GB 31613.1-2021 English PDFUS$309.00 · In stock
Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 31613.1-2021: National food safety standard--Determination of amprolium residues in cattle-derived products by liquid chromatographic-tandem mass spectrometry method and high performance liquid chromatographic method Status: Valid
Basic dataStandard ID: GB 31613.1-2021 (GB31613.1-2021)Description (Translated English): National food safety standard--Determination of amprolium residues in cattle-derived products by liquid chromatographic-tandem mass spectrometry method and high performance liquid chromatographic method Sector / Industry: National Standard Classification of Chinese Standard: X22 Classification of International Standard: 67.120 Word Count Estimation: 16,113 Date of Issue: 2021-09-16 Date of Implementation: 2022-02-01 Issuing agency(ies): National Health Commission of the People's Republic of China, State Administration for Market Regulation Summary: This standard specifies the sample preparation and liquid chromatography tandem mass spectrometry method for the detection of amproline residues in bovine edible tissues. This standard applies to the detection of residues of amphetamine in beef muscle, liver, kidney and fat. GB 31613.1-2021: National food safety standard--Determination of amprolium residues in cattle-derived products by liquid chromatographic-tandem mass spectrometry method and high performance liquid chromatographic method---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 Determination of Amprolium Residues in Bovine Edible Tissues Liquid Chromatography-Tandem Mass Spectrometry and High Performance Liquid Chromatography National Standards of People's Republic of China 1 Scope This document specifies the sample preparation and liquid chromatography-tandem mass spectrometry methods for the detection of ampropion residues in cattle edible tissues: This document is applicable to the detection of amproline residues in beef muscle, liver, kidney and fat: 2Normative reference documents The contents of the following documents constitute essential provisions of this document through normative references in the text: Among them, for dated reference documents, only the version corresponding to the date applies to this document; for undated reference documents, the latest version (including all amendments) applies to this document: GB/T 6682 Specifications and test methods for water used in analytical laboratories 3 Terms and definitionsThere are no terms or definitions to be defined in this document:4 PrinciplesThe remaining amproline in the sample was extracted with phosphate buffer (fat samples were extracted with acetonitrile), purified with HLB solid-phase extraction column, measured by liquid chromatography-tandem mass spectrometry, and quantified by the matrix calibration external standard method: 5Reagents 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 Methanol (CH₃OH): chromatographically pure: 5:1:2 Acetonitrile (CH₃CN): chromatographically pure: 5:1:3 Formic acid (HCOOH): chromatographically pure: 5:1:4 Dipotassium hydrogen phosphate (K₂HPO): 5:1:5 Potassium dihydrogen phosphate (KH₂PO): 5:2 Standard products Amoprolium Hydrochloride (Cu₄HiCIN₄·HCl, CAS No:: 137-88-2), content ≥98:0%: 5:3 Solution preparation 5:3:1 Phosphate buffer (pH 6:0): Take 2:0g of dipotassium hydrogen phosphate and 8:0g of potassium dihydrogen phosphate, add water to dissolve and dilute to 1000mL, and mix well: 5:3:20:1% formic acid solution: Take 1mL of formic acid, dilute it with water to 1000mL, and mix well: 5:3:30:1% formic acid solution-methanol: Take 900 mL of 0:1% formic acid solution and 100 mL of methanol, and mix well: 5:4 Preparation of standard solution 5:4:1 Standard stock solution (100 mg/L): Take an appropriate amount of amprolium hydrochloride standard (approximately equivalent to 10 mg of amprolium), weigh it accurately, dissolve it in methanol, dilute it to a 100mL volumetric flask, and shake well: That’s it: Stored below -18℃, valid for 6 months: 5:4:2 Standard working solution: Accurately pipet an appropriate amount of standard stock solution, and dilute it step by step with 0:1% formic acid solution-methanol to a concentration of 5 μg/L, 20 μg/L, 50 pg/L,:200 μg/L, 500 μg/L and A series of standard working solutions of:2000 μg/L: Ready for use: 5:5 Materials HLB solid phase extraction cartridge: 60 mg/3mL, or equivalent: 6Instruments and equipment 6:1 Liquid chromatography-tandem mass spectrometer: equipped with electrospray ion source: 6:2 Analytical balance: sensitive to 0:00001g and 0:01g: 6:3 Nitrogen blowing instrument: 6:4 Solid phase extraction device: 6:5 Homogenizer: 6:6 Vortex mixer: 6:7 Polypropylene plastic centrifuge tube: 50 mL: 6:8 Centrifuge: 8000 r/min or above:7 Preparation and preservation of samples7:1 