GB/T 39873-2021 English PDFUS$189.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB/T 39873-2021: Determination of quaternary ammonium salt in disinfectant - Liquid chromatography-tandem mass spectrometry Status: Valid
Basic dataStandard ID: GB/T 39873-2021 (GB/T39873-2021)Description (Translated English): Determination of quaternary ammonium salt in disinfectant - Liquid chromatography-tandem mass spectrometry Sector / Industry: National Standard (Recommended) Classification of Chinese Standard: C50 Word Count Estimation: 10,154 Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration GB/T 39873-2021: Determination of quaternary ammonium salt in disinfectant - Liquid chromatography-tandem mass spectrometry---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order. Determination of quaternary ammonium salt in disinfectant - Liquid chromatography-tandem mass spectrometry ICS 11.080.20 CCSC50 National Standards of People's Republic of China Determination of quaternary ammonium salt in disinfectant Liquid chromatography-tandem mass spectrometry Released on 2021-03-09 2021-10-01 implementation State Administration of Market Supervision and Administration Issued by the National Standardization Management Committee ForewordThis document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for Standardization Work Part 1.Structure and Drafting Rules of Standardization Documents" Drafting. This document was proposed and managed by the National Standardization Technical Committee on Inspection Methods for Key Products of Quality Supervision (SAC/TC374). Drafting organizations of this document. Shanghai Institute of Quality Supervision and Inspection Technology, CCIC Warner (Beijing) Quality Technology Center Co., Ltd., Infinite Ji (China) Co., Ltd., Guangzhou Zhongke Testing Technology Service Co., Ltd., China Certification & Inspection Group Guangxi Co., Ltd., Jiangsu Tianrui Instrument Co., Ltd., Guangdong Lost Pharmaceutical Co., Ltd., Warner Pass (Beijing) Certification Co., Ltd. The main drafters of this document. Liu Yang, Zheng Guojian, Yang Jinqing, Weng Shiyu, Lin Yikan, Dai Yanyun, Yang Baogang, Shi Jingwen, Mao Xufeng, Meng Jie, Sun Hongmei, Xu Shulan, Meng Liqiong, Zhou Li, Cai Chaoming, Chen Dongyang. Determination of quaternary ammonium salt in disinfectant Liquid chromatography-tandem mass spectrometry1 ScopeThis document specifies the reagents and materials, instruments and equipment, determination procedures, and results for the determination of quaternary ammonium salts in disinfectants by liquid chromatography-tandem mass spectrometry. Result calculation, precision, detection limit and quantification limit. This document applies to dodecyl dimethyl benzyl ammonium chloride (C12-BAC), tetradecyl dimethyl benzyl ammonium chloride (C14- BAC), Cetyl Dimethyl Benzyl Ammonium Chloride (C16-BAC), Didecyl Dimethyl Ammonium Chloride (DDAC), Dodecyl Trimethyl Ammonium Bromide (DTAB), determination of dodecyldimethyl-2-phenoxy-ethylammonium bromide (EDDAB).2 Normative referencesThe contents of the following documents constitute the indispensable clauses of this document through normative references in the text. Among them, dated quotations Only the version corresponding to that date is applicable to this document; for undated reference documents, the latest version (including all amendments) is applicable to This document. GB/T 6682 Analytical laboratory water specifications and test methods3 Terms and definitionsThere are no terms and definitions that need to be defined in this document.4 PrincipleThe sample was ultrasonically extracted with a methanol solution containing 0.5% formic acid, vortexed, and centrifuged, and filtered with a 0.22 μm organic filter membrane. The test solution was subjected to liquid chromatography- Tandem mass spectrometry determination, retention time and relative ion pair abundance qualitative, external standard method quantification.5 Reagents and materialsUnless otherwise specified, use only chromatographically pure reagents. 5.1 Water. GB/T 6682, level one. 5.2 Acetonitrile (CH3CN). 5.3 0.5% formic acid in methanol. pipette 5mL formic acid in a 1000mL volumetric flask, and methanol to a constant volume. 5.4 0.1% formic acid solution. pipette 1mL formic acid in a 1000mL volumetric flask and dilute to volume with water. 5.5 Quaternary ammonium salt standards. dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride, cetyl dimethyl benzyl chloride Ammonium chloride, didecyl dimethyl ammonium chloride, dodecyl trimethyl ammonium bromide, dodecyl dimethyl-2-phenoxy-ethyl ammonium bromide, the purity is not small At 99.0%, see Appendix A for CAS number, molecular formula, and relative molecular mass. 5.6 Quaternary ammonium salt standard stock solution, 100mg/L. accurately weigh 10mg of each quaternary ammonium salt standard substance (5.5), accurate to 0.1mg, in 100mL In the volumetric flask, dissolve and dilute to the mark with 0.5% formic acid in methanol (5.3). The quaternary ammonium salt standard stock solution is stored at -18℃, and the storage period is 6 months. 