GB 31658.19-2022 English PDFUS$199.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 31658.19-2022: (National Food Safety Standard Determination of Atropine, Scopolamine, Anisodamine, Lidocaine, and Procaine Residues in Animal Foods-Liquid Chromatography-Tandem Mass Spectrometry) Status: Valid
Basic dataStandard ID: GB 31658.19-2022 (GB31658.19-2022)Description (Translated English): (National Food Safety Standard Determination of Atropine, Scopolamine, Anisodamine, Lidocaine, and Procaine Residues in Animal Foods-Liquid Chromatography-Tandem Mass Spectrometry) Sector / Industry: National Standard Classification of Chinese Standard: X04 Word Count Estimation: 10,124 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 31658.19-2022: (National Food Safety Standard Determination of Atropine, Scopolamine, Anisodamine, Lidocaine, and Procaine 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 Health Commission of the People's Republic of China National Food Safety Standards Atropine, scopolamine, anisodamine, Determination of Lidocaine and Procaine Residues 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 Atropine, scopolamine, anisodamine, lidocaine, procaine in animal food Determination of residues by liquid chromatography-tandem mass spectrometry1 ScopeThis document specifies the sample preparation and solutions for the detection of atropine, scopolamine, anisodamine, lidocaine, and procaine residues in animal foods. Phase chromatography-tandem mass spectrometry detection method. This document applies to atropine, scopolamine, anisodamine, lidocaine, and procaine in muscle, liver, kidney, and fat of pigs, cattle, and sheep Determination of single or multiple drug residues.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 analyte remaining in the sample was extracted by phosphate buffer solution, purified by PEP-2 solid phase extraction column, determined by liquid chromatography-tandem mass spectrometry, and external standard method. Quantitative.5 Reagents and materialsUnless otherwise specified, all reagents are of analytical grade, and the water is first-class water in accordance 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 Potassium dihydrogen phosphate (KH2PO4). 5.1.5 Dipotassium hydrogen phosphate (K2HPO4.3H2O). 5.1.6 phosphoric acid (H3PO4). 5.2 Solution preparation 5.2.11 0.1mol/L Potassium dihydrogen phosphate buffer solution. Take 13.6g of potassium dihydrogen phosphate, add 900mL of water to dissolve, adjust the pH to 4.0±0.05, dilute with water to 1000mL, and mix well. 5.2.2 0.2mol/L dipotassium hydrogen phosphate solution. Take 22.8g of dipotassium hydrogen phosphate, add water to dissolve and dilute to 500mL, and mix well. 5.2.3 5% methanol solution. Take 5mL of methanol, add water to dilute to 100mL, and mix well. 5.2.4 30% acetonitrile solution. take 30mL of acetonitrile, add water to dilute to 100mL, and mix well. 5.2.5 0.1% formic acid solution. take 0.5mL of formic acid, add water to dilute to 500mL, and mix well. 5.3 Standards Atropine (Atropine, C17H23NO3, CAS number. 51-55-8), scopolamine (Scopolamine, C17H21NO4, CAS number. 51- 34-3), anisodamine (Anisodamine, C17H23NO4, CAS number. 55869-99-3), lidocaine (Lidocaine C14H22N2O, CAS No.. 137-58-6), procaine (Procaine, C13H20N2O2, CAS No.. 59-46-1), the content is ≥99%. The standard can also be the corresponding salt. 5.4 Preparation of standard solution 5.4.1 Standard stock solution. Take the appropriate amount of atropine, scopolamine, anisodamine, lidocaine and procaine About 10 mg), accurately weighed, add methanol to dissolve and dilute to 10 mL volumetric flask, and prepare a standard concentration of 1 mg/mL Stock solution. Stored at -18°C in the dark, valid for 6 months. 5.4.2 Mixed standard intermediate solution. Accurately measure 1mL of each standard stock solution, put it in a 100mL volumetric flask, dilute it to the mark with methanol, and prepare The mixed standard working solution with a concentration of 10 μg/mL was stored at -18°C in the dark, and the validity period was 1 month. 5.4.3 series of standard working solutions. accurately measure an appropriate amount of mixed standard intermediate solution, dilute with 30% acetonitrile solution, and prepare the concentrations of 1ng/mL, 2ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 50ng/mL and 100ng/mL series of standard solutions. Ready to prepare Now in use. 5.5 Materials 1) The PEP-2 solid-phase extraction column listed here is for reference only and does not involve commercial purposes. Standard users are encouraged to try to use different manufacturers or models of solid-phase extraction columns. 5.5.1 PEP-2 solid phase extraction column 1). The filler is functionalized polystyrene/divinylbenzene, 60mg/3mL, or equivalent. 5.5.2 Microporous nylon filter membrane. 0.22 μm.6 Instruments and equipment6.1 Liquid chromatography-tandem mass spectrometer. with electrospray ion source. 6.2 Analytical balance. Sensitivity 0.01g and 0.00001g. 6.3 Vortex mixer. 6.4 Vortex shaker. 6.5 High-speed refrigerated centrifuge. the speed can reach 10000r/min. 6.6 Solid phase extraction device. 6.7 Tissue homogenizer. 