GB 23200.91-2016 English PDFUS$179.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.91-2016: Food safety national standard -- Determination of 9 organophosphorus pesticide residues in animal-derived foods -- Gas chromatographic method Status: Valid
Basic dataStandard ID: GB 23200.91-2016 (GB23200.91-2016)Description (Translated English): Food safety national standard -- Determination of 9 organophosphorus pesticide residues in animal-derived foods -- Gas chromatographic method Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 9,933 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): SN/T 1776-2006 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.91-2016: Food safety national standard -- Determination of 9 organophosphorus pesticide residues in animal-derived foods -- Gas 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. Food safety national standard - Determination of 9 organophosphorus pesticide residues in animal - derived foods - Gas chromatographic method National Standards of People's Republic of China GB Instead of SN/T 1776-2006 National standards for food safety 9 kinds of organophosphorus pesticide residues in animal - derived food Determination Gas chromatography National food safety standards- Determination of nine organophosphorus pesticides residues in animal-derived Foods Gas chromatography 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 1776-2006 "Method for the determination of nine organophosphorus pesticide residues in foodstuffs of imported and exported animals. This standard compared with SN/T 1776-2006, 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 animal food" to "animal food"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 1776-2006. National standards for food safety Determination of 9 organophosphorus pesticide residues in animal - derived foods - Gas chromatographic method1 ScopeThis standard specifies the preparation of the import and export of ham and pickled fish (鲞) in the 9 kinds of organophosphorus pesticide residue test sample preparation and gas chromatography detection side law. This standard applies to ham and pickled fish (鲞) in the dichlorvos, methamidophos, acephate, methyl parathion, malathion, p- Thiophosphate, quinophosphoric acid, halophosphate, triazophos pesticide residues in the detection of 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 sample was extracted with acetonitrile and chromatographed on a gel column. The sample was quantitated by a gas chromatograph equipped with a flame photometric detector.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 Ethyl acetate (C4H8O2). Chromatographic purity. 4.1.2 acetonitrile (C2H3N). pure chromatography. 4.1.3 Cyclohexane (C6H12). Chromatographic Purification. 4.2 solution preparation 4.2.1 GPC eluent. ethyl acetate cyclohexane (1 1, volume ratio). take 100 mL of ethyl acetate, add 100 mL of cyclohexane, shake spare. 4.3 standards 4.3.1 Organic phosphorus standard. dichlorvos (CAS. 62-73-7), methamidophos, CAS. 10265-92-6), acephate (CAS. 30560-19-1), methyl parathion methyl (CAS. 298-00-0), malathion (CAS. 121-75-5), parathion (CAS. 56-38-2), quinophos (Quinalphos, CAS. 1776-83-6), methidathion (CAS. 950-37-8), triazophos, CAS. 24017-47-8), purity ≥ 99%. 4.4 standard solution preparation 4.4.1 dichlorvos, methamidophos, acephate, methyl parathion, malathion, parathion, quinophosphoric acid, methamphetamine, triazolam Quasi-reserve solution. Weigh the appropriate standard, respectively, with acetone dissolved to 100 mL, the solution concentration of 100 g/mL. Before use According to the need to use acetone diluted to the appropriate concentration, as a mixed standard working fluid. Store in 4 ℃ refrigerator.5 instruments and equipment5.1 Gas Chromatograph with Flame Photometric Detector (Phosphor Filter 525 nm). