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Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.5-2016: Food safety national standard -- Methods for the determination of herbicide residues -- Part 5: Determination of thiocarbamate herbicides in food by liquid chromatography-mass spectrometry / mass spectrometry Status: Valid
Basic dataStandard ID: GB 23200.5-2016 (GB23200.5-2016)Description (Translated English): Food safety national standard -- Methods for the determination of herbicide residues -- Part 5: Determination of thiocarbamate herbicides in food by liquid chromatography-mass spectrometry / mass spectrometry Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 15,149 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): SN/T 1737.5-2010 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.5-2016: Food safety national standard -- Methods for the determination of herbicide residues -- Part 5: Determination of thiocarbamate herbicides 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 - Methods for the determination of herbicide residues - Part 5. Determination of thiocarbamate herbicides in food by liquid chromatography - mass spectrometry/mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 1737.5-2010 National standards for food safety Method for determination of herbicide residue Part 5. Determination by liquid chromatography - mass spectrometry/mass spectrometry Residue of Thiocarbamate Herbicide in Food National food safety standards- Determination of thiocarbmate herbicide residues in 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 1737.5-2010 "Determination of thiourethane herbicide residues in import and export foods Liquid phase color Spectrum-mass spectrometry/mass spectrometry ". Compared with SN/T 1737.5-2010, 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 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 1737.5-2010. National standards for food safety Method for determination of herbicide residue Part 5. Determination of thiosemicarbazones in food by liquid chromatography - mass spectrometry/mass spectrometry Acid herbicide residues1 ScopeThis standard specifies the determination of the residues of nine thiocarbamate pesticides (see Appendix A) for liquid chromatography-mass spectrometry law. This standard applies to rice, soybeans, white radish, cabbage, broccoli, ginger, tea, peanuts, oranges, grapes, chicken, chicken liver And fish in the nine kinds of thiocarbamate pesticide residues in the quantitative determination 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 residual thiocarbamate herbicide was extracted from acetonitrile and the extract was purified by HLB and Envi-Carb solid phase extraction column. Phase chromatography - mass spectrometry detection and confirmation, internal 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, 75-05-8). Chromatographic Purification. 4.1.2 n-hexane (C6H14,110-54-3). 4.1.3 Acetone (C3H6O, 67-64-1). 4.1.4 acetic acid (C2H4O2, 64-19-7). chromatography pure. 4.1.5 Sodium chloride (NaCl, 7647-14-5). 4.2 solution preparation 4.2.1 N-Hexane-Acetone Solution (7 3). Accurately measure 70 mL of n-hexane and 30 mL of acetone and shake well. 4.2.2 acetonitrile - water solution (1 1). accurate measurement of 50 mL of acetonitrile and 50 mL of water, shake back. 4.3 standards 4.3.1 Reference material. see Appendix A, Table A.1, purity is greater than 99%. 4.3.2 Standard reference substance. D3- Carbaryl (100 μg/mL). 4.4 standard solution preparation 4.4.1 Thiocarbamate Pesticide Standard Reserve Solution (100 μg/mL). Accurate weighing of various thiourethane standards Quality, with acetonitrile prepared into a concentration of 100 mg/L standard stock solution, protected from light -18 ℃, the shelf life of 6 months. 4.4.2 Thiourethane Pesticide Mixed Standard Intermediate Solution (1.0 μg/mL). Draw each amount of standard stock solution, Release 1.0 mg/L mixed standard working solution, protected from light -18 ℃, the shelf life of 1 month. 4.4.3 Internal standard solution (1.0 μg/mL). Accurately absorb the appropriate amount of standard material, with acetonitrile prepared into a concentration of 1.0 mg/L Internal standard working solution, light -18 ℃ preservation, shelf life of 1 month. 4.5 Materials 4.5.1 HLB solid phase extraction column or equivalent..200 mg, 6 mL. Use 5 mL of acetonitrile before treatment to keep the cylinder moist. 4.5.2 Envi-Carb solid phase extraction column or equivalent..200 mg, 3 mL. Wash with 5 mL n-hexane-acetone before use to keep the column wet Run. 4.5.3 Microporous membrane. 