GB 23200.70-2016 English PDFUS$219.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.70-2016: Food safety national standard -- Determination of Trifluorocarbazone Residue in Food by Liquid Chromatography-mass spectrometry / Mass Spectrometry Status: Valid
Basic dataStandard ID: GB 23200.70-2016 (GB23200.70-2016)Description (Translated English): Food safety national standard -- Determination of Trifluorocarbazone Residue in Food by Liquid Chromatography-mass spectrometry / Mass Spectrometry Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 11,119 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): SN/T 2807-2011 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of 2016 Issuing agency(ies): National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration GB 23200.70-2016: Food safety national standard -- Determination of Trifluorocarbazone Residue in Food by Liquid Chromatography-mass spectrometry / 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. Food safety national standard - Determination of Trifluorocarbazone Residue in Food by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry ICS case number. National Standards of People's Republic of China GB National standards for food safety Determination of Trifluorocarbazone Residue in Food Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of acifluorfen residue in foods Liquid chromatography - mass spectrometry ×××× - ×× - ×× Release ×××× - ×× - ×× Implementation National Health and Family Planning Commission of the People 's Republic of China Issued by the Ministry of Agriculture of the People 's Republic of China State Administration of Food and Drug Administration 2016-12-18 Release.2017-06-18 Implementation Instead of SN/T 2807-2011 ForewordThis standard replaces SN/T 2807-2011 "Determination of Trifluorocarbazone Residue in Import and Export Foodstuffs in Import and Export Foods - Liquid Chromatography Spectrum/mass spectrometry ". Compared with SN/T 2807-2011, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name and scope of the "import and export food" to "food"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 2807-2011. National standards for food safety Determination of Trifluorocarbazone Residue in Food by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry1 ScopeThis standard specifies the method for the determination of triflate residues in food by liquid chromatography-mass spectrometry/mass spectrometry. This standard applies to soybean, rice, brown rice, soybeans, apples and pork in the determination of triflate residues. Other food can participate According to the implementation.2 normative reference documentsThe following documents are indispensable for the application of this document. For dated references, only the dated edition applies to this file. For undated references, the latest edition (including all modifications) applies to this document. GB 2763 National Standard for Food Safety - Maximum Residue Limit of Pesticides in Foodstuffs GB/T 6682 Analytical laboratory water specifications and test methods3 principleSoy, rice and brown rice samples were soaked in water and extracted with acetonitrile. Other samples were extracted directly with acetonitrile and then washed The extract was purified by liquid-liquid distribution and solid-phase extraction. The liquid was purified by liquid chromatography-mass spectrometry and mass spectrometry.4 reagents and materialsUnless otherwise specified, all reagents are of analytical grade and water is in accordance with the primary water specified in GB/T 6682. 4.1 Reagents 4.1.1 acetonitrile (CH3CN). high performance liquid chromatography grade. 4.1.2 Methanol (CH3OH). High performance liquid chromatography grade. 4.1.3 Formic acid (HCOOH). 4.1.4 Sodium chloride (NaCl). 4.1.5 anhydrous sodium sulfate (Na2SO4). before burning at 650 ℃ for 4 hours, stored in a dryer, cooling and standby. 4.2 solution preparation 4.2.1 Formic acid - acetonitrile solution. 0.5 mL of formic acid was added to 500 mL of acetonitrile and shaken for standby. 4.2.2 Formic acid - aqueous solution. 1.0 mL of formic acid was added to 1000 mL of water and shaken. 4.2.3 constant solution solution. (formic acid - aqueous solution) - acetonitrile (19, V/V) 4.2.4 n-Hexane. add appropriate amount of acetonitrile and shake well before use. 4.3 standards 4.3.1 Reference substance. trifluorocarbamate (CAS. 50594-66-6), purity ≥99%. 