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Delivery: <= 6 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.9-2016: Food safety national standard -- Determination of residues of 475 pesticides and related chemicals in grain -- Gas chromatographic-mass spectrometry Status: Valid
Basic dataStandard ID: GB 23200.9-2016 (GB23200.9-2016)Description (Translated English): Food safety national standard -- Determination of residues of 475 pesticides and related chemicals in grain -- Gas chromatographic-mass spectrometry Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 54,539 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): GB/T 19649-2006 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.9-2016: Food safety national standard -- Determination of residues of 475 pesticides and related chemicals in grain -- Gas chromatographic-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 residues of 475 pesticides and related chemicals in grain - Gas chromatographic - mass spectrometry ICS National Standards of People's Republic of China Replace GB/T 19649-2006 2016-12-18 release 2017-06-18 Implementation National standards for food safety 475 pesticides and related chemical residues in grain Determination Gas chromatography - mass spectrometry National food safety standards- Determination of 475 pesticides and related chemicals residues in grains Gas chromatography-mass spectrometry Directory Preface II 1 Scope 1 2 normative reference document 1 Principle 1 4 reagents and materials 1 5 instruments and equipment 2 6 Preparation of sample 2 7 Analysis Step 2 Calculation and presentation of results 3 9 precision 4 10% limit and recovery rate 4 Appendix A (informative) 475 kinds of pesticides and related chemicals, English name, method of quantitative limit, grouping, solvent selection And mixed standard solution concentrations Appendix B (informative) Retention time of 475 pesticides and related chemicals and internal standard compounds, quantitative ions, The ratio of qualitative and quantitative ions to qualitative ions Appendix C (Informative Appendix) Group A, B, C, D and E Group 5 Selective Ion Monitoring Group for Pesticides and Related Chemicals Table 31 Appendix D (informative) Reference substance Select ion monitoring in wheat matrix GC-MS Figure 35 Appendix E (informative) Relative standard deviation in laboratory Appendix F (informative) Relative standard deviation between laboratories 41 Appendix G (informative) Experimental data on the concentration and recovery of samples ForewordThis standard replaces GB/T 19649-2006 "Determination of 475 pesticides and related chemical residues in grain" Gas chromatography-mass spectrometry " This standard compared with GB/T 19649-2006, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - increase the "other food reference implementation" in the standard range. This standard has been replaced by the previous version of the release. -GB/T 19649-2006. National standards for food safety Determination of 475 pesticides and related chemical residues in grain Gas chromatography - mass spectrometry1 ScopeThis standard specifies the remaining amount of 475 pesticides and related chemicals (see Appendix A) for barley, wheat, oat, rice and maize. Determination of Chromatography - Mass Spectrometry. This standard applies to the determination of 475 pesticides and related chemical residues in barley, wheat, oats, rice and maize. Other grain Can refer to the implementation 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 in an accelerated solvent extraction instrument. The extract was purified by solid phase extraction column and washed with acetonitrile-toluene solution (3 1) De-pesticide and related chemicals, with gas chromatography - 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, 75-05-8). Chromatographic Purification. 