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Basic dataStandard ID: WS/T 685-2020 (WS/T685-2020)Description (Translated English): (Detection methods and evaluation requirements for antifungal drugs in disinfectants and antibacterial agents) Sector / Industry: Health Industry Standard (Recommended) Classification of Chinese Standard: C50 Word Count Estimation: 13,130 Date of Issue: 2020-07-20 Date of Implementation: 2021-02-01 Regulation (derived from): State-health communication (2020) No. 14 Issuing agency(ies): National Health Commission WS/T 685-2020: (Detection methods and evaluation requirements for antifungal drugs in disinfectants and antibacterial agents)---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. (Detection methods and evaluation requirements for antifungal drugs in disinfectants and antibacterial agents) ICS 11.080 C 50 WS People's Republic of China Health Industry Standard Detection methods and evaluation requirements of antifungal drugs in disinfectants and antibacterial agents Issued by the National Health Commission of the People's Republic of China ForewordThis standard was drafted in accordance with the rules given in GB/T 1.1-2009. Drafting organizations of this standard. Shandong Provincial Center for Disease Control and Prevention, China Center for Disease Control and Prevention, Environmental and Health Related Product Safety Institute, Qingdao Food and Drug Inspection and Research Institute of Shandong Province, Jiangsu Province Center for Disease Control and Prevention, Shandong Province Dezhou Center for Disease Control and Prevention, Shandong Province Jining City Center for Disease Control and Prevention, Beijing Municipal Center for Disease Control and Prevention. The main drafters of this standard. Cui Shuyu, Yang Bin, Su Guanmin, Jiang Dafeng, Xin Chenglong, Shen Jin, Zhang Liubo, Lu Jingguang, Xu Yan, Dong Jian, Liu Jun, Sun Huihui, Chen Jindong, Wang Jinyan, Zhu Feng, Yang Xiao, Ding Xiaojing, Wang Ping. Detection methods and evaluation requirements of antifungal drugs in disinfectants and antibacterial agents1 ScopeThis standard specifies the testing methods and evaluation requirements for antifungal drugs in disinfectants and antibacterial agents. This standard applies to griseofulvin, econazole nitrate, fluconazole, ketoconazole, clotrimazole, bifonazole, Determination and evaluation of miconazole nitrate, flucytosine, naftifine hydrochloride and other antifungal drugs.2 Normative referencesThe following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this document. For undated references, the latest version (including all amendments) applies to this document. GB/T 6682 Analytical laboratory water specifications and test methods Pharmacopoeia of the People's Republic of China3 Terms and definitionsThe following terms and definitions apply to this document. 3.1 Antifungal drugs Drugs that have antibacterial and/or bactericidal properties and are used to prevent and treat fungal infections, including antifungal drugs and prescription drugs The rational chemical synthesis of drugs.4 Detection method4.1 Principle After the sample is ultrasonically extracted with 1% formic acid acetonitrile, the cream formulation sample needs to be purified by N-propyl ethylenediamine, and other formulation samples do not need to be purified Measured by ultra performance liquid chromatography-tandem mass spectrometer, and quantified by external standard method. 4.2 Reagents and materials Unless otherwise stated, the reagents used are all chromatographically pure, and the experimental water is the first grade water specified in GB/T 6682. 4.2.1 Reagents 4.2.1.1 Acetonitrile (CH3CN). 4.2.1.2 Formic acid (HCOOH). 4.2.1.3 N-propyl ethylenediamine (C5H14N2). 