6.8 pH meter.7 Preparation and storage of samples7.1 Preparation of samples Take an appropriate amount of fresh or thawed blank or test tissue, mince it, and make it homogeneous. 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 a standard solution of appropriate concentration, and add the sample as a blank. 7.2 Storage of samples Store below -18°C.8 Measurement steps8.1 Extraction Take 2 g of the test material (accurate to ±0.05 g) into a 50 mL centrifuge tube, and add 20 mL of 0.1 mol/L potassium dihydrogen phosphate buffer solution accurately. (fat samples were heated in a 60°C water bath for 10min), vortexed for 1min, shaken for 10min, and centrifuged at 10000r/min for 10min at 4°C. Take 10 mL of supernatant to another centrifuge tube, add 5 mL of 0.2 mol/L dipotassium hydrogen phosphate solution, mix well and set aside. If the solution is turbid, Centrifuge at 10000r/min for 10min, and take the supernatant for later use. 8.2 Purification The PEP-2 solid-phase extraction column was activated with methanol 3mL and water 3mL respectively, all the spare liquid was pipetted, passed through the column, water 3mL, 5% methanol solution Rinse with 3mL, drain, and accurately pipette 2mL of 30% acetonitrile solution for eluting, drain, collect the eluate, pass through a microporous nylon filter membrane, and use it for liquid chromatography-series Combined mass spectrometry. 8.3 Preparation of matrix-matched standard curve Accurately pipette 100 μL each of the series of standard working solutions, dilute to 1 mL with the eluent of the blank sample after processing in steps 8.1-8.2, and prepare A series of matrices with concentrations of 0.1ng/mL, 0.2ng/mL, 0.5ng/mL, 1ng/mL, 2ng/mL, 5ng/mL and 10ng/mL were prepared Match the standard solution and pass through the microporous nylon filter membrane for liquid chromatography-tandem mass spectrometry. The matrix matching standard solution concentration is the abscissa, the matrix matching standard curve is drawn, and the regression equation and correlation coefficient are calculated. 8.4 Determination 8.4.1 Reference conditions for liquid chromatography a) Chromatographic column. C18 chromatographic column (100mm×2.1mm, 1.7μm), or equivalent; b) Column temperature. 35°C; c) Injection volume. 2 μL; d) Flow rate. 0.3mL/min; e) Mobile phase. A is 0.1% formic acid solution; B is methanol. The gradient elution program is shown in Table 1. 8.4.2 Reference conditions for mass spectrometry a) Ion source. electrospray ion source; b) Scanning mode. positive ion scanning; c) Detection method. multiple reaction monitoring; d) Spray voltage. 1.0kV; e) Sheath gas. 30Arb; f) Auxiliary gas. 5Arb; g) Ion transfer tube temperature. 325°C; h) Atomization temperature. 300°C; i) Refer to Table 2 for the reference values of retention time, qualitative ion pair, quantitative ion pair, cone voltage and collision energy of the drug to be tested. 8.4.3.1 Qualitative determination Under the same test conditions, the retention time of the drug peak of the analyte in the test solution was similar to that of the corresponding peak in the matrix-matched standard solution. The deviation is within ±2.5%, and the detected relative ion abundance should be equal to the relative ion abundance of the matrix matching standard solution with the same concentration. The allowable deviation should meet the requirements of Table 3. 8.4.3.2 Quantitative determination Take the sample solution and the corresponding matrix-matched standard solution for single-point or multi-point calibration, and use the external standard method to quantify the chromatographic peak area. Matrix-matched The response values of the analytes in the standard working solution and the sample solution should be within the linear range of the instrument detection. See Appendix A for the characteristic ion mass chromatograms prepared with standard solutions. 8.5 Blank test The blank sample was taken, except that no drug was added, and the same determination steps were used for determination.9 Calculation and presentation of resultsThe residual amount of the analyte in the sample is calculated according to the standard curve or formula (1). 10 Detection method sensitivity, accuracy and precision 10.1 Sensitivity The detection limit of this method in the muscle and adipose tissue of pigs, cattle, and sheep was 0.2 μg/kg, and the limit of quantification was 0.5 μg/kg; in the kidneys of pigs, cattle, and sheep The limit of detection in liver and liver tissues was 0.5 μg/kg, and the limit of quantification was 1.0 μg/kg. 10.2 Accuracy The recovery rate of this method at the concentration level of 0.5 μg/kg~5 μg/kg in muscle and adipose tissue of pigs, cattle and sheep is 60%~ 120%; the recovery rate was 60%~120% at the concentration level of 1.0μg/kg~10μg/kg in the kidney and liver tissues of pigs, cattle, and sheep. 10.3 Precision In this method, the relative standard deviation within the batch was ≤15%, and the relative standard deviation between batches was ≤15%. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 31658.19-2022_English be delivered?Answer: Upon your order, we will start to translate GB 31658.19-2022_English as soon as possible, and keep you informed of the progress. 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