4.1.2 diatomaceous earth (SiO2, 61790-53-2). excellent grade pure. 4.1.3 anhydrous sodium sulfate (Na2SO4,7757-82-6). analytical grade. Before burning at 650 ℃ for 4h, stored in a dryer, cooling and standby. 4.1.4 toluene C7H8, 108-88-3). excellent grade pure. 4.1.5 Acetone (CH3COCH3,67-64-1). Analytical pure, re-distilled. 4.1.6 dichloromethane (CH2Cl2, 75-09-2). chromatographic purity. 4.2 standards Pesticide and Related Chemical Reference Material. Purity ≥95%, see Appendix A. 4.3. Standard solution preparation 4.3.1 Standard stock solution Accurately weighed 5mg ~ 10mg (accurate to 0.1mg) pesticides and related chemicals in the standard 10mL volumetric flask, according to the standard The solubility of the quasi-material and the determination of the need to select toluene, toluene - acetone mixture, dichloromethane and other solvents dissolved and constant volume to the scale (solvent selection See Appendix A). 4.3.2 Mixing standard solutions (mixed standard solutions A, B, C, D and E) According to the nature of pesticides and related chemicals and retention time, will be 475 kinds of pesticides and related chemicals into A, B, C, D, E five And the concentration of each pesticide and associated chemical in the instrument to determine the concentration in the mixed standard solution. This is the standard 475 groups of pesticides and related chemicals and their mixed standard solution concentrations are given in Appendix A, Depending on the group number of each pesticide and associated chemical, the concentration of the standard solution and the concentration of the standard stock solution, Pesticide and related chemicals Standard stock solution (4.3.1) in a 100 mL volumetric flask, fixed to the mark with toluene. Mixed standard solution to avoid Light 4 ℃ preservation, shelf life of one month. 4.3.3 internal standard solution Accurately weighed 3.5mg epoxy heptachlor in 100mL volumetric flask, with toluene volume to the scale. 4.3.4 matrix mixed standard working solution A, B, C, D, E group of pesticides and related chemical matrix mixed standard working solution is 40μL standard solution (4.3.3) and a certain Volume of the mixed standard solution were added to 1.0 mL of the sample blank matrix extract, mix, dubbed the matrix mixed standard working solution A, B, C, D and E. Matrix mixed standard working solution should be used with the current distribution. 4.4 Materials 4.5.1 Envi-18 Column 1). 12 mL, 2 g or equivalent. 4.5.2 Envi-Carb Column 1). 6 mL, 0.5 g or equivalent. 4.5.3 Sep-Pak NH2 column 2). 3 mL, 0.5 g or equivalent.5 instruments and equipment5.1 Gas Chromatography-Mass Spectrometer. Equipped with an electron impact source (EI). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Accelerated solvent extraction. equipped with 34 mL extraction tank. 5.4 nitrogen dryers. 5.5 Pear bottles..200mL. 5.6 pipettes. 1 mL.6 Preparation and storage of samples6.1 Preparation of the sample Grain samples taken according to GB 5491 were crushed by pulverizer. All samples were passed through a standard screen of 425 μm, and the samples were prepared. Divided into two, packed into a clean sample container, sealed and marked.7 Analysis steps7.1 Extraction Weigh 10 g of sample (accurate to 0.01 g) and mix with 10 g of diatomaceous earth and move into a 34 mL extraction cell of an accelerated solvent extractor. 10.34MPa pressure, 80 ℃ under the conditions of heating 5min, with acetonitrile static extraction 3min, cycle 2 times, and then use the pool volume of 60% of the B Nitrile (20.4 mL) was rinsed and purged with nitrogen for 100 seconds. After extraction, the extract was mixed and the samples with little oil content were mixed Take a half of the volume of the extract (equivalent to 5 g of the sample), and take a quarter of the volume of the extract from the larger oil sample (equivalent to 2.5g sample volume), to be purified. 