4.2.2 Reagent preparation 4.2.2.1 0.1% formic acid aqueous solution. take 1.0 mL of formic acid, dilute to 1000 mL with water, and mix. 4.2.2.2 1% formic acid aqueous solution. take 10.0 mL of formic acid, dilute to 1000 mL with water, and mix. 4.2.2.3 0.1% formic acid acetonitrile solution. take 1.0 mL of formic acid, dilute to 1000 mL with acetonitrile, and mix. 4.2.2.4 1% formic acid acetonitrile solution. take 10.0 mL of formic acid, dilute to 1000 mL with acetonitrile, and mix. 4.2.2.5 0.1% formic acid acetonitrile aqueous solution. Take 300 mL of acetonitrile, add 1.0 mL of formic acid, dilute to 1000 mL with water, and mix. 4.2.3 Standard products Griseofulvin, ketoconazole, clotrimazole, econazole nitrate, miconazole nitrate, fluconazole, bifonazole, flucytosine, naphthalene hydrochloride Fen has a purity greater than 98.5% or a standard substance certified by the country and granted a standard substance certificate. For other relevant information, see Appendix A. 4.2.4 Standard solution preparation 4.2.4.1 Standard stock solution (1000 μg/mL). Weigh 50.0 mg (accurate to 0.1 mg) of the standard respectively, and dissolve it with a small amount of acetonitrile. After the solution, transfer to a 50 mL volumetric flask, add acetonitrile to dissolve and dilute to the mark, and mix well, and the mass concentration will be 1000 μg/mL The standard stock solution, stored at -20℃±2℃, is valid for 3 months. 4.2.4.2 Mixed standard intermediate solution. Take an appropriate amount of the above standard stock solution and use acetonitrile to prepare the ketoconazole mass concentration of 10 μg/mL, The mass concentration of pyrimidine is 5 μg/mL, the mass concentration of fluconazole, griseofulvin, and bifonazole is 1 μg/L, econazole nitrate, miconazole nitrate, The mixed standard intermediate solution of naftifine hydrochloride and clotrimazole with a mass concentration of 0.5 μg/mL, stored in cold storage and protected from light, is valid for 1 month. 4.2.4.3 Mixed standard series solution. draw different volumes of mixed standard intermediate solution, and use the blank sample extract to prepare the appropriate quality concentration The standard working solution of ketoconazole is 10 μg/L, 25 μg/L, 50 μg/L, 100 μg/L, 150 μg/L,.200 μg/L. The mass concentration of flucytosine is 5 μg/L, 12.5 μg/L, 25 μg/L, 50 μg/L, 75 μg/L, 100 μg/L, fluconazole, griseofulvin, The mass concentration of bifonazole is 1 μg/L, 2.5 μg/L, 5 μg/L, 10 μg/L, 15 μg/L, 20 μg/L, econazole nitrate, miconazole nitrate The mass concentrations of azole, naftifine hydrochloride and clotrimazole are 0.5 μg/L, 1.25 μg/L, 2.5 μg/L, 5 μg/L, 7.5 μg/L, and 10 μg/L, which are prepared for immediate use. 4.2.5 Materials Organic filter membrane. pore size is 0.22 μm. 4.3 Apparatus and equipment 4.3.1 Ultra-high performance liquid chromatography-tandem mass spectrometer. charged electrospray ion source (ESI source). 4.3.2 Analytical balance. the smallest division value is 0.1 mg. 4.3.3 Centrifuge. speed ≥9000 r/min. 4.3.4 Vortex mixer. 4.3.5 Ultrasonic cleaner. 4.4 Analysis steps 4.4.1 Sample preparation 4.4.1.1 Purification treatment of cream dosage form samples Weigh 0.5 g (accurate to 1 mg) of sample into a 15 mL centrifuge tube, add 8.0 mL of 1% formic acid acetonitrile, vortex for 1 min, add 50 mg N-propyl ethylene diamine, ultrasonic extraction for 30 min, centrifugation (9000 r/min) for 5 min, transfer the supernatant to a 10 mL volumetric flask, 1% ethyl formic acid Nitrile is made to volume. After mixing, take 1.0 mL and place it in a 10 mL volumetric flask, dilute to the mark with 0.1% formic acid acetonitrile aqueous solution, mix and transfer to Centrifuge the tube (9000r/min) for 5 minutes, take the supernatant and filter it through the membrane for use. 4.4.1.2 Sample processing of other dosage forms Weigh 0.5 g (accurate to 1 mg) of the sample into a 15 mL centrifuge tube, add 8.0 mL of 1% formic acid acetonitrile, vortex for 1 min, and ultrasonically extract After 30 minutes, centrifuge (9000 r/min) for 5 minutes, transfer the supernatant to a 10 mL volumetric flask, and dilute to the mark with 1% formic acid acetonitrile. Take after mixing Place 1.0 mL in a 10 mL volumetric flask, dilute the volume to the mark with the initial mobile phase, transfer to a centrifuge tube after mixing, and centrifuge (9000 r/min) for 5 min. Take the supernatant and filter it through the membrane for use. 4.4.2 Sample determination 4.4.2.1 Reference conditions for liquid chromatography The reference conditions of liquid chromatography are as follows. a) Chromatographic column. C18 column (column length is 100 mm, inner diameter is 2.1 mm, particle diameter is 1.7 μm), or equivalent; b) Mobile phase. Phase A is 0.1% formic acid aqueous solution, Phase B is 1% formic acid acetonitrile solution; c) Flow rate. 0.3 mL/min; d) Column temperature. 