GB 31658.17-2021 English PDF

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GB 31658.17-2021: (National Food Safety Standard Determination of Tetracyclines, Sulfonamides and Quinolones Residues in Animal Foods Liquid Chromatography-Tandem Mass Spectrometry)
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 31658.17-2021	239	Add to Cart	3 days	(National Food Safety Standard Determination of Tetracyclines, Sulfonamides and Quinolones Residues in Animal Foods Liquid Chromatography-Tandem Mass Spectrometry)	Valid

Similar standards

GB 31650.1   GB/T 37517   GB/T 30636   GB 31658.20   GB 31658.21   GB 31658.19   

Basic data

Standard ID: GB 31658.17-2021 (GB31658.17-2021)
Description (Translated English): (National Food Safety Standard Determination of Tetracyclines, Sulfonamides and Quinolones Residues in Animal Foods Liquid Chromatography-Tandem Mass Spectrometry)
Sector / Industry: National Standard
Classification of Chinese Standard: X04
Word Count Estimation: 12,127
Issuing agency(ies): National Health Commission of the People's Republic of China, State Administration for Market Regulation

GB 31658.17-2021: (National Food Safety Standard Determination of Tetracyclines, Sulfonamides and Quinolones Residues in Animal Foods 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.
National food safety standards Tetracyclines, sulfonamides and quinolones in animal foods Determination of substance residues by liquid chromatography-tandem mass spectrometry National Standards of People's Republic of China Released by the National Health Commission of the People's Republic of China State Administration for Market Regulation Ministry of Agriculture and Rural Affairs of the People's Republic of China

Foreword

This document is drafted in accordance with the provisions of GB/T 1:1-2020 "Standardization Work Guidelines Part 1: Structure and Drafting Rules of Standardization Documents": This document is published for the first time:

1 Scope

This document specifies sample preparation and liquid chromatography-tandem mass spectrometry methods for the detection of tetracyclines, sulfonamides and quinolones residues in animal foods: This document applies to tetracyclines (tetracycline, chlortetracycline, oxytetracycline, doxycycline), sulfonamides (acesulfonamide, sulfapyridine, sulfadiazine, Sulfamethazole, sulfathiazole, sulfamethazine, sulfamethoxazole, sulfamethoxazole, benzoylsulfonamide, sulfamethoxazine, sulfamethoxazine, sulfamethoxine, sulfamethoxypyridazine , sulfamethoxazine, sulfachlorpyridazine, sulfa-dimethoxine, sulfamethoxazole, sulfaphenazole, phthalosulfathiazole) and quinolones (norfloxacin, enoxacin, Profloxacin, pefloxacin, lomefloxacin, danofloxacin, enrofloxacin, ofloxacin, mabofloxacin, sarafloxacin, difloxacin, quinoacid, flumequine) drugs Determination of residual amounts:

2 Normative reference documents

The contents of the following documents constitute essential provisions of this document through normative citations in the text: Among them, the cited documents with dates are: Only the version corresponding to the date applies to this document; for undated referenced documents, the latest version (including all amendments) applies to this document: document: GB/T 6682 Specifications and test methods for water used in analytical laboratories

3 Terms and definitions

There are no terms or definitions that need to be defined in this document:

4 Principles

The remaining tetracyclines, sulfonamides and quinolones in the sample were extracted with Mclvaine-Na2EDTA buffer and the hydrophilic-lipophilic balance was used: Solid-phase extraction column purification, liquid chromatography-tandem mass spectrometry determination, and external standard method for quantitation:

5 Reagents and materials

Unless otherwise specified, all reagents are of analytical grade and the water is first-grade water that complies with GB/T 6682: 5:1 Reagents 5:1:1 Acetonitrile (CH3CN): chromatographically pure: 5:1:2 Methanol (CH3OH): chromatographically pure: 5:1:3 Ethyl acetate (C4H8O2): chromatographically pure: 5:1:4 Formic acid (HCOOH): chromatographically pure: 5:1:5 Disodium ethylenediaminetetraacetate dihydrate (C10H14N2Na2O8:2H2O): 5:1:6 Concentrated ammonia (NH3H2O): 5:1:7 Disodium hydrogen phosphate: Dodecahydrate (Na2HPO4:12H2O): 5:1:8 Sodium dihydrogen phosphate dihydrate (NaH2PO4:2H2O): 5:1:9 Citric acid: Monohydrate (C6H8O7:H2O): 5:1:10 Sodium hydroxide (NaOH): 5:2 Solution preparation 5:2:1 0:05mol/L sodium dihydrogen phosphate solution: Take 7:8g of sodium dihydrogen phosphate dihydrate, dissolve it in water and dilute it to 1000mL: 5:2:2 0:05mol/L disodium hydrogen phosphate solution: Take 17:9g of disodium hydrogen phosphate and dodecahydrate, dissolve it in water and dilute it to 1000mL: 6:2 Analytical balance: sensitivity 0:00001g and 0:01g: 6:3 High-speed refrigerated centrifuge: -2℃, 14000r/min: 6:4 Tissue homogenizer: 6:5 Vortex mixer: 6:6 Solid phase extraction device: 6:7 Nitrogen blower: 6:8 Ultrasonic cleaning instrument: 7: Preparation and preservation of samples 7:1 Preparation of samples Take an appropriate amount of fresh or thawed blank or test tissue, mince it, and homogenize it: a) Take the homogenized test sample as the test material; b) Take the homogenized blank sample as the blank sample; c) Take the homogenized blank sample, add the standard working solution of appropriate concentration, and add the sample as a blank: 7:2 Storage of samples Store below -18℃:

