GB 23200.36-2016 English PDFUS$219.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.36-2016: Food safety national standard -- Determination of chloroplopidic acid, fenpropathrin, furazolidone and thiazole niacin herbicide residues in plant-derived foods by liquid chromatography-mass spectrometry / mass spectrometry Status: Valid
Basic dataStandard ID: GB 23200.36-2016 (GB23200.36-2016)Description (Translated English): Food safety national standard -- Determination of chloroplopidic acid, fenpropathrin, furazolidone and thiazole niacin herbicide residues in plant-derived foods by liquid chromatography-mass spectrometry / mass spectrometry Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 11,181 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): SN/T 2214-2008 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.36-2016: Food safety national standard -- Determination of chloroplopidic acid, fenpropathrin, furazolidone and thiazole niacin herbicide residues in plant-derived foods 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 chloroplopidic acid, fenpropathrin, furazolidone and thiazole niacin herbicide residues in plant-derived foods by liquid chromatography-mass spectrometry/mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 2214-2008 National standards for food safety Plant-derived food chlorofluoropyoxyacetic acid, fenpropathrin, Determination of vanillin hydrazone and thiazole niacin herbicide residues Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of fluroxypyr, dithiopyr, diflufenzopyr and thiazopyr Residues in plant-derived foods Liquid chromatography - mass spectrometry 2016-12-18 Release.2017-06-18 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 ForewordThis standard replaces SN/T 2214-2008 "Flavonoids, Fluorothiocuronide, Fipronil and Hydrazone Herbicides in Import and Export Plant Foods Determination of Residue by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry ". Compared with SN/T 2214-2008, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name of the "import and export of plant-derived food" to "plant-derived food"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 2214-2008. National standards for food safety Flavulanic acid, fenpropathrin, furazolidone and thiazole niacin in plant-derived food Determination of residual residue by liquid chromatography - mass spectrometry/mass spectrometry1 ScopeThis standard specifies the chlorpyrifluoroacetic acid, fenpropathrin, fluphenhydrazone and thiazole nicotinic acid in the plant source food. Determination of Chromatography - Mass Spectrometry/Mass Spectrometry. This standard applies to cabbage, corn and oranges in the chlorofluoropyoxyacetic acid, fenpropathrin, fenugreeosone and thiazole nicotinic acid four kinds of pyridine Determination and determination of herbicide residues, other food can refer 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 article Pieces. 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 principleThe residual chlorofluoropyoxyacetic acid in the sample, fenpropathrin, furazolidone and thiazole niacin were extracted with acetonitrile and purified by Supelclean C18 solid Phase extraction column, with liquid chromatography - mass spectrometry/mass spectrometry detection and confirmation, external standard method quantitative.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). Chromatographically pure. 4.1.2 Methanol (CH3OH). Chromatographic Purification. 4.1.3 Formic acid (HCOOH). Chromatographic pure. 4.1.4 Sodium chloride (NaCl). 4.2 solution preparation 4.2.1 0.1% formic acid in water solution. Accurately absorb 1 mL of formic acid, transfer into a 1 000 mL volumetric flask, set the volume to the mark with water, mix Evenly. 4.2.2 0.1% formic acid - methanol (50 50, V/V). Take 0.1% formic acid as an aqueous solution 500 mL to 1 000 mL volumetric flask. Methanol constant volume to the scale, mixed evenly. 4.3 standards 4.3.1 Pyridine Herbicides Standard. See Appendix A. 4.4 standard solution preparation 4.4.1 standard reserve solution. accurately weighed the appropriate amount of chlorofluorophenoxy acetic acid, fenpropathrin, thiazole nicotinic acid were dissolved with methanol and volume to Brown volumetric flask, the concentration is equivalent to 500 mg/L, the stock solution can be stored at 0 ℃ ~ 4 ℃ dark for 6 months. 