0.22 μm, organic phase type.5 instruments and equipment5.1 Liquid Chromatography-Mass Spectrometer. Equipped with an electrospray ion source (ESI). 5.2 Analysis of balance. 0.1 mg and 0.01 g. 5.3 blowing nitrogen enrichment instrument. 5.4 Centrifuge. speed not less than 5 000 r/min. 5.5 homogenizer. 5.6 Vortex Mixer. 5.7 solid phase extraction device. 5.8 Pipettes. 10 to 100 μL and 100 to 1,000 μL. 5.9 Polypropylene centrifuge tube. 50 mL or 15 mL, with plug. 5.10 capacity bottle. 25 mL.6 Preparation and storage of samples6.1 Preparation of the sample 6.1.1 Rice, soybeans, peanuts and tea leaves Approximately 500 g of the sample was taken and pulverized thoroughly with a pulverizer. All samples were passed through a standard screen of 425 μm. Mix well. The samples are divided into two Copies, into a clean container, sealed, and marked with a mark. 6.1.2 White radish, cabbage, broccoli, ginger, oranges, grapes, chicken, chicken and fish Approximately 500 g of the sample was taken and it was chopped (not washed with water). The sample was processed into a slurry by a mash and mixed. Samples are Divided into two, packed into a clean container, sealed and marked with a mark. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Rice, soybeans, peanuts and tea samples kept at room temperature. White radish, cabbage, broccoli and other samples in -18 C below frozen storage. During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue.7 Analysis steps7.1 Extraction 7.1.1 Rice, soybeans, tea and peanuts Weigh 5 g (accurate to 0.01 g) sample in 50 mL stoppered centrifuge tube, weighed 2.5 g, add 100 μL internal standard intermediate solution, Add 10 mL of water, mix and place for 1 h. Then add 4.0 g of sodium chloride, then add 15 mL of acetonitrile high-speed homogeneous extraction 3 min, the oscillation to mention Take 15 min and centrifuge at 5 000 r/min for 5 min, transfer the acetonitrile layer to a 25 mL volumetric flask. The residue was again extracted with 10 mL of acetonitrile The combined extracts were combined and bound to 25 mL with acetonitrile. 7.1.2 White radish, cabbage, broccoli, ginger, oranges, grapes, chicken, chicken and fish Weigh 5 g (accurate to 0.01 g) sample in a 50 mL stoppered centrifuge tube, add 100 μL of the internal standard solution and 4.0 g of sodium chloride, The following operation is the same as 7.1.1. 7.2 Purification 7.2.1 rice, white radish, cabbage, broccoli, ginger, oranges, grapes, chicken and fish Take 5.0 mL of the extract in 15 mL centrifuge tube, 40 ℃ with N2 blowing to near dry. The residue was dissolved in 2.0 mL of n-hexane-acetone solution The solution was added to the treated Envi-Carb solid phase extraction column and the sample solution was passed through a solid phase extraction column at a flow rate of about 1.5 mL/min. The sample tubes were rinsed with 5 mL of n-hexane-acetone solution and the rinsing solution was added to the Envi-Carb solid phase extraction column to collect the total effluent in 15 ML centrifuge tube, 40 ℃ blowing nitrogen to near dry. The residue was fixed to 1.0 mL with acetonitrile-water solution. After vortexing, the residue was passed through a microfiltration membrane Determination by GC - MS. 7.2.2 Soybean, tea, peanuts and chicken liver Take 5.0 mL extract in 15 mL centrifuge tube, tea extract to take 10.0 mL, 40 ℃ with N2 to 2.0 mL or so. will The concentrate was transferred to a treated HLB solid phase extraction column, and the sample solution was passed through a solid phase extraction column at a flow rate of about 1.5 mL/min, ML of acetonitrile was rinsed and the solid phase extraction column was drained. The whole effluent was collected in a 15 mL centrifuge tube and purged with N2 at 40 ° C. The residue was dissolved in 2.0 mL of n-hexane-acetone solution and the solution was added to the treated Envi-Carb solid phase extraction column at about 1.5 ML/min. The sample solution was passed through a solid phase extraction column and the sample tube was rinsed with 5 mL of n-hexane-acetone solution and the rinsing solution was added The Envi-Carb solid phase extraction column was collected and the whole effluent was collected in a 15 mL centrifuge tube and the nitrogen was blown at 40 ° C to near dryness. The residue was eluted with acetonitrile - water To 1.0 mL, vortex after mixing, through the microporous membrane, for liquid chromatography - mass spectrometry. 7.3 Determination 7.3.1 Liquid Chromatographic Reference Conditions A) Column. Acquity BEH C18 column, 50 mm × 2.1 mm (id), 1.7 μm, or equivalent; B) Column temperature. 