GB/T 39993-2021 English PDF

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GB/T 39993-2021: Determination of permitted preservatives dimethyl oxazolidine, 7-ethylbicyclooxazolidine and 5-bromo-5-nitro-1, 3-dioxane in cosmetics
Status: Valid

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GB/T 39993-2021	259	Add to Cart	3 days	Determination of permitted preservatives dimethyl oxazolidine, 7-ethylbicyclooxazolidine and 5-bromo-5-nitro-1, 3-dioxane in cosmetics	Valid

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Basic data

Standard ID: GB/T 39993-2021 (GB/T39993-2021)
Description (Translated English): Determination of permitted preservatives dimethyl oxazolidine, 7-ethylbicyclooxazolidine and 5-bromo-5-nitro-1, 3-dioxane in cosmetics
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: Y42
Word Count Estimation: 14,179
Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration

GB/T 39993-2021: Determination of permitted preservatives dimethyl oxazolidine, 7-ethylbicyclooxazolidine and 5-bromo-5-nitro-1, 3-dioxane in cosmetics

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Determination of permitted preservatives dimethyl oxazolidine, 7-ethylbicyclooxazolidine and 5-bromo-5-nitro-1, 3-dioxane in cosmetics ICS 71.100.70 Y42 National Standards of People's Republic of China The restricted preservatives used in cosmetics are dimethyl oxazolidine, 7-Ethylbicyclic oxazolidine and 5-bromo-5-nitro- Determination of 1,3-dioxane Released on 2021-04-30 2021-11-01 implementation State Administration of Market Supervision and Administration Issued by the National Standardization Management Committee

Foreword

This standard was drafted 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 the National Standardization Technical Committee for Fragrance, Flavor and Cosmetics (SAC/TC257). Drafting organizations of this standard. Suzhou Shipu Testing Technology Co., Ltd., Suzhou Institute of Quality Testing and Research, Jiangsu Longliqi Biotechnology Co., Ltd. Co., Ltd., Suzhou Luye Daily Necessities Co., Ltd., Guangdong Yalijie Fine Chemical Co., Ltd., Perfect (Guangdong) Daily Necessities Co., Ltd., Guangzhou State Quality Supervision and Inspection Institute, Shanghai Daily Chemical Industry Research Institute, Oushiman Biological Co., Ltd., Shanghai Xiangyi Herbal Cosmetics Co., Ltd., Shantou Linnaji Skin Care Co., Ltd., Jiawenli (Fujian) Cosmetics Co., Ltd., Infinitus (China) Co., Ltd., Guangzhou Guerlain Cosmetics Co., Ltd., Johnson & Johnson (China) Co., Ltd., Jiangsu Product Quality Supervision and Inspection Institute, Jiangsu Food and Drug Institute of Supervision and Inspection, Kunshan Drug Administration, Suzhou Inspection Branch of Jiangsu Drug Administration, Food Inspection Research of Hebei Province Institute, Suzhou Drug Inspection and Testing Research Center. The main drafters of this standard. Zhang Zheng, Huang Yufeng, Ma Juan, Liu Dong, Zhou Jianqing, Zhu Dandan, Ma Ming, Xun Zhiqing, Lu Zhi, Shen Min, Yang Qiongli, Chu Yeguo, Lin Jianping, Yang Mei, Zhang Lihua, Zhang Yan, Gu Jie, Lu Yingjie, Chen Wei, Kang Meifen, Chen Cong, Hou Aixia, Lu Xiaoyu, Chen Linlin, Yang Safety, Chen Yingyin, Li Shuqin, Zhang Yanhong, Wang Chenxia, Liu Xiangmei, Huang Jinfeng, Guo Xindong, Wu Guanjiao, Dai Dan, Ye Zhuhong, Liu Qunlin, Gao Hongying, Zhu Yirong, Lu Jian. The restricted preservatives used in cosmetics are dimethyl oxazolidine, 7-Ethylbicyclic oxazolidine and 5-bromo-5-nitro- Determination of 1,3-dioxane Warning---Personnel using this standard should have practical experience in formal laboratory work. This standard does not point out all possible safety issues question. The user is responsible for taking appropriate safety and health measures and ensuring compliance with the relevant state regulations.