7.2 Purification 7.2.1 The Envi-18 column was pre-washed with 10 mL of acetonitrile and the Envi-18 column was placed on a holder and the pear-shaped flask was transferred to the above- And the Envi-18 column was washed with 15 mL of acetonitrile, the extract and the washings were collected and the collected liquid was concentrated to about 1 mL on a rotary evaporator, spare. 1) Envi-18 columns and Envi-Carb are the trade names of SUPELCO's products. This information is intended for the convenience of this standard and does not imply endorsement of the product. If it is His equivalent product has the same effect, you can use these equivalent products. 2) The Sep-PakNH2 column is the product name of Waters' products, and this information is provided for the convenience of this standard and is not intended to be a recognition of the product. If other equivalent products With the same effect, you can use these equivalent products. 7.2.2 Add about 2 cm of high anhydrous sodium sulfate to the Envi-Carb column and connect the column to the top of the Sep-PakNH2 column with 4 mL of acetonitrile- Toluene solution (3 1) pre-wash the series column, the next pear-shaped bottle, into the fixed frame. The sample concentrate was transferred to a tandem column, The vial was washed with 3 x 2 mL of acetonitrile-toluene solution and the wash was transferred to the column. A 50 mL reservoir was added to the column and 25 mL Acetonitrile-toluene solution, all of the effluent was collected in a pear-shaped flask and concentrated in a water bath at 40 ° C to about 0.5 mL. Add 2 x 5 mL n-hexane for solvent exchange twice, and finally make the sample volume about 1 mL, add 40 μL of internal standard solution, mix for Determination by Gas Chromatography - Mass Spectrometry. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. DB-1701 (30m × 0.25mm × 0.25μm) quartz capillary column or equivalent; B) Column temperature. 40 ℃ for 1min, then 30 ℃/min program temperature to 130 ℃, then 5 ℃/min temperature to 250 ℃, And then to 10 ℃/min temperature to 300 ℃, keep 5 min; C) Carrier gas. helium, purity ≥99.999%, flow rate. 1.2mL/min; D) Inlet temperature. 290 ° C; E) Injection volume. 1 μL; F) Injection method. no split injection, 1.5 min after the opening of the diversion valve and septum purge valve; G) electron bombardment source. 70 eV; H) ion source temperature. 230 ° C; I) GC-MS interface temperature. 280 ° C; J) Select ion monitoring. Each compound selected a quantitative ion, 2 to 3 qualitative ions. Each group needs to be tested Ions in accordance with the peak sequence, respectively, sub-time detection. The retention time of each compound, the quantitative ion, the qualitative ion and the quantitative ion The ratio of ion abundances is given in Appendix B. Refer to Appendix C for the start time and dwell time of each group to detect ions. 7.3.2 Qualitative determination When the sample is measured, if the retention time of the detected peaks is consistent with the standard sample, and after the background mass In the figure, the selected ions are present, and the selected ion abundance ratio is consistent with the ion abundance ratio of the standard sample (relative abundance > 50% Allow ± 10% deviation; relative abundance > 20% to 50%, allow ± 15% deviation; relative abundance > 10% to 20%, allow ± 20% deviation; Relative abundance ≤ 10%, allowing ± 50% deviation), you can determine the presence of this pesticide or related chemicals in the sample. If it can not be confirmed, should be heavy New injection, in scanning mode (with sufficient sensitivity) or by adding other confirmed ions or with other higher sensitivity analytical instruments To confirm. 