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Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 31613.6-2022: (National food safety standards Determination of virginiamycin M1 residues in edible tissues of pigs and poultry by liquid chromatography-tandem mass spectrometry) Status: Valid
Basic dataStandard ID: GB 31613.6-2022 (GB31613.6-2022)Description (Translated English): (National food safety standards Determination of virginiamycin M1 residues in edible tissues of pigs and poultry by liquid chromatography-tandem mass spectrometry) Sector / Industry: National Standard Word Count Estimation: 9,970 Date of Issue: 2022-09-20 Date of Implementation: 2023-02-01 Issuing agency(ies): National Health Commission of the People's Republic of China, State Administration for Market Regulation GB 31613.6-2022: (National food safety standards Determination of virginiamycin M1 residues in edible tissues of pigs and poultry by 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 Health Commission of the People's Republic of China National food safety standard pig and poultry edibility organization Determination of Residues of Virginiamycin M1 Liquid Chromatography-Tandem Mass Spectrometry National Standards of People's Republic of China release State Administration for Market Regulation Ministry of Agriculture and Rural Affairs of the People's Republic of China forewordThis document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for Standardization Work Part 1.Structure and Drafting Rules for Standardization Documents" drafting. This document is published for the first time. National Food Safety Standards Determination of virginiamycin M1 residues in edible tissues of pigs and poultry Liquid chromatography-tandem mass spectrometry1 ScopeThis document specifies the sample preparation and liquid chromatography-tandem mass spectrometry for detection of virginiamycin M1 residues in edible tissues of pigs and poultry. method. This document is applicable to the determination of virginiamycin M1 residues in muscle, liver, kidney and skin + fat of pigs and poultry (including chicken, duck and goose) detection.2 Normative referencesThe content in the following documents constitutes the essential provisions of this document through normative references in the text. Among them, the dated reference documents, Only the version corresponding to the date applies to this document; for undated references, the latest version (including all amendments) applies to this document document. GB/T 6682 Analytical laboratory water specifications and test methods3 Terms and DefinitionsThis document does not have terms and definitions that need to be defined.4 principlesThe residual virginiamycin M1 in the sample was extracted with acetonitrile, degreased with n-hexane, detected by liquid chromatography-tandem mass spectrometry, and quantified by external standard method.5 Reagents and materialsThe reagents used below are all analytical reagents unless otherwise specified; the water is the first-class water in accordance with the provisions of GB/T 6682. 5.1 Reagents 5.1.1 Acetonitrile (CH3CN). chromatographically pure. 5.1.2 Formic acid (HCOOH). chromatographically pure. 5.1.3 Acetonitrile (CH3CN). 5.1.4 n-Hexane (C6H14). 5.2 Solution preparation 5.2.1 Acetonitrile solution. Take 600mL of acetonitrile and 400mL of water, and mix them evenly. 5.2.2 0.1% formic acid solution. take 1mL of formic acid, dilute it with water to 1000mL, and mix well. 5.3 Standards Virginiamycin M1 (Virginiamycin M1, C28H35N3O7, CAS number. 21411-53-0) content was ≥90%. 5.4 Preparation of standard solution 5.4.1 Standard stock solution. Take 10 mg of virginiamycin M1 standard product, weigh it accurately, dissolve it with acetonitrile and dilute to volume. 200mL brown volumetric flask, prepared into a standard stock solution of virginiamycin M1 with a concentration of 50μg/mL. Store below 4°C, and the expiration date is 7d. 5.4.2 Standard intermediate solution. Accurately measure 0.1mL, 0.5mL, 1mL, 2mL and 3mL of standard stock solution, and put them into 50mL brown container Diluted to the mark with acetonitrile to prepare vitamins with concentrations of 0.1 μg/mL, 0.5 μg/mL, 1 μg/mL, 2 μg/mL and 3 μg/mL. Geniamycin M1 standard intermediate solution. Store below 4°C, with a validity period of 7 days. 5.5 Materials 5.5.1 Graduated test tube. 10mL. 5.5.2 Organic filter membrane. 0.22 μm.6 Instruments and equipment6.1 Liquid chromatography-tandem mass spectrometer. distribution of electrospray ionization source. 6.2 Analytical balance. Sensitivity 0.00001g and 0.01g. 6.3 Homogenizer. 6.4 Ultrasound machine. 6.5 Centrifuge. ≥4000r/min. 6.6 Vortex shaker. 6.7 Pipettes.7 Preparation and storage of samples7.1 Preparation of samples Take an appropriate amount of fresh or thawed blank or test tissue, mince and homogenize. a) Take the homogeneous test sample as the test sample; b) Take a homogeneous blank sample as a blank sample; c) Take a homogeneous blank sample, add standard working solution of appropriate concentration, and add the sample as a blank. 7.2 Storage of samples Store below -40°C and avoid repeated freezing and thawing.8 Measurement steps8.1 Extraction Take 2 g of the sample (accurate to ±0.05 g), add 4 mL of acetonitrile (add 2 mL of water to the muscle tissue first), vortex for 2 min, and sonicate for 30 min. Centrifuge at 4000r/min for 10min, take the supernatant and transfer it to a 15mL centrifuge tube with a stopper. Add 2mL of acetonitrile to the residue and repeat the extraction once, and combine The supernatant was set aside to obtain the extract. 