GB 31658.18-2022 English PDFUS$199.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 31658.18-2022: (National Food Safety Standard - Determination of Triazine Residues in Animal Foods - High Performance Liquid Chromatography) Status: Valid
Basic dataStandard ID: GB 31658.18-2022 (GB31658.18-2022)Description (Translated English): (National Food Safety Standard - Determination of Triazine Residues in Animal Foods - High Performance Liquid Chromatography) Sector / Industry: National Standard Classification of Chinese Standard: X04 Word Count Estimation: 9,912 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 31658.18-2022: (National Food Safety Standard - Determination of Triazine Residues in Animal Foods - High Performance Liquid Chromatography)---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 Determination of triazine residues in food of animal origin HPLC 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 triazine residues in animal food by high performance liquid chromatography1 ScopeThis document specifies the sample preparation and high performance liquid chromatography detection methods for the detection of triazine residues in animal foods. This document is applicable to the detection of triazine residues in muscle, liver, kidney tissue, milk and goat milk of cattle and sheep.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 triazine in the sample was extracted with acetonitrile water (the residual triazine in milk was extracted with acetic acid acetonitrile solution), weak cation exchange solid phase extraction The column was purified, determined by high performance liquid chromatography-ultraviolet method, and quantified by external standard method.5 Reagents and materialsThe reagents used in the following 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 Methanol (CH3OH). chromatographically pure. 5.1.2 Formic acid (HCOOH). chromatographically pure. 5.1.3 Ammonium formate (CH5NO2). chromatographically pure. 5.1.4 Ammonia (NH3.H2O). 5.1.5 Glacial acetic acid (CH3COOH). 5.2 Solution preparation 5.2.1 60% acetonitrile solution. Take 60mL of acetonitrile, add 40mL of water, and mix well. 5.2.2 0.5% acetic acid in acetonitrile solution. Take 2.5 mL of glacial acetic acid, dilute to 500 mL with acetonitrile, and mix well. 5.2.3 5% ammonia solution. take 5mL of ammonia water, add 95mL of water, and mix well. 5.2.4 Acetic acid methanol solution (pH 7.0). Take 6 mL of glacial acetic acid, add 94 mL of methanol, mix well, adjust the pH to 7.0 ± 0.05 with ammonia water. 5.2.5 0.02mol/L ammonium formate solution (pH4.0). take 1.26g of ammonium formate, add 900mL of water to dissolve, adjust the pH to 4.0±0.0 with formic acid 0.05, dilute with water to 1000mL. 5.3 Standards Diacetamide triazine amidine (Diminazene acetic acid, C14H15N7.2C4H7NO3, CAS number. 908-54-3), content ≥ 91%. 5.4 Preparation of standard solution 5.4.1 Standard stock solution. Take an appropriate amount of diacetamide triazine standard (equivalent to about 10 mg of triazine), weigh it accurately, add water to dissolve and dilute to a 10mL brown volumetric flask, and prepare a standard stock solution of triazine with a concentration of 1mg/mL. Store in the dark at 4°C, and the validity period is 1 month. 5.4.2 Standard working solution. Accurately measure 1mL of 1mg/mL standard stock solution, put it in a 100mL brown volumetric flask, dilute with water to the mark, Prepare the triazine standard working solution with a concentration of 10 μg/mL, store it in the dark at 4°C, and have a validity period of 7 d. 5.5 Materials 5.5.1 Weak cation exchange solid phase extraction column. 60mg/3mL, or equivalent. 5.5.2 Microporous nylon filter membrane. 0.22 μm.6 Instruments and equipment6.1 High performance liquid chromatography. equipped with ultraviolet detector or diode array detector. 6.2 Analytical balance. Sensitivity 0.00001g and 0.01g. 6.3 pH meter. 6.4 Vortex mixer. 6.5 Vortex shaker. 6.6 High-speed refrigerated centrifuge. speed ≥ 10000r/min. 6.7 Solid phase extraction device.7 Preparation and storage of samples7.1 Preparation of samples 7.1.1 Organization Take an appropriate amount of fresh or thawed blank or test tissue, mince it, and homogenize it. 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 a standard solution of appropriate concentration, and add a sample as a blank. 