40 ° C; C) Injection volume. 10 μL; D) The mobile phase, flow rate and gradient elution conditions are shown in Table 1. Table 1 Mobile phase, flow rate and gradient elution conditions time Min Flow rate ML/min 0.1% acetic acid aqueous solution Methanol 0 0.25 70 30 15.0 0.25 0 100 15.1 0.25 70 30 18.0 0.25 70 30 7.3.2 Mass spectrometry reference conditions A) ionization mode. electrospray ion source; B) Scanning mode. positive ion scanning; C) Detection method. Multiple reaction monitoring (MRM); D) Resolution. Unit resolution; See Appendix B for other reference mass spectrometry conditions. 7.4 Standard working curve (1.0 μg/mL) and the internal standard solution (1.0 μg/mL) were mixed with a blank sample extraction solution 10 μg/L, 100 μg/L, 100 μg/L, 100 μg/L, 100 μg/L, 100 μg/L, Quasi-working solution, the internal standard concentration of 20.0 μg/L. Preparation for use, for liquid chromatography - mass spectrometry. To be measured and internal standard Peak area ratio of the ordinate, matrix mixed standard working solution concentration for the abscissa to draw the standard working curve. 7.5 Determination 7.5.1 Qualitative determination Each selected component selected one parent ion, two or more child ions, in the above experimental conditions, the sample retention time of the material to be tested, And the substrate standard solution retention time deviation within ± 2.5%; and the sample of each component of the relative abundance of ions and concentrations close to the matrix Comparing the relative abundance of the corresponding qualitative ions in the standard working solution, the deviation does not exceed the range specified in Table 2, There is a corresponding test substance in the product. 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% 7.5.2 Quantitative determination In the best working conditions of the instrument, the standard solution of the mixed working solution of the matrix was measured with the ratio of the peak area of the analyte and the internal standard, Matrix mixed standard working solution concentration for the abscissa to draw the standard working curve, with the standard working curve of the sample quantitative, sample solution The response value of the test object should be within the linear range of the instrument; if the linear range is exceeded, the blank matrix solution is used for proper dilution Injection assay. A multi-reaction monitoring (MRM) chromatogram of the nine thiocarbamate herbicide reference materials is shown in Figure C.1 in Appendix C. 7.6 blank experiment In addition to the standard sample, according to the above measurement steps.8 results are calculated and expressedThe amount of thiourethane herbicide in the sample was calculated according to formula (1). MAAc VAAcc Sisi Sii (1) Where. X - the amount of the component to be measured in the sample, in micrograms per kilogram, μg/kg; C - the concentration of the drug in the standard working solution in micrograms per liter, μg/L; Ci - the concentration of the internal standard in the sample solution, in micrograms per liter, μg/L; A - the peak area of the drug in the sample solution; Asi - the peak area of the internal standard in the standard working solution; V - the final volume of the sample solution in milliliters, mL; Csi - the concentration of the internal standard in the standard working solution in micrograms per liter, μg/L; The peak area of the internal standard in the sample solution; As - the peak area of the drug in the standard working solution; 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 E 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 F requirements. 10% limit and recovery rate 10.1 Quantitation limits The limit of quantification for nine thiocarbamate herbicides was 5.0 μg/kg. 10.2 Recovery rate In the range of 5.0 μg/kg ~.200 μg/kg, add rice, soybeans, white radish, cabbage, broccoli, ginger, tea, flower The recovery rates of nine thiocarbamate herbicides in raw, orange, grape, chicken, chicken and fish are shown in Appendix D.Appendix A(Informative) Table A.1 Information on 9 thiocarbamate herbicides Compound English name CAS No. Molecular formula Cobalt pebulate 1114-71-2 C10H21NOS Grasses of molybdenum Green grass enemy EPTC 759-94-4 C9H19NOS Cotyledon thiobencarb 28249-77-6 C12H16ClNOS Oat enemy Butterone Wild tartan triallate 2303-17-5 C10H16Cl3NOS Cedar enemies vernolate 1929-77-7 C10H21NOS Cyclocane Cycloxy 1134-23-2 C11H21NOSAppendix B(Informative) Reference to mass spectrometry conditions A) electrospray voltage. 