Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed by the China National Light Industry Council.
This standard is under the jurisdiction of National Technical Committee on Fragrance and Flavor Cosmetic of Standardization Administration of China (SAC/TC 257).
Introduction
The substances tested in this standard are forbidden substances specified in the Safety and technical standards for cosmetics (Edition 2015).
Forbidden substances refer to those which cannot be added in cosmetics as raw materials or components during cosmetics production. According to the Safety and technical standards for cosmetics (Edition 2015): if it is technically impossible to avoid the adulteration of forbidden substances as impurities in cosmetics, safety risk assessment shall be conducted to ensure that such substances do not cause harm to human health under normal, reasonable and foreseeable service conditions.
At present, the limits of these substances are not specified in China. The preparation of this standard only provides detection methods for determining these substances in cosmetics.
Determination of 10 forbidden glycol ethers and esters in cosmetics - GC-MS
1 Scope
This standard specifies the reagents and materials, instruments and equipment, analysis steps, result calculation, recovery rate and precision, allowable deviation, etc. of the GC-MS determination method for 10 forbidden glycol ethers and esters in cosmetics, namely ethylene glycol dimethyl ether, 2-methoxyethanol, 2-methoxypropanol, 2-ethoxyethanol, 2-methoxypropyl acetate, 2-methoxyethyl acetate, 2-ethoxyethyl acetate, dimethoxy diglycol, 2-(2-methoxyethoxy) ethanol and triethylene glycol dimethyl ether.
This standard is applicable to the determination of 10 forbidden glycol ethers and esters in cosmetics.
See Table A.1 in Annex A for the limits of detection and quantitation of the method in this standard.
2 Principle
The sample is extracted with ethyl acetate-methanol mixed solvent by ultrasound, determined by gas chromatograph-mass spectrometer, and quantified by external standard method.
3 Reagents and materials
Unless otherwise specified, analytically-pure reagents shall be adopted.
3.1 Ethyl acetate: chromatographically pure.
3.2 Methanol: chromatographically pure.
3.3 Anhydrous sodium sulfate.
3.4 20% ethyl acetate methanol solution (V/V, volume ratio): measure 200mL ethyl acetate (3.1) and mix with 800mL methanol (3.2).
3.5 Standard samples/substances of 10 forbidden glycol ethers and esters: the purity shall not be less than 98%. See Table B.1 in Annex B for the Chinese names, English names, CAS numbers, molecular formulas, relative molecular masses and chemical structural formulas of ethylene glycol dimethyl ether, 2-methoxyethanol, 2-methoxypropanol, 2-ethoxyethanol, 2-methoxypropyl acetate, 2-methoxyethyl acetate, 2-ethoxyethyl acetate, dimethoxy diglycol, 2-(2-methoxyethoxy) ethanol and triethylene glycol dimethyl ether.
3.6 Standard stock solutions (2,000mg/L respectively): accurately weigh 20mg (accurate to 0.1mg) various standard products (3.5), place them in 10mL brown volumetric flasks respectively, dissolve to the scale with methanol (3.2), and shake well.
3.7 Mixed standard stock solution (100mg/L): accurately pipette 0.5mL each of the standard stock solutions (3.6) respectively, put them into a 10mL brown volumetric flask respectively, dilute to the scale with methanol (3.2), and shake well.
3.8 Mixed standard working solution: accurately pipette an appropriate amount of mixed standard stock solution (3.7) and dilute it step by step with 20% ethyl acetate methanol solution (3.4) to a series of mixed standard working solutions of 0.1mg/L~10.0mg/L for later use.
4 Instruments and equipment
4.1 Gas chromatograph-mass spectrometer (GC-MS): equipped with electron impact ionization source (EI source).
4.2 Vortex oscillator.
4.3 Ultrasonic cleaner.
4.4 Centrifuge: with rotation speed not lower than 10,000r/min.
4.5 Analytical balance: with a sensitivity of 0.1mg.
5 Analysis steps
5.1 Sample treatment
Accurately weigh 0.5g non-wax-based specimen (accurate to 0.001g) into a 15mL plastic centrifuge tube with plug, add 2mL ethyl acetate (3.1), add 7mL methanol (3.2) after vortex dispersion, mix well, perform ultrasonic extraction for 15min, cool to room temperature, and dilute to 10mL with methanol (3.2). Take 3mL supernatant into a centrifuge tube, add 1g anhydrous sodium sulfate (3.3), perform vortex dispersion, centrifuge the supernatant at 10,000r/min for 2min, and measure after filtering with a 0.22μm filter membrane.
The sampling mass of wax-based specimens is 0.25g, and other steps are the same as those of non-wax-based samples.
5.2 Determination
As the test result depends on the instrument used, it is impossible to provide the general parameters of gas chromatograph-mass spectrometer. The set parameters shall ensure the effective separation between the tested component and other components during chromatographic determination; the reference conditions for gas chromatography-mass spectrometry are as follows:
Foreword i
Introduction ii
1 Scope
2 Principle
3 Reagents and materials
4 Instruments and equipment
5 Analysis steps
6 Result calculation
7 Recovery rate and precision
8 Allowable deviation
Annex A (Informative) Limits of detection and quantitation for this method
Annex B (Informative) Chinese names, English names, CAS numbers, molecular formulas, relative molecular masses and chemical structural formulas of 10 forbidden glycol ethers and esters
Annex C (Informative) Quantitative and qualitative selective ion parameters of 10 forbidden glycol ethers and esters
Annex D (Informative) GC-MS selective ion chromatograms of standard substances of 10 forbidden glycol ethers and esters
Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed by the China National Light Industry Council.