30℃; e) Injection volume. 2 μL; f) Gradient elution procedure. see Appendix B. 4.4.2.2 Mass spectrometry reference conditions The mass spectrometry reference conditions are as follows. a) Ionization method. ESI; b) Ion source temperature. 150℃; c) Capillary voltage. 3.0 kV; d) Desolventizing gas temperature. 400℃; e) Desolventizing gas (N2) flow rate. 800 L/h; f) Cone gas (N2) flow rate. 150 L/h; g) Monitoring method. multiple reaction monitoring (MRM) mode; h) Other mass spectrometry parameters. see Appendix C. 4.4.2.3 Preparation of standard curve The mixed standard series solutions were injected into the liquid chromatography tandem mass spectrometer according to the mass concentration from low to high, and the corresponding peak surface was measured. product. Take the mass concentration of each antifungal drug standard working solution as the abscissa and the peak area of each antifungal drug as the ordinate to draw the standard curve. The ion pair is used for qualitative analysis, and the external standard method is used for quantitative analysis. See Appendix D for the standard spectrum. 4.4.2.4 Qualitative determination Under the same test conditions, the retention time of the target compound chromatographic peak in the sample is compared with the retention time of the corresponding standard chromatographic peak. The chemical range is within ±2.5%, and the detected relative ion abundance should be consistent with the relative ion abundance in the standard solution with equivalent mass concentration. The relative ion abundance ratio deviation should meet the requirements of Table 1. 4.4.2.5 Quantitative determination According to the external standard method for quantitative calculation, the response value of the antifungal drug in the standard solution and the sample solution should be within the linear response range of the instrument Inside. If the concentration exceeds the range of the standard curve, it should be diluted to an appropriate mass concentration before analysis. 4.4.2.6 Determination of the target compound in the sample Inject the sample solution into the liquid chromatography-tandem mass spectrometer for retention time and two pairs of ions (characteristic ion pair/quantitative ion pair) The relative abundance of the corresponding chromatographic peak area is qualitative, and the mass concentration of the target compound in the sample solution is calculated according to the standard curve. 4.4.3 Blank test Except that no sample solution is added, the steps in 4.4.2.6 are followed. 4.4.4 Calculation and expression of results The content of the target compound in the sample is calculated according to formula (1). 4.4.5 Precision The absolute difference between two independent determination results obtained under repeatability conditions should not exceed 15% of the arithmetic mean. Recovery rate of this method And precision see Annex E. 4.4.6 Detection limit and quantification limit When the sampling volume is 0.5 g and the quantitative volume is 10 mL, the detection limit and quantification limit of this method are shown in Appendix F.5 Testing methods for other antifungal drugsYou can refer to the method of "The Pharmacopoeia of the People's Republic of China" and perform method verification. Test methods for antifungal drugs not covered by the Pharmacopoeia of the People’s Republic of China. The methods reported in the literature can be referred to and can be used after certification.6 Evaluation requirements6.1 Antifungal drugs should not be added to disinfectants and antibacterial agents. 6.2 In disinfectants and antibacterial agents, griseofulvin, ketoconazole, clotrimazole, econazole nitrate, miconazole nitrate, fluconazole, bifonazole, The content or total amount of flucytosine and naftifine hydrochloride should not exceed 100 mg/kg. 6.3 The content or total amount of other antifungal drugs in disinfectants and antibacterial agents should not exceed 1% of the minimum specification of external drugs. A ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of WS/T 685-2020_English be delivered?Answer: Upon your order, we will start to translate WS/T 685-2020_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. 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