3000 V; B) Auxiliary gas flow rate. 700 L/h; C) collision gas. argon; D) curtain air flow rate. 50 L/h; E) ion source temperature. 105 ° C; F) Auxiliary gas temperature. 350 ° C; G) Qualitative ion pair, quantitative ion pair, acquisition time, extraction voltage and collision energy are shown in Table B.1. Table B.1 Mass spectrometric parameters for the determination of 9 thiocarbamate herbicides Analyte Reference retention time Min Parent ion Acquisition time Extraction voltage Collision energy EV Grasshopper 7.20 188 126 * 0.10 32 Rhizoctonia enemy 8.57 190 128 * 0.05 28 Bitter enemy 10.56 218 57 * 0.05 32 Destroy the enemy 9.79 204 86 * 0.05 30 The enemy is 9.84 204 57 * 0.05 28 Wild pills 11.62 306 86 * 0.05 30 Grasses 9.77 258 100 * 0.05 28 Ring grass enemy 9.89 216 154 * 0.05 24 Ophiopogon 10.30 270 86 * 0.05 34 D3- Carbaryl 4.22 205 145 * 0.05 20 10 Note. * for the quantitative ions, for different mass spectrometry equipment, instrument parameters may be different, should be measured before the mass spectrometry parameters to optimize the best. Non-commercial statement. The reference mass spectrometry conditions listed in Appendix A are performed on a Waters Quattro Premier LC/MS. The list of test instruments listed below is for reference only and does not involve commercial purposes and encourages standard users to try different manufacturers or models of instruments.Appendix C(Informative) Standard multi-reaction monitoring (MRM) chromatograms Figure C.1 5.0 μg/L 9 Thiocarbamate Herbicides Standard Solution Multiple Reaction Monitoring (MRM) ChromatogramAppendix D(Informative) The recovery of nine thiocarbamate pesticides in different substrates Table D.1 Experimental data on the concentration and recovery of the sample The name of the compound Add level Μg/kg Rice Recovery rate Soybeans Recovery rate range White radish Recovery rate Cabbage Recovery rate Broccoli Recovery rate Ginger Recovery rate range orange Recovery rate range grape Recovery rate range peanut Recovery rate range tea Recovery rate range chicken Recovery rate range Chicken liver Recovery rate Fish Recovery rate Grass enemies 5.0 83.3 to 99.1 73.6 to 95.6 61.5 to 79.7 76.1 to 92.7 66.0 to 84.0 66.1 to 80.1 73.4 to 86.6 80.4 to 95.4 75.1 to 97.5 75.9 to 93.2 80.9 to 91.1 69.8 to 88.5 77.1 to 90.4 10.0 88.3 to 104 72.2 to 87.2 64.4 to 78.4 67.1 to 79.2 66.3 to 84.3 65.4 to 79.8 68.9 to 83.5 77.5 to 93.2 73.6 to 88.9 70.8 to 85.0 73.6 to 90.2 74.2 to 91.8 70.2 to 86.0 20.0 81.7 to 91.5 70.3 to 85.5 65.8 to 83.6 77.6 to 97.5 79.5 to 93.5 68.5 to 82.6 74.2 to 82.8 80.0 to 85.8 71.7 to 87.2 68.5 to 83.4 70.4 to 85.3 74.7 to 92.4 67.1 to 81.3 Rice. 100 Soybeans, white radish, cabbage, Broccoli, ginger, oranges, grapes, Tea, peanuts, chicken, chicken liver, Fish. 50.0 84.3 to 95.1 75.4 to 89.6 71.6 to 90.2 81.2 to 89.8 82.4 to 96.4 69.6 to 81.8 67.2 to 83.8 80.6 to 88.6 76.9 to 91.4 73.5 to 87.4 71.2 to 87.8 76.4 to 87.0 67.9 to 83.7 Mussel enemy 5.0 87.2 to 104 70.9 to 85.8 63.0 to 79.3 74.2 to 88.2 63.2 to 79.8 68.1 to 78.0 74.2 to 89.9 66.3 to 90.3 73.7 to 89.2 69.1 to 83.7 90.6 to 99.5 67.6 to 85.2 86.4 to 94.9 10.0 82.3 to 94.4 69.1 to 86.1 67.8 to 81.9 77.4 to 94.6 65.5 to 77.8 68.3 to 86.3 78.5 to 96.6 76.7 to 89.3 71.9 to 89.5 67.4 to 83.9 71.5 to 92.7 62.2 to 77.9 68.2 to 88.4 20.0 71.2 to 79.1 68.6 to 78.4 65.2 to 80.5 87.4 to 101 67.6 to 78.6 79.2 to 93.8 77.9 to 97.8 68.6 to 80.2 71.3 to 81.5 67.8 to 76.4 76.1 to 87.3 74.4 to 93.3 72.6 to 83.2 Rice, soybeans, white radish, small Cabbage, broccoli, ginger, oranges, Grapes, peanuts, peanuts Chicken, chicken liver, fish. 50.0 68.5 to 76.9 68.5 to 76.9 68.5 to 85.1 88.2 to 99.8 68.5 to 80.5 78.5 to 90.8 80.9 to 92.1 69.1 to 82.1 71.2 to 80.0 66.8 to 75.0 77.8 to 88.2 71.6 to 86.2 74.2 to 84.1 Grams of grass enemy 5.0 94.9 to 112 79.9 to 88.2 70.0 to 83.2 66.1 to 82.5 71.5 to 80.4 70.8 to 88.6 67.6 to 92.1 71.6 to 99.9 83.1 to 92.1 77.9 to 86.4 80.2 to 97.0 71.0 to 81.2 76.5 to 92.5 10.0 87.3 to 107 72.8 to 86.6 64.1 to 82.0 67.3 to 80.1 63.2 to 79.7 70.4 to 79.6 68.9 to 89.5 70.4 to 92.2 75.7 to 90.1 71.0 to 84.4 71.2 to 88.4 68.2 to 86.4 67.9 to 84.3 20.0 87.0 to 92.6 74.5 to 84.2 74.9 to 85.8 84.4 to 99.1 71.0 to ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 23200.5-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.5-2016_English as soon as possible, and keep you informed of the progress. 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