7.1.2 Milk Take an appropriate amount of fresh or thawed blank or test milk sample, and mix well. a) Take the uniformly mixed test sample as the test sample; b) Take a uniformly mixed blank sample as a blank sample; c) Take a uniformly mixed blank sample, add a standard solution of appropriate concentration, and add a sample as a blank. 7.2 Storage of samples Store below -18°C.8 Measurement steps8.1 Extraction 8.1.1 Organization Take 2g of the sample (accurate to ±0.05g), put it in a 50mL polypropylene centrifuge tube, add 18mL of 60% acetonitrile solution, vortex for 1min, and store it on ice. Adjust the pH to 5.5±0.1 with acetic acid, shake for 10 min, centrifuge at 10,000 r/min for 5 min, take the supernatant, and dilute it with 60% acetonitrile solution to 20.0mL, mix well, take 2.0mL (muscle samples take 10.0mL), set aside. 8.1.2 milk Take 5g of the sample (accurate to ±0.05g), put it in a 50mL polypropylene centrifuge tube, add 10mL of 0.5% acetic acid acetonitrile solution accurately, vortex 1 min, shake for 10 min, centrifuge at 10000r/min for 10 min, remove all the supernatant, and set aside. 8.2 Purification Take a weak cation-exchange solid-phase extraction column, and activate it with 3mL of methanol and 3mL of water in turn. Take the spare liquid to pass through the column, and then dissolve it with 5% ammonia water in turn. Wash with 3 mL of methanol solution and 3 mL of methanol, drain, add 1.0 mL of acetic acid methanol solution (pH 7.0), elute, drain, collect eluate, pass through microporous nylon filter membrane for determination by high performance liquid chromatography. 8.3 Preparation of standard curve Precisely measure an appropriate amount of standard working solution, dilute it with acetic acid-methanol solution (pH 7.0), and prepare a concentration of 0.05 μg/mL, 0.1 μg/mL, 0.2μg/mL, 0.5μg/mL, 1μg/mL, 2μg/mL, 5μg/mL series of standard solutions, passed through microporous nylon filter membrane, for HPLC Chromatographic determination. With triazine chromatographic peak area as the ordinate and standard solution concentration as the abscissa, draw a standard curve. Find the regression equation and correlation coefficient. 8.4 Determination 8.4.1 Reference conditions for liquid chromatography a) Chromatographic column. C18 column (250mm×4.6mm, particle size 5μm), or equivalent; b) Mobile phase. A is 0.02mol/L ammonium formate solution (pH4.0); B is methanol; c) Gradient elution. see Table 1 for elution conditions; d) Column temperature. 30°C; e) Injection volume. 20 μL; f) Detection wavelength. 370nm. 8.4.2 Determination method Take the sample solution and the corresponding standard solution for single-point or standard curve calibration, and calculate the peak area according to the external standard method. Standard working solution and sample The response value of triazine in the solution should be within the linear range of instrument detection. The retention time of triazine in the test sample and the retention time of triazine in the standard solution The relative deviation of the retention time should be within ±2.5%. The chromatogram of the standard solution is shown in Appendix A. 8.5 Blank test Take the blank sample, except that no drug is added, the exact same determination steps are used for determination.9 Calculation and presentation of resultsThe content of the analyte in the sample is represented by the mass fraction X, and the unit is milligrams per kilogram (mg/kg), calculated according to formula (1). 10 Detection method sensitivity, accuracy and precision 10.1 Sensitivity The detection limit of this method in beef and mutton is 0.05 mg/kg, and the limit of quantification is 0.1 mg/kg. In bovine liver, bovine kidney, goat liver and goat kidney The limit of detection was 0.2 mg/kg, the limit of quantification was 0.5 mg/kg, the limit of detection in cow and goat milk was 0.01 mg/kg, the limit of quantification was 0.02mg/kg. 10.2 Accuracy This method is effective in beef and mutton 0.1mg/kg~1mg/kg, beef liver and sheep liver 0.5mg/kg~24mg/kg, beef kidney and sheep kidney 0.02mg/kg~0.3mg/kg for cow's milk and goat's milk, the recoveries were 60%~110%. 10.3 Precision In this method, the relative standard deviation within the batch was ≤10%, and the relative standard deviation between batches was ≤10%. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 31658.18-2022_English be delivered?Answer: Upon your order, we will start to translate GB 31658.18-2022_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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