4.4.2 mixed standard intermediate solution. accurate absorption of the appropriate amount of chlorofluoropyoxy acetic acid, fenpropathrin, thiazole niacin standard reserve solution in brown capacity And the addition of other pyridine herbicides and other concentrations of picarbazone hydrazone, with a fixed volume of methanol to the scale, a variety of pyridine herbicides Concentration of 1 mg/L, the intermediate solution can be stored at 0 ℃ ~ 4 ℃ dark for 1 month. 4.4.3 mixed standard working solution. according to need, before use to absorb a certain amount of mixed standard intermediate solution, with a blank sample matrix solution Preparation. 4.5 Materials 4.5.1 Solid phase extraction column. Supelclean C18,500 mg/3 mL, or equivalent. Before use with 5 mL acetonitrile treatment, keep the column wet Run. 4.5.2 Microporous membrane. 0.22 μm, organic phase type.5 instruments and equipment5.1 Liquid Chromatography - Mass Spectrometry/Mass Spectrometer with ESI Ion Source. 5.2 Balance. 0.0001 g and 0.01 g. 5.3 Crusher. 5.4 Polypropylene centrifuge tube. 15 mL and 50 mL, with plug. 5.5 Centrifuge. 5 000 r/min. 5.6 Scroll Mixer. 5.7 blowing nitrogen enrichment instrument. 5.8 solid phase extraction device.6 Preparation and storage of samples6.1 Preparation of the sample 6.1.1 Chinese cabbage and oranges Take about 500 g of the sample, (not water wash). After shredding, the sample is processed into a slurry, mixed, Sealed, marked and marked. 6.1.2 Corn Replace the sample about 500 g, fully crushed, mix, into a clean container, sealed and marked. 6.2 Sample storage Samples were stored at 0 ° C and 4 ° C. During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 7. Determination steps 7.1 Extraction Weigh 5 g (accurate to 0.01 g) sample in a 50 mL centrifuge tube and add proper amount of deionized water for a while. 10 mL of acetonitrile was added, Mix on a vortex mixer for 3 min, centrifuge at 5000 r/min for 5 min, transfer the supernatant to another centrifuge tube. Respectively, with 10 mL, 5 mL of acetonitrile Repeat the above extraction process and combine the extracts. Add appropriate amount of sodium chloride, full oscillation, centrifugation in 5000 for 3 min. Take 5 mL of the upper layer Acetonitrile extract to 15 mL centrifuge tube, at 40 ℃ blowing nitrogen concentrated to about 2 mL, fully mixed. 7.2 Purification The sample extract was transferred to a C18 solid phase extraction column. Eluting with 4 mL of acetonitrile and collecting the entire effluent (approximately 6 mL) from the sample The solid phase extraction purification process controls the flow rate to no more than 1 d/s. The effluent was blown to near dryness at 40 ° C with 0.1% formic acid-methanol (50 50, V/V) to 1.0 mL, and the mixture was vortexed and passed through a 0.22 μm microporous membrane for liquid chromatography-mass spectrometry/mass spectrometry. 7.3 Determination 7.3.1 Liquid Chromatography Chromatographic Reference Conditions A) Column. ACQUITY BEH C18 column, 50 x 2.1 mm (inner diameter), 1.7 μm, or equivalent. B) Column temperature. 40 ° C. C) Flow rate. 0.3 mL/min. D) Injection volume. 20 μL. E) Flow phase and gradient elution conditions are shown in Table 1. Table 1 Mobile phase and gradient elution conditions time Min Flow rate ML/min 0.1% formic acid in water Methanol 0 0.3 80 20 6 0.3 0 100 7.5 0.3 80 20 7.3.2 Mass spectrometry reference conditions A) Ionization mode. electrospray ionization positive ion mode (ESI). B) Resolution. Unit mass resolution. C) Capillary voltage (kv). 3.00. D) Source temperature (° C). 105. E) Desolvation gas temperature (° C). 350 ° C. F) Desolvent gas flow rate (L/hr). 750. G) Monitoring mode. Multiple reaction monitoring (MRM), see Appendix A Table A.1 for setting conditions. 7.3.3 Determination and confirmation of chromatography According to the above conditions to determine the sample and mixed matrix standard solution, the sample retention time of the material to be tested and the substrate standard solution retention And the relative abundance of the qualitative ion pair is consistent with the relative abundance of the standard solution of the mixed matrix equivalent to the concentration. Degree deviation does not exceed the provisions of Table 2, you can determine the existence of the corresponding sample in the sample. In the best working conditions of the instrument, the standard solution of the mixed working solution of the matrix, with the peak area as the ordinate, the