8.2 Purification Take the above extract, add water to about 9.5mL, vortex and mix for 30s, add n-hexane 3mL, vortex for 30s, centrifuge at 4000r/min for 10min, Discard the upper layer of n-hexane, and repeat the degreasing once. Transfer the lower layer solution to a 10mL graduated test tube, add water to 10mL, vortex for 30s, and prepare Use. Take the spare solution (liver. take 2.0mL of the spare solution, add 4.0mL of acetonitrile solution, mix well; kidney, sebum. take 2.0mL of the spare solution, add acetonitrile solution (6.0 mL, mixed), filtered, and determined by liquid chromatography-tandem mass spectrometry. 8.3 Preparation of standard curve 8.3.1 Preparation of poultry muscle and liver matrix matching standard curve Accurately measure virginiamycin M1 standards with concentrations of 0.1 μg/mL, 0.5 μg/mL, 1 μg/mL, 2 μg/mL and 3 μg/mL Add.200 μL of each intermediate solution to the blank tissue extract after degreasing treatment with 7.1 and 7.2 n-hexane, add water to 10 mL, mix well, Treated in the same way. Preparation of virginiamycin M1 concentration of 2ng/mL, 10ng/mL, 20ng/mL, 40ng/mL and 60ng/mL series Match the standard solution with the column matrix, filter it, prepare it immediately before use, and use it for liquid chromatography coupled with mass spectrometer for determination. Take the measured characteristic ion peak area as the ordinate, and The concentration of the corresponding standard solution is the abscissa, and the standard curve is drawn. Find the regression equation and correlation coefficient. 8.3.2 Preparation of standard curves of other tissues Accurately measure virginiamycin M1 at concentrations of 0.1 μg/mL, 0.5 μg/mL, 1 μg/mL, 2 μg/mL and 3 μg/mL Add acetonitrile solution to.200 μL of each standard intermediate solution to 10.0 mL, and prepare virginiamycin M1 with a concentration of 2 ng/mL, 10 ng/mL, 20ng/mL, 40ng/mL and 60ng/mL series of standard working solutions, prepared immediately before use, for determination by liquid chromatography coupled with mass spectrometer. The area of the characteristic ion peak is the ordinate, and the corresponding concentration of the standard solution is the abscissa, and the standard curve is drawn. Find the regression equation and the correlation coefficient. 8.4 Determination 8.4.1 Chromatographic conditions a) Chromatographic column. C18 (100mm×2.1mm, 1.7μm), or equivalent; b) Column temperature. 30°C; c) Injection volume. 5 μL; d) Flow rate. 0.2mL/min; e) Mobile phase. A is acetonitrile, B is 0.1% formic acid aqueous solution, and the gradient elution program is shown in Table 1. 8.4.2 Mass Spectrometry Conditions a) Ion source. electrospray ion source; b) Scanning mode. positive ion scanning; c) Detection method. multiple reaction monitoring (MRM); d) Ion source temperature. 150°C; e) Desolventization temperature..200°C; f) Capillary voltage. 3.0kV; g) Desolvation gas flow rate. 800L/h. h) Cone back blowing air flow rate. 150L/h. i) See Table 2 for qualifier ion pairs, quantifier ion pairs, cone voltage and collision energy. 8.5 Determination method 8.5.1 Qualitative determination Under the same test conditions, the retention time of the chromatogram of virginiamycin M1 in the sample solution was the same as that in the corresponding standard working solution. The deviation between them should not be greater than ±2.5%; and the relative abundance of the detected ions should be consistent with the relative abundance of the standard solution with the same concentration. The permissible deviation should meet the requirements in Table 3. 8.5.2 Quantitative determination Take the sample solution and the corresponding matrix matching standard working solution/standard working solution for single-point or multi-point calibration, and quantify by peak area according to the external standard method. Matrix matching standard working solution/response value of virginiamycin M1 in standard working solution and sample solution should be within the linear range of instrument detection See Appendix A for the characteristic ion mass chromatograms of virginiamycin M1 matrix-matched standard solution under the above chromatography-mass spectrometry conditions. 8.6 Blank test Take the blank sample, except that no drug is added, the same steps are used for parallel operation.9 Calculation of resultsThe residual amount of virginiamycin M1 in the sample was calculated according to the standard curve or formula (1). 10 Method sensitivity, accuracy and precision 10.1 Sensitivity The detection limits of virginiamycin M1 in muscle, liver, kidney and sebum were 2 μg/kg, 6 μg/kg, 8 μg/kg and The quantitative limit of muscle was 10 μg/kg, and the quantitative limit of other tissues was 50 μg/kg. 10.2 Accuracy In this method, virginiamycin M1 is effective in poultry and pig muscle tissue at 10 μg/kg~200 μg/kg, liver and kidney tissue at 50 μg/kg~ 600 μg/kg, and sebum tissue 50 μg/kg-800 μg/kg, the recovery rate was 70%-120%. 10.3 Precision In this method, the relative standard deviation within the batch was ≤20%, and the relative standard deviation between batches was ≤20%. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 31613.6-2022_English be delivered?Answer: Upon your order, we will start to translate GB 31613.6-2022_English as soon as possible, and keep you informed of the progress. 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