4.4 standard solution preparation 4.4.1 Standard stock solution. accurately weighed the appropriate standard (accurate to 0.1 mg), dissolved in methanol, prepared into a concentration of 100 μg/mL Of the standard stock solution, -18 ℃ below the frozen light preservation, valid for 3 months. 4.4.2 standard intermediate solution. accurate removal of 1 mL standard stock solution in 10 mL volumetric flask, with constant volume solution to the volume, prepared into Concentration of 10 μg/mL standard intermediate solution, 0 ℃ ~ 4 ℃ cold storage, valid for 1 month. 4.5 Materials 4.5.1 solid phase extraction column. carbon eighteen column, 3 mL, or equivalent, before use with 10 mL formic acid - acetonitrile solution pre-leaching. 4.5.2 Microporous membrane. 0.20 μm, organic phase type. 4.5.3 Nitrogen. Purity ≥99.999%.5 instruments and equipment5.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer. Equipped with an electrospray ion source (ESI). 5.2 Sample grinder. with 20 mesh sample sieve. 5.3 Analysis of balance. 0.01 g and 0.0001 g. 5.4 plastic centrifuge tube. 50 mL, with plug. 5.5 Oscillator. 5.6 Centrifuge. 5.7 Rotating Concentrator. 5.8 nitrogen blowing instrument. 5.9 Scroll Mixer.6 Preparation and storage of samples6.1 Soy, rice and brown rice samples 500 g of the sample was taken and pulverized with a pulverizer and passed through a 20 mesh sample. Mix well and fit into a clean container Inside, sealed and identified, in 0 ℃ ~ 4 ℃ dark preservation. 6.2 Soybeans, apples and pork 500 g of the sample was taken, crushed and mixed evenly with a pulverizer, filled in a clean container, sealed and identified, and cooled at -18 ° C Frozen light preservation. During sample and sample preparation, the sample should be protected from contamination or changes in the residue content. Note. The above sample sampling site according to GB 2763 Appendix A implementation.7 Analysis steps7.1 Extraction Weigh the sample 5 g (accurate to 0.01 g) and place it in a 50 mL stoppered plastic centrifuge tube. For soy, rice and brown rice samples, join 10 mL of water, vortex mixed for 30 min after adding 20 mL of acetonitrile; for soybeans, apples and pork samples, add 20 mL Acetonitrile. After 30 min of shaking and centrifuged at 4 000 r/min for 3 min, the supernatant was transferred to another 50 mL stoppered plastic centrifuge tube, The residue was extracted once again with 15 mL of acetonitrile and the supernatant was combined. To the supernatant was added 3 g of sodium chloride and the mixture was vortexed at 4 000 r/min After centrifugation for 1 min, the upper layer solution was transferred to a separatory funnel. Then add 15 mL of acetonitrile repeated extraction time, combined with the upper solution, to be purified. 7.2 Purification 7.2.1 Liquid-liquid distribution purification 20 mL of n-hexane was added to the solution to be purified and allowed to stand for 5 min. The lower layer of the solution was passed through an anhydrous sodium sulfate funnel and collected Shrink bottle. In 40 ℃ below the water bath spin concentrated to near dry, and then dry with nitrogen. The residue was dissolved in 1 mL of formic acid-acetonitrile solution. 7.2.2 solid phase extraction purification The effluent was collected while the formic acid-acetonitrile solution was transferred to the ENVI-18 solid phase extraction column. And then with 5 mL of formic acid-acetonitrile solution Elute all the effluent. The whole solid phase extraction purification process controls the flow rate not to exceed 2 mL/min. The effluent is used below 40 ° C Nitrogen blown dry. The residue was dissolved in 1.0 mL constant solution and the mixture was vortexed and passed through a 0.2 μm microporous membrane for instrumentation. 7.2.3 Preparation of matrix standard working solution Weigh five blank samples and follow the 7.1 steps. In step 7.2, a volume of standard solution is removed and added to each Purified effluent by solid phase extraction, the rest of the steps with 7.2. Matrix standard working solution should be used with the current distribution. 7.3 Determination 7.3.1 Liquid Chromatographic Reference Conditions A) Column. C18,150 mm × 2.1 mm (id), 5 μm, or equivalent. B) Column temperature. 40 ° C. C) Flow rate. 0.2 mL/min. D) Injection volume. 10 μL. E) Mobile phase. acetonitrile. formic acid - water (%) (90 10, volume ratio) 7.3.2 Mass spectrometry reference conditions See Table A.1 and Table A.2. 