This standard is under the jurisdiction of National Technical Committee on Fragrance and Flavor Cosmetic of Standardization Administration of China (SAC/TC 257).
Introduction
The substances tested in this standard are forbidden substances specified in the Safety and technical standards for cosmetics (Edition 2015).
Forbidden substances refer to those which cannot be added in cosmetics as raw materials or components during cosmetics production. According to the Safety and technical standards for cosmetics (Edition 2015): if it is technically impossible to avoid the adulteration of forbidden substances as impurities in cosmetics, safety risk assessment shall be conducted to ensure that such substances do not cause harm to human health under normal, reasonable and foreseeable service conditions.
At present, the limits of these substances are not specified in China. The preparation of this standard only provides detection methods for determining these substances in cosmetics.
Determination of 10 forbidden glycol ethers and esters in cosmetics - GC-MS
1 Scope
This standard specifies the reagents and materials, instruments and equipment, analysis steps, result calculation, recovery rate and precision, allowable deviation, etc. of the GC-MS determination method for 10 forbidden glycol ethers and esters in cosmetics, namely ethylene glycol dimethyl ether, 2-methoxyethanol, 2-methoxypropanol, 2-ethoxyethanol, 2-methoxypropyl acetate, 2-methoxyethyl acetate, 2-ethoxyethyl acetate, dimethoxy diglycol, 2-(2-methoxyethoxy) ethanol and triethylene glycol dimethyl ether.
This standard is applicable to the determination of 10 forbidden glycol ethers and esters in cosmetics.
See Table A.1 in Annex A for the limits of detection and quantitation of the method in this standard.
2 Principle
The sample is extracted with ethyl acetate-methanol mixed solvent by ultrasound, determined by gas chromatograph-mass spectrometer, and quantified by external standard method.
3 Reagents and materials
Unless otherwise specified, analytically-pure reagents shall be adopted.
3.1 Ethyl acetate: chromatographically pure.
3.2 Methanol: chromatographically pure.
3.3 Anhydrous sodium sulfate.
3.4 20% ethyl acetate methanol solution (V/V, volume ratio): measure 200mL ethyl acetate (3.1) and mix with 800mL methanol (3.2).
3.5 Standard samples/substances of 10 forbidden glycol ethers and esters: the purity shall not be less than 98%. See Table B.1 in Annex B for the Chinese names, English names, CAS numbers, molecular formulas, relative molecular masses and chemical structural formulas of ethylene glycol dimethyl ether, 2-methoxyethanol, 2-methoxypropanol, 2-ethoxyethanol, 2-methoxypropyl acetate, 2-methoxyethyl acetate, 2-ethoxyethyl acetate, dimethoxy diglycol, 2-(2-methoxyethoxy) ethanol and triethylene glycol dimethyl ether.
3.6 Standard stock solutions (2,000mg/L respectively): accurately weigh 20mg (accurate to 0.1mg) various standard products (3.5), place them in 10mL brown volumetric flasks respectively, dissolve to the scale with methanol (3.2), and shake well.
3.7 Mixed standard stock solution (100mg/L): accurately pipette 0.5mL each of the standard stock solutions (3.6) respectively, put them into a 10mL brown volumetric flask respectively, dilute to the scale with methanol (3.2), and shake well.
3.8 Mixed standard working solution: accurately pipette an appropriate amount of mixed standard stock solution (3.7) and dilute it step by step with 20% ethyl acetate methanol solution (3.4) to a series of mixed standard working solutions of 0.1mg/L~10.0mg/L for later use.
4 Instruments and equipment
4.1 Gas chromatograph-mass spectrometer (GC-MS): equipped with electron impact ionization source (EI source).
4.2 Vortex oscillator.
4.3 Ultrasonic cleaner.
4.4 Centrifuge: with rotation speed not lower than 10,000r/min.
4.5 Analytical balance: with a sensitivity of 0.1mg.
5 Analysis steps
5.1 Sample treatment
Accurately weigh 0.5g non-wax-based specimen (accurate to 0.001g) into a 15mL plastic centrifuge tube with plug, add 2mL ethyl acetate (3.1), add 7mL methanol (3.2) after vortex dispersion, mix well, perform ultrasonic extraction for 15min, cool to room temperature, and dilute to 10mL with methanol (3.2). Take 3mL supernatant into a centrifuge tube, add 1g anhydrous sodium sulfate (3.3), perform vortex dispersion, centrifuge the supernatant at 10,000r/min for 2min, and measure after filtering with a 0.22μm filter membrane.
The sampling mass of wax-based specimens is 0.25g, and other steps are the same as those of non-wax-based samples.
5.2 Determination
As the test result depends on the instrument used, it is impossible to provide the general parameters of gas chromatograph-mass spectrometer. The set parameters shall ensure the effective separation between the tested component and other components during chromatographic determination; the reference conditions for gas chromatography-mass spectrometry are as follows:
Contents of GB/T 35894-2018
Foreword i
Introduction ii
1 Scope
2 Principle
3 Reagents and materials
4 Instruments and equipment
5 Analysis steps
6 Result calculation
7 Recovery rate and precision
8 Allowable deviation
Annex A (Informative) Limits of detection and quantitation for this method
Annex B (Informative) Chinese names, English names, CAS numbers, molecular formulas, relative molecular masses and chemical structural formulas of 10 forbidden glycol ethers and esters
Annex C (Informative) Quantitative and qualitative selective ion parameters of 10 forbidden glycol ethers and esters
Annex D (Informative) GC-MS selective ion chromatograms of standard substances of 10 forbidden glycol ethers and esters