1 Scope

This standard specifies the gas chromatography of dimethyl oxazolidine, 7-ethyl bicyclic oxazolidine and 5-bromo-5-nitro-1,3-dioxane in cosmetics. The principle of mass spectrometry and high performance liquid chromatography, reagents or materials, instruments and equipment, test procedures, calculation of results, recovery and precision, allowable Xu Cha and other content. This standard applies to dimethyl oxazolidine, 7-ethylbicyclic oxazolidine and 5-bromo-5-bromo-5-methyloxazolidine in water, oil-in-water and water-in-oil cosmetics. Determination of nitro-1,3-dioxane. Among them, the first method is applicable to 7-ethylbicyclooxazole in aqueous, oil-in-water and water-in-oil cosmetics Determination of alkane and 5-bromo-5-nitro-1,3-dioxane, and the determination of dimethyloxazolidine in water-in-oil cream cosmetics; the second method is applicable to Determination of dimethyloxazolidine in water, oil-in-water and water-in-oil cosmetics. The method detection limit and quantification limit of this standard. the method detection limit of the first method is 15.0mg/kg, and the quantification limit is 50.0mg/kg; The detection limit of the second method is 15.0mg/kg, and the limit of quantification is 50.0mg/kg.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document. GB/T 6682 Analytical laboratory water specifications and test methods 3 The first method of gas chromatography-mass spectrometry 3.1 Principle The analyte in the sample is extracted by tetrahydrofuran and determined by gas chromatography-mass spectrometry; the selected ion monitoring (SIM) mode is used for scanning Tracing, qualitatively based on retention time and abundance ratio of characteristic ions, and quantified by external standard method. 3.2 Reagents or materials 3.2.1 Tetrahydrofuran. analytically pure. 3.2.2 Acetone. chromatographically pure. 3.2.3 Anhydrous sodium sulfate. analytically pure, burned at 650℃ for 4h, stored in a closed desiccator. 3.2.4 Standard material. English name and national standard of dimethyl oxazolidine, 7-ethyl bicyclic oxazolidine and 5-bromo-5-nitro-1,3-dioxane standard material International cosmetics raw material name (INCI name), Chemical Abstracts Registration Number (CAS number), molecular formula, relative molecular mass and chemical structural formula, see Table A.1 in Appendix A, the purity should not be less than 95%. 3.2.5 Mixed standard working solution. accurately weigh appropriate amounts of standard materials (3.2.4) (accurate to 0.0001g), and prepare them with acetone (3.2.2) A single-label standard stock solution with a mass concentration of 1000 mg/L (stored at 4°C and protected from light, preferably for 3 months). Take the corresponding blank sample, Process according to 3.4.1 to obtain a matrix solution. Accurately pipet an appropriate amount of each single-standard standard stock solution, and dilute it step by step with the matrix solution to a mass concentration Series of mixed standard working solutions with a degree of 2.50mg/L, 5.00mg/L, 10.0mg/L, 20.0mg/L, 50.0mg/L, 100mg/L (Should be equipped for immediate use). 3.2.6 Membrane. PTFE membrane with a pore size of 0.22μm. 3.3 Equipment 3.3.1 Gas chromatography-mass spectrometer. equipped with an electron impact source (EI). 3.3.2 Analytical balance. the division value is 0.001g and 0.0001g. 3.3.3 Ultrasonic cleaner. the maximum operating frequency is not less than 40kHz. 3.3.4 Vortex oscillator. the maximum speed is not less than 3000r/min. 3.3.5 Centrifuge. the maximum speed is not less than 4000r/min. 3.4 Test procedure 3.4.1 Sample processing Weigh 0.5g of sample (accurate to 0.001g) into a 50mL centrifuge tube with stopper, add 10.0mL tetrahydrofuran (3.2.1) accurately, add Add 0.5g of anhydrous sodium sulfate (3.2.3), vortex to mix, cover and extract ultrasonically for 10min, after cooling, centrifuge at 4000r/min for 3min, take the supernatant After the solution is passed through the 0.22μm filter membrane, sample solution A is obtained, which is to be determined. 3.4.2 Measurement conditions The reference working conditions of gas chromatography-mass spectrometry are as follows. a) Chromatographic column. 5% phenyl-95% methyl polysiloxane silica capillary column (30m×250μm×0.25μm), or equivalent Principal b) Inlet temperature. 220℃; c) Carrier gas. helium, constant flow mode, flow rate 1.0mL/min; d) Heating program. the initial temperature is 60℃, keep for 6min, raise the temperature to.200℃ at 10℃/min, and then raise it to 15℃/min 280℃, keep for 5min; e) Sampling method. split injection with a split ratio of 5.1; f) Injection volume. 1.0μL; g) Transmission line temperature. 280℃; h) Ionization method. electron impact ionization (EI); i) Ionization energy. 70eV; j) Ion source temperature. 230℃; k) Scan mode. Select ion scan, solvent delay 3min; l) See Table 1 for the retention time, characteristic selective ion and abundance ratio of the tested compound. Table 1 Retention time, characteristic selective ion and abundance ratio of the three compounds to be tested 3.4.3 Drawing standard working curve Measure the series of mixed standard working solutions (3.2.5) according to the measurement conditions (3.4.2), and use the peak surface of each analyte to quantify the ion chromatographic peak The product is the ordinate, the corresponding standard solution concentration is plotted on the abscissa, and the standard working curve is drawn. Refer to Figure B.1 in Appendix B for the gas chromatography-mass spectrometry total ion current diagrams of the three preservative reference materials. 3.4.4 Qualitative analysis Under the measurement conditions (3.4.2), the characteristic selective ion chromatographic peaks of sample solution A and standard working solution are at the same retention time. (±0.5%) appears, and the characteristic ion relative ion abundance of sample solution A is equivalent to the characteristic ion relative ion of the standard working solution. If the relative deviation of sub-abundance does not exceed the range specified in Table 2, it can be determined that there are related target compounds in the sample. Table 2 Relative ion abundance and maximum allowable deviation of characteristic ions during qualitative confirmation 3.4.5 Quantitative analysis This standard adopts external standard calibration curve method for quantitative determination. Take the peak area of the quantitative ion chromatographic peak of each analyte as the ordinate, and the corresponding standard The concentration of the quasi-solution is the abscissa, and the standard curve is drawn. The peak area of the quantitative ion chromatographic peak of the compound to be tested in the sample is compared with the standard curve More quantitative. The response value of the test compound in the sample solution A should be within the linear range of the standard curve, and the sample solution A beyond the linear range It can be measured after proper dilution. 3.4.6 Blank test Except that the sample is not weighed, the measurement is carried out according to 3.4.1~3.4.2. 3.5 Result calculation The content of the test compound in the sample is calculated according to formula (1). 3.6 Recovery rate and precision In the range of 50.0mg/kg~500mg/kg, the recovery rate is 80%~110%. Relative standard deviation is small Less than 10%. 3.7 Allowance The absolute difference between the two independent measurement results obtained under repeatability conditions is not more than 10% of the arithmetic mean of the two measurement values.