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Rotary Evaporator 5.4 Gel Purified Finished Product Column (GPC). 25 mmID x 400 mm; Filler. Bio-Beads, S-X3,38 m-75 m (need to do the elution curve before use). 5.5 constant temperature oscillator. 5.6 Mixer.6 Preparation and storage of samplesA typical sample of about 500 g was taken from all ham or pickled fish samples. The sampling site was carried out according to GB 2763 Appendix A, Crushed with a pulverizer, mixed evenly, are divided into two, respectively, into the clean container as a sample. Sealed and marked with mark. During sample and sample preparation, contamination of the sample or changes in the residue content should be prevented. Store the sample at -18 ° C ice Save under the box.7 Analysis steps7.1 Extraction Weigh 20 g of the pulverized homogeneous sample (accurate to 0.01 g) in a 100 mL stoppered flask, add 50 mL of acetonitrile at 30 ° C 2 ℃ oscillator, shake 2 h, filter, with a small amount of acetonitrile washing residue several times, combined filtrate, set below 40 ℃ water bath under reduced pressure to Near dry. 7.2 Purification Residue with 4.2.1 solvent volume to 10 mL, mix 2 min, centrifuge 5 min, 3000r/min. Take 5.0 mL supernatant over GPC Column at a flow rate of 5 mL/min, eluted with 4.2.1 solvent, discarded the first 100 mL of eluent, collected 100 mL to 165 mL of eluent, 40 ℃ below the water bath under reduced pressure to near dry, add 8 mL of ethyl acetate dissolved, quantitative transfer to 10 mL centrifuge tube, below 40 ℃ water Bath with a gentle nitrogen flow to dry, ham samples accurately add 1.0 mL of acetone, aquatic products (pickled products) to accurately add 5.0 mL of acetone, Mixing, gas chromatographic determination. 7.3 Determination 7.3.1 Gas Chromatographic Reference Conditions A) Column. quartz capillary column, DB-1701, 30 m x 0.53 mm (inner diameter) x 1.0 μm (film thickness), or equivalent; B) Carrier gas. nitrogen (purity greater than 99.999%); carrier gas flow rate 10 mL/min; tail gas flow rate. 30 mL/min; 75 mL/min, air flow rate. 100 mL/min; C) Column temperature. initial temperature 150 ° C for 2 min, rise to 270 ° C at 8 ° C/min for 18 min; D) Inlet temperature. 250 ° C; E) Detector temperature. 250 ° C; F) Injection method. no split injection; G) Injection volume. 2 μL; H) Opening time. 1.5 min. 7.3.2 Determination and confirmation of chromatography According to the content of organophosphorus pesticides in the sample, the standard working solution with similar peak area is selected. Standard working solution and sample solution The response value of organophosphorus should be within the linear range of the instrument. Standard working solution and sample volume and other volume interspersed injection determination. In the above chromatographic conditions The chromatogram of the lower standard is shown in Appendix A, Figure A.1. 7.4 blank experiment In addition to the sample, according to the above determination steps.8 results are calculated and expressedUse the chromatographic data processor or calculate the organic phosphorus pesticide content in the sample according to the following formula (1). MΑsi VCsiAi X .. (1) Where. Xi - Residual content of each organophosphorus pesticide in the sample in milligrams per kilogram, mg/kg; The peak area of each organophosphorus pesticide in the sample solution; V - the final volume of the sample solution, in milliliters, mL; Asi - the peak area of each organophosphorus pesticide in standard working fluid; Csi - the concentration of organophosphorus pesticide in standard working fluid in micrograms per milliliter, g/mL; M - the amount of sample represented by the final 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 B 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 C requirements. 