8 Measurement steps

8:1 Extraction Weigh 1g of the sample (accurate to ±0:01g), add 8mL of Mclvaine-Na2EDTA buffer, vortex for 1min, and sonicate for 20min: Centrifuge at -2°C and 10,000 r/min for 5 min, collect the supernatant: Add 8 mL of phosphate buffer to the residue, repeat the extraction once, combine the two extracts, mix well, and set aside: 8:2 Purification The solid-phase extraction column was activated with 5 mL of methanol and 5 mL of water in sequence, and the reserve solution was passed through the column, followed by 5 mL of water and 20% methanol aqueous solution: Elute with 5 mL, drain, and elute with 10 mL of eluent: Collect the eluate and blow dry with nitrogen in a 45°C water bath: Add 1:0 mL of the complex solution and vortex: Dissolve the residue for 1 minute, centrifuge at 14000 r/min for 5 minutes, filter with a microporous membrane, and measure by liquid chromatography-tandem mass spectrometry: 8:3 Preparation of matrix matching standard curve Precisely measure an appropriate amount of the mixed standard working solution, add it to 6 extracted and purified blank sample residues, and blow dry with nitrogen in a 45°C water bath: Add 1:0 mL of the complex solution and vortex to dissolve the residue, and prepare a series of matrix-matched mixed standard solutions with concentrations of 2 μg/L, 10 μg/L, 50 μg/L, 100 μg/L, 250 μg/L, and 500 μg/L: Microporous filter Membrane filtration, liquid chromatography-tandem mass spectrometer measurement: Taking the measured characteristic ion peak area as the ordinate and the corresponding standard solution concentration as the abscissa, draw a standard curve and find the regression equation and correlation coefficient: 8:4 Determination 8:4:1 Liquid chromatography reference conditions a) Chromatographic column: C18 (50mm×2:1mm, 1:7μm), or equivalent; b) Column temperature: 35℃; c) Injection volume: 10μL; d) Flow rate: 0:3mL/min; e) Mobile phase: A is 0:1% formic acid aqueous solution, B is methanol:acetonitrile (2:8, containing 0:1% formic acid, volume ratio) solution, gradient elution bar See Table 1 for details: 8:4:2 Mass spectrometry reference conditions a) Ion source: electrospray ion source; b) Scanning method: positive ion scanning; GB 31658:17-2021 c) Detection method: multiple reaction monitoring; d) Ion source temperature: 100℃; e) Atomization temperature: 450℃; f) Ionization voltage: 3:0kV; g) Cone air flow rate: 30L/h; h) Atomizing gas flow rate: 1000L/h; i) Qualitative ion pairs, quantitative ion pairs, cone voltage and collision energy are shown in Table 2: 8:4:3 Qualitative determination Under the same test conditions, the retention time of tetracyclines, sulfonamides, and quinolones in the sample solution is the same as that in the matrix-matched standard solution: The retention time of corresponding tetracyclines, sulfonamides, and quinolones should have a deviation within ±2:5%, and the detected relative ion abundance should be consistent with Matrix-matched standard solutions with equivalent concentrations have the same relative ion abundance: The allowable deviations should meet the requirements of Table 3: 8:4:4 Quantitative determination Set the instrument conditions according to 8:4:1 and 8:4:2, use the concentration of the matrix matching standard solution as the abscissa and the peak area as the ordinate to draw the standard Working curve, make single point or multi-point calibration, calculate the residual amount of drug in the sample according to the external standard method, the matrix matching standard solution and the target substance response value in the sample solution should be within the linear range of the instrument detection: Standard solution The characteristic ion mass chromatogram is shown in Appendix B: 8:5 Blank test Take a blank sample and perform parallel operations using exactly the same measurement steps:

9 Calculation and presentation of results

The residual amounts of tetracyclines, sulfonamides, and quinolones in the sample are calculated according to the standard curve or formula (1): 10 Method sensitivity, accuracy and precision 10:1 Sensitivity The detection limit of this method is 2 μg/kg, and the quantification limit is 10 μg/kg: 10:2 Accuracy The recovery rate of this method at the added concentration level of 10μg/kg~500μg/kg is 60%~110%: 10:3 Precision The intra-batch relative standard deviation of this method is ≤15%, and the inter-batch relative standard deviation is ≤20%: ......

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