4 The second method high performance liquid chromatography

4.1 Principle The dimethyl oxazolidine in the sample is extracted by 50% (volume fraction) acetonitrile solution, and the extract is purified by n-hexane, centrifuged, and 9-fluorene methoxycarbonyl After the acid chloride is derivatized, it is determined by high performance liquid chromatography. Qualitative by retention time and spectrogram, and quantified by external standard method. 4.2 Reagents and materials Unless otherwise stated, all reagents used are of analytical grade. 4.2.1 Water, GB/T 6682, Class I. 4.2.2 Acetonitrile. chromatographically pure. 4.2.3 n-hexane. chromatographically pure. 4.2.4 Sodium tetraborate (Na2B4O7·10H2O). pure superior grade. 4.2.5 9-Fluorene methoxycarbonyl chloride (FMOC-Cl). the purity is not less than 99%. 4.2.6 50% (volume fraction) acetonitrile solution. accurately measure 50mL acetonitrile (4.2.2) and 50mL water, mix well and set aside. 4.2.7 Acetonitrile-saturated n-hexane. Measure 20 mL of acetonitrile (4.2.2) and 50 mL of n-hexane (4.2.3) to a 100 mL conical flask with stopper. In the middle, mix well and let stand. The upper layer is n-hexane saturated with acetonitrile. 4.2.8 Buffer solution. accurately weigh out 5.0g of sodium tetraborate (4.2.4), dissolve it in 90mL of water at 50℃, transfer it into a 100mL volumetric flask, and set it with water. To the mark. 4.2.9 9-Fluorenyl methoxycarbonyl chloride solution (10.0g/L). accurately weigh 0.50g of 9-fluorenyl methoxycarbonyl chloride (4.2.5) and dissolve in 20mL acetonitrile (4.2.2), transfer into a 50mL volumetric flask, and dilute to the mark with acetonitrile (4.2.2). 4.2.10 Standard curve working solution. accurately weigh 25.0 mg (accurate to 0.1 mg) of the dimethyl oxazolidine standard product (3.2.4) and place it in 50 mL In a brown volumetric flask, dissolve and dilute with acetonitrile (4.2.2) to obtain a standard stock solution with a mass concentration of 500 mg/L (stored at 4°C in the dark, It should be kept for 3 months). Accurately pipette an appropriate amount of standard stock solution and dilute it step by step with 50% acetonitrile solution (4.2.6) to a mass concentration of 2.50mg/L, 5.00mg/L, 10.0mg/L, 20.0mg/L, 50.0mg/L, 100mg/L standard working solution (should be prepared for current use). 4.2.11 Membrane. PTFE membrane with a pore size of 0.22μm. 4.3 Equipment 4.3.1 High performance liquid chromatograph. equipped with a diode array detector. 4.3.2 Analytical balance. the division value is 0.001g and 0.0001g. 4.3.3 Vortex oscillator. the maximum speed is not less than 3000r/min. 4.3.4 Ultrasonic cleaner. the maximum operating frequency is not less than 40kHz. 4.3.5 High-speed centrifuge. the speed is not less than 4000r/min. 4.4 Test procedure 4.4.1 Sample handling Weigh 0.5g of the sample (accurate to 0.001g), place it in a 10mL colorimetric tube with a stopper, add 8mL of 50% acetonitrile solution (4.2.6), vortex Rotate for 1 min, ultrasonically extract for 10 min, cool to room temperature, dilute to 10 mL with 50% acetonitrile solution (4.2.6), mix well, and take 5 mL Transfer the extract to a centrifuge tube, add 3 mL of acetonitrile saturated n-hexane (4.2.7), vortex for 1 min, centrifuge at 4000 r/min for 2 min, Make sure to remove 1.0 mL of the lower layer of clear liquid, add 0.2 mL of buffer solution (4.2.8), vortex to mix evenly, and then add 0.2 mL of 9-fluorenyl methoxycarbonyl Chlorine solution (4.2.9), react at room temperature for 10 minutes, and the derivative solution is filtered by a membrane to obtain sample solution B, which is measured by high performance liquid chromatograph. Note. If the raw materials identified in the ingredient list contain amino or secondary amino groups, the amount of 9-fluorenyl methoxycarbonyl chloride solution should be appropriately increased to 0.5 mL. 4.4.2 Measurement conditions The reference working conditions of high performance liquid chromatography are as follows. a) Chromatographic column. C18 column, 1.8μm, 50mm×2.1mm (inner diameter) or C18 column, 5.0μm, 150mm×4.6mm (inner diameter), or Equivalent b) Mobile phase. acetonitrile (4.2.2) and water, the gradient elution conditions are shown in Table 3; c) Flow rate. 0.4mL/min; d) Column temperature. 