based on the retention time and the spectrum. By sample The peak area of the solution, the corresponding analyte concentration was found from the standard curve. The response value of the test object in the sample solution should be determined by the instrument. Within the linear range, the sample solution beyond the linear range needs to be diluted with acetonitrile aqueous solution (4.5) before determination. If necessary, use HPLC Spectrum-mass spectrometry/mass spectrometry for confirmation experiments, see Appendix C. 6.5 Blank test Except that no sample is added, the measurement is performed according to 6.1 ~ 6.2.

7 Results calculation

Calculate the content of the test substance in the sample according to formula (1). w = (ρ-ρ0) × V × 1000 m × 1000 (1) Where. w --- the content of each test substance in the sample, the unit is milligram per kilogram (mg/kg); ρ --- mass concentration corresponding to the peak area of each analyte in the sample solution, the unit is micrograms per milliliter (μg/mL) ρ0 --- the mass concentration of each test substance in the blank test, the unit is micrograms per milliliter (μg/mL); V --- constant volume, unit is milliliter (mL); m --- sample mass in grams (g). The calculation result is accurate to one digit after the decimal point.

8 Recovery and precision

In liquid preparations, emulsions, creams, powder cosmetics, phenol, p-chloro-cresol, o-cymene-5-ol, 4-tert-butylphenol, 2,4,6-tris Chlorophenol and pentachlorophenol are in the range of 8.5mg/kg ~ 85.0mg/kg, and the recovery rate is between 80% ~ 110%. The quasi deviation is less than 10%; Among wax-based cosmetics, phenol, p-chloro-cresol, o-cymene-5-ol, 4-tert-butylphenol, 2,4,6-trichlorophenol, and pentachlorophenol are being added. When the concentration is 17.0mg/kg ~ 170.0mg/kg, the recovery rate is between 80% ~ 110%, and the relative standard deviation is less than 10%.

9 tolerance

The absolute difference between the two independent determination results obtained under repeatable conditions shall not exceed 10% of the arithmetic mean.

Appendix A

(Informative appendix) Information on 6 phenolic antimicrobial reference materials Chinese name, INCI name, English name, CAS number, molecular formula, relative molecular mass and chemical structural formula of 6 phenolic antibacterial agents See Table A.1. Table A.1 Chinese name, INCI name/English name, CAS number, molecular formula, Relative molecular mass and chemical structural formula Chinese name INCI name English name CAS number Molecular formula Relative molecular mass Chemical structural formula Phenol 108-95-2 C6H5OH 94.1 P-chlorom-cresol p -chloro-m- cresol 4-chloro- m-cresol 59-50-7 C7H7ClO 142.6 O-cymen-5-ol 4-isopropyl- m-cresol 3228-02-2 C10H14O 150.2 4-tert-butylphenol- 4-tert- butylphenol 98-54-4 C10H14O 150.2 2,4,6-trichlorophenol- 2,4,6-trichlor ophenol 88-06-2 C6H3Cl3O 197.5 Pentachlorophenol-p entachlorop henol 87-86-5 C6HCl5O 266.3

Appendix B

(Informative appendix) High performance liquid chromatography of phenol, p-chloro-m-cresol, o-cymene-5-ol, 4-tert-butylphenol, 2,4,6-trichlorophenol, pentachlorophenol The high performance liquid chromatograms of the six phenolic antibacterial agents are shown in Figure B.1. Explanation. 1 --- phenol; 2--p-chloro-m-cresol; 3--o-cymene-5-ol; 4 --- 4-tert-butylphenol; 5--2,4,6-trichlorophenol; 6 --- Pentachlorophenol. Figure B.1 HPLC chromatograms of six phenolic antibacterial agents

Appendix C

(Informative appendix) Confirmatory test C.1 Reference conditions for liquid chromatography The reference conditions for liquid chromatography are as follows. a) Chromatographic column. C18 column, 1.7 μm, 150 mm × 2.1 mm (inner diameter); b) Mobile phase. 5mmol ammonium acetate aqueous solution acetonitrile = 60 40 (volume ratio); c) Flow rate. 0.3mL/min; d) Column temperature. 30 ℃; e) Injection volume. 5 μL. C.2 Reference conditions for mass spectrometry The mass spectrometry conditions are as follows. a) Ion source. Electrospray ion source (ESI); b) scanning method. negative ion scanning; c) Electrospray voltage. -4500V; d) Ion source temperature. 500 ° C; e) Air curtain gas. nitrogen, 0.207MPa; f) collision gas. nitrogen, 0.055MPa; g) Detection method. Multiple reaction monitoring (MRM). See Table C.1 for retention time, quantitative ion pairing, qualitative ion pairing, declustering voltage, and collision voltage of the six phenolic antibacterial agents. The extracted ion chromatogram of the antibacterial standard solution is shown in Figure C.1. Table C.1. Optimization parameters of the mass spectrometry MRM mode of six phenolic antibacterial agents Target retention time/min Quantitative ion pair (m/z) Qualitative ion pairs (m/z) De-clustering voltage/V Impact voltage/V Phenol 2.37 93.0/65.0 93.0/93.0 -75.0 -5.0, -24.0 P-chlorom-cresol 5.10 141.0/105.0 141.0/114.0 -75.0 -50.0, -21.0 O-cymene-5-ol 8.20 149.1/133.0 149.1/117.0 -75.0 -63.0, -21.0 4-tert-butylphenol 8.59 149.1/133.0 149.1/117.0 -75.0 -63.0, -21.0 2,4,6-trichlorophenol 4.56 196.9/161.0 196.9/123.0 -75.0 -39.0, -30.0 Pentachlorophenol 3.69 265.8/265.8 263.6/263.6 -75.0 -5.0, -5.0 Figure C.1 Extracted ion chromatograms of six phenolic antibacterial agents C.3 Qualitative determination When performing sample measurement, dilute the sample appropriately, and determine the sample solution and standard working solution according to liquid chromatography-mass spectrometry/mass spectrometry conditions. The retention time of the chromatographic peak is consistent with that of the standard material, and the selected ion appears in the spectrum of the sample after subtracting the background, and And the relative abundance of the selected ion is compared with that of the reference material, and the relative deviation does not exceed the range specified in Table C.2, then the existence of the Among these phenolic antibacterials. Table C.2 Allowable deviation of relative ion abundance during qualitative confirmation Relative ion abundance /% > 50 > 20 ~ 50 > 10 ~ 20 ≤10 Allowable relative deviation /% ± 20 ± 25 ± 30 ± 50

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