Preparation of samples Take an appropriate amount of fresh or thawed air 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℃ and conduct analysis and testing within 3 months:8 Measurement steps8:1 Extraction 8:1:1 Bovine muscle, liver and kidneys Take 2g of the sample (accurate to ±0:02g), add 10:0 mL of phosphate buffer, homogenize at 10000 r/min for 1 min, centrifuge at 8000 r/min for 5 min, collect the supernatant, and add 10:0 mL of phosphate buffer to the residue: , repeat the extraction once, combine the supernatants, and set aside: 8:1:2 Beef fat Take 2g of the sample (accurate to ±0:02g), add 10:0 mL of acetonitrile, homogenize at 10000 r/min for 1 min, centrifuge at 8000 r/min for 5 min, and put the supernatant into a 50 mL plastic centrifuge tube: Add 10 mL of acetonitrile to the residue, repeat the extraction once, combine the two supernatants, blow to dryness with nitrogen in a 50°C water bath, dissolve the residue with 20:0 mL of phosphate buffer, and set aside: 8:2 Purification The solid phase extraction column was activated with 3 mL each of methanol and water: Pass 5:0 mL of the backup solution through the column: When the liquid level reaches the surface of the column bed, rinse with 3 mL of water: Squeeze until it is almost dry: Add 2 mL of methanol and elute: The eluate is blown dry with nitrogen in a 40°C water bath: Use 0:1% formic acid solution-methanol (90:10, V/V) Dissolve the residue in 1:0 mL, pass it through a 0:22 μm filter membrane, and measure it with a liquid chromatography-tandem mass spectrometer: 8:3 Preparation of matrix matching standard curve Take the empty sample and process it in sequence according to 8:1 and 8:2 until it is blown dry with nitrogen, add 1:0mL of standard working solution of a series of concentrations to dissolve the residue, and make the concentrations of 5 μg/L, 20 μg/L, 50 μg/L,:200 μg/L, and 500 μg/L: and:2000 μg/L series matrix-matched standard solutions for liquid chromatography-tandem mass spectrometry measurement: Draw a standard curve with the peak area of the characteristic ion mass chromatogram as the ordinate and the concentration of the matrix matching standard solution as the abscissa: Find the regression equation and correlation coefficient: 8:4:1 Liquid Chromatography Reference Conditions a) Chromatographic column: C₁s chromatographic column (150mm×2:1mm, 3:5 μm) or equivalent; b) Mobile phase: 0:1% formic acid solution-methanol (90:10, V/V); c) Flow rate: 0:2mL/min; d) Column temperature: 30℃; e) Injection volume: 10 μL: 8:4:2 Mass spectrometry reference conditions a) Ion source: electrospray (ESI) ion source; b) Scanning method: positive ion scanning; c) Detection method: multiple reaction monitoring (MRM); d) Capillary voltage: 3000 V; e) RF lens voltage: 0:5V; f) Ion source temperature: 150℃; g) Desolvation gas temperature: 350℃; h) Cone air flow rate: 50 L/h; i) Desolvation gas flow rate: 1000 L/h; j) Secondary collision gas: argon; k) Qualitative ion pairs, quantitative ion pairs, collision energy and cone voltage are shown in Table 1: 8:4:3 Determination method Take the sample solution and the corresponding matrix-matched standard solution for single-point or multi-point calibration, and quantify the chromatographic peak area according to the external standard method: The characteristic ion mass chromatographic peak areas of the matrix-matched standard solution and the target drug in the sample solution should be within the linear range of instrument detection: The retention time of ampropion in the sample solution is within ±2:5% of the retention time of amproline in the matrix-matched standard solution, and the relative ion abundance in the sample solution is consistent with the relative ion abundance in the matrix-matched standard solution: ratio, meeting the requirements of Table 2: Please see the attachment for the multiple reaction monitoring chromatogram of the standard solution: Record A: 8:5 Blank test Take a blank sample and perform parallel operations using the same measurement steps except that no standard solution is added:9 Calculation and presentation of resultsThe residual amount of ampropion in the sample is calculated according to the standard curve or formula (1): ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 31613.1-2021_English be delivered?Answer: Upon your order, we will start to translate GB 31613.1-2021_English as soon as possible, and keep you informed of the progress. The lead time is typically 2 ~ 4 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of GB 31613.1-2021_English with my colleagues?Answer: Yes. The purchased PDF of GB 31613.1-2021_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet.Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to Sales@ChineseStandard.net. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay. |