matrix mixed working solution concentration The standard working curve is drawn for the abscissa, and the sample is quantified by the standard working curve. The response value of the sample to be measured in the sample solution should be Determination of the linear range. Under the above liquid chromatography-mass/mass spectrometry conditions, chlorofluorophenoxyacetic acid, fluphenhydrazone, fenpropathrin and thiazole The retention time of nicotinic acid is given in Appendix A, Table A.1. Total Ion Flow Chromatography and Multiple Reaction Monitoring (MRM) of Four Pyridine Herbicides Reference Materials See Appendix B, Figure B.1 and Figure B.2 for chromatograms. Table 2 The maximum allowable deviation of relative ion abundance when qualitative confirmation Relative ion abundance > 50% > 20% to 50% > 10% to 20% ≦ 10% Maximum permissible deviation ± 20% ± 25% ± 30% ± 50% 7.4 blank experiment In addition to the sample, according to the above determination steps.8 results are calculated and expressedThe contents of the four pyridine herbicides in the sample were calculated according to the following formula (1). MΑs VCsA (1) Where. The content of four pyridine herbicides in the X - sample, in micrograms per kilogram, μg/kg; The peak area of pyridine herbicide in A - sample solution; As - standard working solution of pyridine herbicides peak area; Cs - four pyridine herbicides from standard working curves in micrograms per liter, μg/L; V - the final volume of the sample solution, in milliliters, mL; M - the final sample quality of the sample, 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 limits of quantification of Chinese cabbage and orange substrate. chlorofluoropyoxyacetic acid, fenpropathrin, fluphenazine and thiazole nicotinic acid were 5 μg/kg; The limit of quantification of corn matrix. chlorofluoropyoxyacetic acid and fluphenhydrazone is 10 μg/kg, and the limit of quantification of fenpropathrin and thiazole nicotinate is 5 Μg/kg. 10.2 Recovery rate In the range of 0.005 mg/kg to 0.04 mg/kg, the recovery rates of the four pyridine herbicides are given in Appendix C.Appendix A(Informative) Basic information, retention time and mass spectrometry parameters of four pyridine herbicides Table A.1 Basic information, retention time and mass spectral parameters of four pyridine herbicides Pesticide Chinese name Pesticide English name CAS number Molecular formula Molecular weight Reserved time Min Mother ion M/z Ion M/z Retention time Cone hole voltage Collision energy EV Chlorofluorophenoxy Acetic acid Fluroxypyr C7H5Cl2FN2O3 69377-81-7 255.03 2.85 255 209 * 0.2 30 15 181 0.2 30 20 2 Fluoropyrazone diflufenzopyr C15H12F2N4O3 109293-97-2 334.28 3.50 335 206 * 0.2 30 15 162 0.2 30 15 3 Fisulfuride dithiopyr C15H16F5NO2S2 97886-45-8 401.41 5.25 402 354 * 0.05 30 18 272 0.05 30 30 4 thiazole niacin thiazopyr C16H17F5N2O2S 117718-60-2 396.37 4.81 397 377 * 0.2 30 21 335 0.2 30 29 Note. * Quantitative detection of ions. For different mass spectrometry instruments, there may be differences in instrument parameters, and the mass spectrometry parameters should be optimized to the best.Appendix B(Informative) The total ion chromatogram of the standard and the multi - reaction monitoring (MRM) chromatogram Figure B.2 5 μg/L pyridine herbicide standard multi-reaction monitoring (MRM) chromatogram Figure B.1 5 μg/L pyridine herbicide standard total ion chromatogram 1. chlorofluoropyoxyacetic acid; 2. fluphenhydrazone; 3. thiazole niacin; 4. fenpropathrin. Chlorofluorophenoxyacetate Thiazole nicotinic acid thiazole niacin Fluoride Sulfonated FenpropathrinAppendix C(Informative) Addition Recovery of Four Pyridine Herbicides in Different Substrates Table C.1 Recovery rates of four pyridine herbicides in different matrices No. pesticide name Sample matrix Cabbage oranges Chlorofluorophenoxy Acetic acid 89.4% ~ 117.8% 86.4% ~ 119.4% 63.5% ~ 117.5% 2 Fluoropyrazine 79.8% ~ 120.0% 71.4% ~ 112.2% 65.7% ~ 122.3% 3 Fisulfurism 60.5% ~ 94.0% 78.4% ~ 115.7% 76.7% ~ 118.0% 4 thiazole niacin 98.0% ~ 112.0% 80.4% ~ 103.0% 84.6% ~ 111.0%Appendix D(Normative appendix) Laboratory repeatability requirements Table 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 23200.36-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.36-2016_English as soon as possible, and keep you informed of the progress. 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