7.3.3 Quantitative determination This method uses the internal standard method to determine the single ion quantification. The internal standard is epoxy heptachlor. To reduce the impact of the matrix, the quantitative criteria should be empty White sample preparation of mixed standard working solution. The concentration of the standard solution should be close to the concentration of the compound to be tested. A, B, C, D, E of this method Five groups of reference materials in the grain matrix selection of ion monitoring GC-MS Figure See Appendix D. 7.4 parallel test Perform the parallel test of the same sample according to the above steps. 7.5 blank test Unless the sample is not weighed, according to the above steps.8 results are calculated and expressedThe result of gas chromatography-mass spectrometry can be calculated automatically by computer according to internal standard method, and can be calculated according to formula (1) X = Cs × Ci Asi (1) As Csi Ai m 1000 Where. Residue of the test substance in milligrams per kilogram (mg/kg); Cs The concentration of the test substance in the standard working solution, in micrograms per milliliter (μg/mL); The chromatographic peak area of the analyte in the sample solution; As Matrix chromatographic peak area of the test solution in the standard working solution; Ci The concentration of the internal standard in the sample solution, in micrograms per milliliter (μg/mL); Csi The concentration of the internal standard in the standard working solution of the matrix, in micrograms per milliliter (μg/mL); Asi Matrix chromatographic peak area of standard working solution; Ai The chromatographic peak area of the internal standard in the sample solution; The final volume of the sample solution in milliliters (mL); The mass of the sample represented by the sample solution, in grams (g). The result of the calculation should be deducted from the blank value. The result of the measurement is expressed by the arithmetic mean of the parallel measurement, and the two valid digits are retained.9 precision9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the Record the requirements of D. 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 the Record the requirements of E. 10% limit and recovery rate 10.1 Quantitation limits The quantitative limits of this method are given in Appendix A. 10.2 Recovery rate When adding levels of LOQ, 4 × LOQ, add the recovery rate see Appendix G.Appendix A(Informative) 475 Pesticides and Related Chemicals Method Quantification limits, grouping, solvent selection and mixing Standard solution concentrations A.1 475 Pesticides and Related Chemicals Chinese and English Name, Method Quantification, Grouping, Solvent Selection and Mixing Standard Solution Concentration Table A.1 Serial number Chinese name English name The limit of quantitation/ (Mg/kg) Solvent Mixed standard dissolved Liquid concentration / (Mg/L) Internal standard epichlorohydrin Heptachlor-epox Toluene Group A 1 2-Propyl Acetate Allidochlor 0.0500 Toluene 5 2 allyl grasses Dichlormid 0.0500 toluene 5 3 soil fungus Etridiazol 0.0750 Toluene 7.5 4 Chloromethylthiophosphate Chlormephos 0.0500 Toluene 5 5 Aniline Ling Propham 0.0250 Toluene 2.5 6 ring grass enemy Cycloate 0.0250 toluene 2.5 7 biphenyl diamine Diphenylamine 0.0250 Toluene 2.5 8 Ethylene Fluoroline Ethalfluralin 0.1000 Toluene 10 9 Phorate Phorate 0.0250 Toluene 2.5 10 Methyl Bium Phosphate Thiometon 0.0250 Toluene 2.5 11 Pentachlorobenzene Quintozene 0.0500 Toluene 5 12 deethyletrazine Atrazine-desethyl 0.0250 Toluene Acetone (8 2) 2.5 13 Clamazone 0.0250 Toluene 2.5 14 Diazinon 0.0250 Toluene 2.5 15 Diposulfuron Fonofos 0.0250 Toluene 2.5 16 pyrimethazine Etrimfos 0.0250 toluene 2.5 17 Simaxin Simazine 0.0250 Methanol 2.5 18 Amphetamine Propetamphos 0.0250 Toluene 2.5 19 sec-butyl