10% limit and recovery rate 10.1 Quantitation limits Ham samples. dichlorvos, methamidophos, methamphetamine, methyl parathion, malathion, parathion, quinophosphoric acid, Phosphorus is 0.01 mg/kg. Pickled fish (鲞) samples. dichlorvos, methamidophos, acephate, methyl parathion, malathion, parathion, quinophos, Phosphorus and triazophos were 0.05 mg/kg. 10.2 Recovery rate The recoveries and precision of the experimental data (in the range of different additive concentrations) are as follows. Ham samples. A) dichlorvos. The recovery was 74% 106% and the precision was 6.4% 11.7% at 0.01 mg/kg, 0.02 mg/kg and 0.1 mg/kg. B) methamidophos. The recovery was 74.5% 106% and the precision was 9.6% 11.1% at 0.01 mg/kg, 0.02 mg/kg and 0.1 mg/kg. C) acephate. The recoveries were 74% 106% and the precision of 10.9% 11.7% at 0.01 mg/kg, 0.02 mg/kg and 0.1 mg/kg. D) methyl parathion. The recoveries were 74% 103% at 0.01 mg/kg, 0.02 mg/kg and 0.1 mg/kg. , Precision 8.6% 11.5% E) malathion. The recoveries were 72% 104% and the precision of 7.4% 10.9% at 0.01 mg/kg, 0.02 mg/kg and 0.1 mg/kg. F) Parathion. The recovery was 71% 105% and the precision was 6.5% 13.1% at 0.01 mg/kg, 0.02 mg/kg and 0.1 mg/kg. G) quetiophosphoric acid. The recovery was 78% 105% and the precision was 8.0% 9.5% at 0.01 mg/kg, 0.02 mg/kg and 0.1 mg/kg. H) Pomperide. The recovery was 79% 105% and the precision was 7.5% 9.2% at 0.01 mg/kg, 0.02 mg/kg and 0.1 mg/kg. I) triazophos. The recoveries were 78% 105% and the precision of 7.8% 9.5% at 0.01 mg/kg, 0.02 mg/kg and 0.1 mg/kg. Aquatic products (pickled products) samples. A) dichlorvos. The recovery was 72% 103% and the precision was 9.8% 11.0% at the concentration of 0.05 mg/kg, 0.1 mg/kg and 0.5 mg/kg. B) methamidophos. The recovery was 78% 108% at the concentration of 0.05 mg/kg, 0.1 mg/kg and 0.5 mg/kg, and the precision was 7.0% 9.4% C) acephate. The recovery was 70% 104% at the concentration of 0.05 mg/kg, 0.1 mg/kg and 0.5 mg/kg, and the precision was 9.0% 9.8% D) methyl parathion. The recovery was 82% at 0.05 mg/kg, 0.1 mg/kg and 0.5 mg/kg, and the precision was 7.3% 10.1% E) malathion. The recoveries were 78% 104%, and the precision was 8.4% 9.2% at the concentration of 0.05 mg/kg, 0.1 mg/kg and 0.5 mg / F) Parathion. The recoveries were 80% 109% at the concentration of 0.05 mg/kg, 0.1 mg/kg and 0.5 mg/kg, and the precision was 7.2% 11.3% G) quetiophosphoric acid. The recoveries were 74% 104% at the concentration of 0.05 mg/kg, 0.1 mg/kg and 0.5 mg/kg, and the precision was 9.6% 11.4% H) Pomperide. The recovery was 72% 105% at the concentration of 0.05 mg/kg, 0.1 mg/kg and 0.5 mg/kg, and the precision was 9.6% 11.2% I) triazophos. The recovery was 79% 105% at the concentration of 0.05 mg/kg, 0.1 mg/kg and 0.5 mg/kg, and the precision was 7.4% 8.2%Appendix A(Informative) Standard chromatogram 1 - dichlorvos (2.4 min) 2 - methamidophos (3.3 min) 3 - acephate (5.9 min) 4 - methyl parathion (10.4 min) 5 - malathion (10.7 min) 6 - parathion (11.3 min) 7 - quinophos (11.7 min) 8 - Mopapine (12.6 min) 9 - triazophos (14.9 min) Figure A.1 Gas chromatograms of 9 organophosphorus standardsAppendix B(Normative appendix) Laboratory repeatability requirements Table B.1 Laboratory repeatability requirements Measured component content Mg/kg Precision 0.001 36 > 0.01 > 1 14Appendix C(Normative appendix) Inter-laboratory reproducibility requirements Table C.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 23200.91-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.91-2016_English as soon as possible, and keep you informed of the progress. 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