30℃; e) Wavelength. 265nm; f) Injection volume. 2μL; g) After running time. 3min. Table 3 HPLC gradient elution conditions Time/min Acetonitrile/% Water/% 0.0 20 80 6.0 60 40 9.9 80 20 10.0 20 80 4.4.3 Drawing standard working curve Accurately pipette 1.0 mL of each standard working solution (4.2.10), add 0.2 mL buffer solution (4.2.8), vortex to mix evenly, and then add 0.2mL 9-fluorenyl methoxycarbonyl chloride solution (4.2.9), react at room temperature for 10 minutes, the derivative solution is filtered by the filter membrane, and then work according to the high performance liquid chromatography reference Condition (4.4.2) is measured, the peak area of the chromatographic peak is used as the ordinate, and the corresponding solution concentration is plotted on the abscissa, and the standard work is drawn curve. Refer to Figure C.1 in Appendix C for the liquid chromatogram of the dimethyl oxazolidine standard substance derivative, dimethyl oxazolidine standard substance derivative See Figure C.2.for the spectrogram. 4.4.4 Sample measurement Measure the sample solution B (4.4.1) according to the reference working conditions of high performance liquid chromatography (4.4.2), if the retention time of the detected chromatographic peak is consistent with the standard The quasi-substance is consistent, and in the sample chromatogram after deducting the background, the spectrum of the substance is consistent with that of the standard substance, it can be preliminarily determined The sample is a positive sample, and the peak area of the chromatographic peak is recorded and quantified by external standard method. The response value of the analyte in the sample solution B should be in the standard work Within the linear range of the curve. If the sample solution B exceeds the linear range, the underivatized lower layer of the sample should be dissolved in 50% acetonitrile. The solution (4.2.6) is appropriately diluted and re-derivatized for measurement. 4.4.5 Blank test Except that the sample is not weighed, the measurement is carried out according to 4.4.1~4.4.2. 4.5 Result calculation The content of the test compound in the sample is calculated according to formula (2). w= (ρ-ρ0)×V×1000 m×1000 (2) Where. w --- The content of the tested component in the sample, in milligrams per kilogram (mg/kg); ρ --- The mass concentration of the tested component in the sample solution (4.4.1) obtained from the standard curve, in milligrams per liter (mg/L); ρ0 --- The mass concentration of the tested component in the blank sample (4.4.5) obtained from the standard curve, in milligrams per liter (mg/L); V ---The constant volume of the sample solution, the unit is milliliters (mL); m ---The mass of the sample, in grams (g). The result retains three significant figures. 4.6 Recovery rate and precision When the additive concentration is in the range of 50.0mg/kg~500mg/kg, the recovery rate is 80%~110%, and the relative standard deviation is less than 10%. 4.7 Allowance The absolute difference between the two independent measurement results obtained under repeatability conditions is not more than 10% of the arithmetic mean of the two measurement values. ......

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