pass Secbumeton 0.0250 Toluene 2.5 20 Diplox Dichlofenthion 0.0250 Toluene 2.5 21 propargyl alcohol Toluene Acetone (9 1) 2.5 22 Zeke Mexacarbate 0.0750 Toluene 7.5 Aldrin 0.0500 Toluene 5 24 Amificin Dinitramine 0.1000 Toluene 10 25 Flies Phosphorus Ronnel 0.0500 Toluene 5 Potatoes Prometryne 0.0250 Toluene 2.5 27 Cycloprene Cyprazine 0.2000 Toluene Acetone (9 1) 28 Vinylloxacin Vinclozolin 0.0250 Toluene 2.5 29 β-666 Beta-HCH 0.0250 Toluene 2.5 30 metalaxyl metalaxyl 0.0750 toluene 7.5 31 Chlorpyrifos Chlorochrifos (-ethyl) 0.0250 Toluene 2.5 32 methyl parathion Methyl-Parathion 0.1000 Toluene 10 Serial number Chinese name English name The limit of quantitation/ (Mg/kg) Solvent Mixed standard dissolved Liquid concentration / (Mg/L) 33 anthraquinone anthraquinone 0.0250 dichloromethane 2.5 34 δ-666 Delta-HCH 0.0500 Toluene 5 35 times thiophosphate Fenthion 0.0250 toluene 2.5 36 malathion 0.1000 Toluene 10 37 Fenitrothion 0.0500 Toluene 5 38 Paraoxon-ethyl 0.1000 Toluene 10 39 Triadimefon 0.0500 Toluene 5 40 Parathion 0.1000 Toluene 10 41 pendimethalin Pendimethalin 0.1000 Toluene 10 Long Valley Toluene Acetone (9 1) 43 Acetylidene Chlorobenzene 0.0500 Toluene 5 44 Ethyl bromothiophosphate Bromophos-ethyl 0.0250 Toluene 2.5 45 Quetiapine Quinalphos 0.0250 Toluene 2.5 46 trans-Chlordane 0.0250 Toluene 2.5 Pondo Powder 48 Pyrazolamine Metazachlor 0.0750 Toluene 7.5 49 Benzylthio Fenothiocarb 0.0500 Acetone 5 Prothiophos 0.0250 Toluene 2.5 Flocculated Alcohol Chlorflurenol 0.0750 Toluene Acetone (9 1) 7.5 52 Dieldrin Dieldrin 0.0500 Toluene 5 53 Procymidone 0.0250 Toluene 2.5 Methidathion 0.0500 Toluene 5 55 Diclofenac Napropamide 0.0750 Toluene 7.5 56 oxadoxine Oxadiazone 0.0250 Toluene 2.5 57 benzene line phosphorus Fenamiphos 0.0750 toluene 7.5 58 dexamethasone sulfur chloride Tetrasul 0.0250 toluene 2.5 59 Mite special Aramite 0.0250 Dichloromethane 2.5 60 Ethyl pyrimethanone Bupirimate 0.0250 Toluene 2.5 61 Moisturizer Carboxin 0.0750 Toluene 7.5 62 fluoroamide Flutolanil 0.0250 Toluene 2.5 63 p, p'-drop 4,4'-DDD 0.0250 toluene 2.5 Ethoxine.2000 Ethylene 5 65 thiophosate Sulprofos 0.0500 Toluene 5 66 Ethylenediazol-1 Etaconazole-1 0.0750 Toluene 7.5 67 Ethylenediazol-2 Etaconazole-2 0.0750 Toluene 7.5 Myclobutanil 0.0250 Toluene 2.5 69 Strawberry Diclofop-methyl 0.0250 Toluene 2.5 70 Propiconazole 0.0750 Toluene 7.5 71 Forskyl Phosphorus Fansulfothion 0.0500 Toluene 5 72 bifenthrin Bifenthrin 0.0250 n-hexane 2.5 73 Mirex Mintx 0.0250 Toluene 2.5 Serial number Chinese name English name The limit of quantitation/ (Mg/kg) Solvent Mixed standard dissolved Liquid concentration / (Mg/L) 74 wheat rust Ling Benodanil 0.0750 toluene 7.5 Fluorophenylpyrrolidone Nuarimol 0.0500 Toluene Acetone (9 1) 76 Methoxy Dioxide Methoxychlor 0.0250 Toluene 2.5 77 Oxolipine Oxadixyl 0.0250 Toluene 2.5 78 Tetramethrin 79 tebuconazole 0.0750 toluene 7.5 80 Fluorobenzene Norflurazon 0.0250 Toluene Acetone (9 1) 2.5 81 pyridazine phosphoric acid Pyridaphenthion 0.0250 Toluene 2.5 82 Amimidophos Phosmet 0.0500 Toluene 5 83 Diclofenac Tetraflon 0.0250 Toluene 2.5 84 Oxidic acid Oxycarboxin 0.1500 Toluene Acetone (9 1) 85 cis-permethrin cis-Permethrin 0.0250 toluene 2.5 86 trans-permethrin trans-Permethrin 0.0250 toluene 2.5 87 Pyralophosphate Pyrazophos 0.0500 Toluene 5 88 cypermethrin 0.0750 toluene 7.5 Fenvalerate 0.1000 Toluene 10 Deltamethrin 0.1500 Toluene 15 Group B 91 Green grass enemy EPTC 0.0750 Toluene 7.5 92 Butylate 0.0750 Toluene 7.5 93 Diclovir Dichlobenil 0.0050 Toluene 0.5 94 grams of grass enemy Pebulate 0.0750 toluene 7.5 95 Trichloromethylpyridine Nitrapyrin 0.0750......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 23200.9-2016_English be delivered?Answer: Upon your order, we will start to translate GB 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