7.3.3 Qualitative determination The sample and matrix standard solutions were determined according to the above conditions if the mass retention time of the sample was compared with that of the mixed matrix standard solution The relative abundance of the qualitative ion pair is consistent with the relative abundance of the matrix standard solution corresponding to the concentration, and the relative abundance deviation does not exceed the table 1, you can determine the existence of the corresponding sample in the sample. Table 1 Maximum allowable deviation of relative ion abundance at qualitative determination Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% 7.3.4 Quantitative determination According to the external standard method for quantitative calculation. According to the concentration from small to large order, followed by analysis of matrix standard working solution, the concentration and peak Product of the work curve. The response value of the analyte in the sample solution should be within the working curve. Under the above liquid chromatography-mass/mass spectrometry conditions, The retention time of the triflate was 2.3 min. Mass Spectrometer/Mass Spectrometry Multi-Reaction Monitoring (MRM) Chromatogram Particle Mass Spectrometry See Appendix B.8 results calculatedThe residual content of the analyte in the sample shall be calculated according to equation (1) or by a data processor using a detection instrument. Vc (1) Where. The content of the analyte in the X-sample, in milligrams per kilogram, mg/kg; C - the content of the analyte in the sample solution obtained from the matrix standard curve, in ng/ml for ng/mL; V - the final volume of the sample solution, in milliliters, mL; M-the final sample of the sample quality, in grams, g. Note. The result of the calculation shall be deducted from the blank value. The result of the measurement shall be expressed as the arithmetic mean of the parallel measurement, and two valid digits shall be retained.9 precision9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with Appendix D requirements. 9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with Appendix E requirements. 10% limit and recovery rate 10.1 Quantitation limits The quantification limit of the method is 352 mg/kg. 10.2 Recovery rate When the levels were 0.002 mg/kg, 0.004 mg/kg, 0.02 mg/kg, 0.1 mg/kg, the addition recovery of trifluorocarbamate See Appendix C.Appendix A(Informative) Table A.1 Mass spectrometry conditions Ion source ESI- Capillary voltage of 4.0 kV Drying gas temperature 350 ℃ The atomizer pressure is 40 psi Dry gas flow rate nitrogen, flow rate 8 L/min Collision gas nitrogen Scanning mode Anion scanning Monitoring Multiple Response Monitoring (MRM) Table A.2 Multi-reaction monitoring conditions Chinese name ion ion ion residence time fragmentation voltage collision energy Trifluorocarbamate 360.1 316.1 * 0.20 s 80 V 3 eV 286.1 0.20 s 80 V 10 eV Note. Add "*" ions for quantitation. 1) Non-commercial statement. Appendix A The parameters listed in Table A are done on the Agilent 6410 QQQ mass spectrometer. The test instrument model is listed here only for Provide reference, does not involve commercial purposes, to encourage standard users to try to use different manufacturers or models of equipment.Appendix B(Informative) Multi - reaction monitoring mass chromatogram Figure B.1 Standard Multi-Reaction Monitoring Quality ChromatogramAppendix C(Informative) Add concentration and recovery range Table C.1 Add concentration and recovery range sample name Add concentration Mg/kg Recovery rate range Soybeans 0.002 81.1 to 91.8 0.004 80.4 to 97.3 0.02 81.4 to 97.1 0.1 84.4 ~ 98.0 Rice 0.002 80.1 to 94.2 0.004 81.0 to 97.5 0.02 81.0 to 95.3 0.1 84.1 to 97.3 brown rice 0.002 82.8 ~ 94.2 0.004 80.1 to 97.3 0.02 80.1 to 96.7 0.1 85.3 ~ 97.1 Soybeans 0.002 84.3 ~ 92.7 0.004 80.5 to 94.7 0.02 81.8 ~ 94.9 0.1 86.2 to 96.6 apple 0.002 80.7 to 95.0 0.004 80.7 to 96.5 0.02 81.8 to 96.2 0.1 86.1 to 96.1 pork 0.002 80.7 to 94.6 0.004 84.6 to 97.0 0.02 84.6 ~ 96.0 0.1 85.9 to 97.5Appendix D(Normative appendix) Laboratory repeatability requirements D.1 Laboratory repeatability requirements Measured component content Mg/kg Precision 0.001 36 > 0.01 > 1 14Appendix E(Normative appendix) Inter-laboratory reproducibility requirements Table E.1 Inter-laboratory reproducibility requirements Measured component content Mg/kg Precision 0.001 54 > 0.01 > 1 19 ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 23200.70-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.70-2016_English as soon as possible, and keep you informed of the progress. 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