5.7 Standard working solution. Use 0.5% formic acid in methanol (5.3) to prepare a series of mass concentrations of the above standard stock solution (5.6) respectively. The standard working solutions of 0.050mg/L, 0.100mg/L, 0.200mg/L, 0.500mg/L, 1.00mg/L are currently prepared. 5.8 Filter membrane. 0.22μm, organic membrane.6 Apparatus and equipment6.1 Liquid chromatography-tandem mass spectrometer, power distribution spray ion source. 6.2 Analytical balance, the sensitivity is 0.001g and 0.0001g. 6.3 Ultrasonic oscillator. 6.4 Centrifuge, the speed is greater than or equal to 8000r/min. 6.5 Vortex oscillator.7 Measurement procedure7.1 Sample processing Weigh 1g of sample (accurate to 0.001g), sample 1mL of liquid sample, add 70mL of 0.5% formic acid in a 100mL volumetric flask Methanol solution (5.3), vortex mixing for 1 min, ultrasonic extraction for 20 min, dilute to volume with 0.5% formic acid in methanol (5.3). Take part The sample solution was centrifuged at 8000r/min for 10min, filtered through a 0.22μm filter membrane, and the filtrate was used as the sample solution to be tested for later use. If the content of the tested component is higher High, it can be diluted with 0.5% formic acid in methanol (5.3), filtered through a 0.22μm filter membrane, and the filtrate used as the sample solution to be tested for later use. 7.2 Measurement conditions 7.2.1 Reference conditions for liquid chromatography Depending on the equipment, the measurement conditions may be different. The following measurement conditions have been confirmed to be feasible. a) Chromatographic column. C18, 50mm×2.1mm (particle size 1.7μm), or other equivalent performance; b) Flow rate. 0.3mL/min; c) Column temperature. 35℃; d) Injection volume. 1μL; e) Mobile phase. solvent A. acetonitrile (5.2), solvent B. 0.1% formic acid solution (5.4); f) The gradient elution conditions of liquid chromatography are shown in Table 1. Table 1 Liquid chromatography elution conditions 7.2.2 Reference conditions for mass spectrometry Depending on the equipment, the measurement conditions may be different. The following measurement conditions have been confirmed to be feasible. a) Ionization method. electrospray ionization, positive ion; b) Detection method. multi-reaction monitoring; c) Capillary voltage. 3000V; d) Atomizing gas temperature. 450℃; e) Atomizing gas flow rate. 800L/h; f) Cone air flow rate. 150L/h; g) Ion source temperature. 150℃. See Table 2 for monitoring ion pair, collision energy and cone voltage. Table 2 Multi-reaction monitoring conditions 7.3 Drawing standard working curve According to the measurement conditions of 7.2, draw 1μL of standard working solution (5.7) respectively and measure the concentration from low to high, and quantify the ion pair The peak area is the ordinate, the corresponding solution concentration is the abscissa, and the regression equation of the standard curve is obtained. Refer to Appendix B for the liquid chromatography-tandem mass spectrometry chromatogram of the reference material quaternary ammonium salt. 7.4 Determination of liquid chromatography-tandem mass spectrometry 7.4.1 Qualitative determination When the sample is measured under the same test conditions, the retention time of the detected chromatographic peak is compared with the standard sample, and the variation range is Within ±2.5%; and in the sample mass spectrum, the selected ion pairs appear, and the selected relative ion pair abundance is equivalent to the concentration Compared with the standard solution, the allowable relative deviation does not exceed the range specified in Table 3, then the target analyte can be qualitatively confirmed. 7.4.2 Quantitative determination The liquid chromatography-tandem mass spectrometry in this document adopts the external standard-calibration curve method for quantitative determination, and the response of the tested components in the tested samples should be ensured. The response value is within the range of the standard curve. 7.5 Blank test Except that no sample is added, it shall be implemented in accordance with the provisions of 7.1 to 7.4.8 Result calculationThe calculation of the content of each quaternary ammonium salt in the sample is calculated according to formula (1).9 PrecisionIn the same laboratory, the same operator uses the same equipment, according to the same test method, and compares the same object under test in a short period of time. The absolute difference between the two independent test results obtained by independent tests shall not be greater than 10% of the arithmetic mean of the two measured values. 10 Detection limit and quantification limit When the sampling volume is 1g and the constant volume is 100mL, the detection limit is 0.003g/kg, and the quantification limit is 0.01g/kg. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB/T 39873-2021_English be delivered?Answer: Upon your order, we will start to translate GB/T 39873-2021_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of GB/T 39873-2021_English with my colleagues?Answer: Yes. 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