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Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.96-2016: Food safety national standard -- Determination of the content of chlordimeform and its metabolites in honey by liquid chromatography-mass spectrometry / mass spectrometry Status: Valid
Basic dataStandard ID: GB 23200.96-2016 (GB23200.96-2016)Description (Translated English): Food safety national standard -- Determination of the content of chlordimeform and its metabolites in honey by liquid chromatography-mass spectrometry / mass spectrometry Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 11,114 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): SN/T 0213.1-2011 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.96-2016: Food safety national standard -- Determination of the content of chlordimeform and its metabolites in honey 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 the content of chlordimeform and its metabolites in honey by liquid chromatography-mass spectrometry/mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 0213.1-2011 National standards for food safety Determination of the Residue of Chlordimeform and Its Metabolites in Honey Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of chlordimeform and its metabolite residues in honey 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 0213.1-2011 "Determination of the content of chlordimeform and its metabolites in the export of honey by liquid chromatography-mass spectrometry Spectrum method ". Compared with SN/T 0213.1-2011, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the standard name "export honey" to "honey"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 0213.3-1993 -SN/T 0213.1-2011. National standards for food safety Determination of the content of chlordimeform and its metabolites in honey by liquid chromatography-mass spectrometry/mass spectrometry1 ScopeThis standard specifies a method for the determination of chlordimeform and its metabolite (4-chloro-o-toluidine) in honey by liquid chromatography-mass spectrometry/mass spectrometry. This standard applies to honey (acacia honey, Vitex honey, honey honey, miscellaneous honey, wild honey, etc.) in the chlordimeform and its metabolite (4-chloro Toluidine) residue in liquid chromatography-mass spectrometry/mass spectrometry and other food samples.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 diluted with aqueous sodium hydroxide solution, purified by HLB solid phase extraction column, liquid chromatography-tandem mass spectrometer, external standard the amount.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 pure. 4.1.2 methanol (CH3OH), high performance liquid chromatography pure. 4.1.3 Sodium hydroxide (NaOH). 4.1.4 sulfuric acid (H2SO4). 4.1.5 Formic acid (HCOOH), purity ≥99%. 4.2 solution preparation 4.2.1 0.02 mol/L sodium hydroxide solution. dissolved 800 mg sodium hydroxide in 1 L water, the use of a period of 1 month. 4.2.2 1 mol/L sulfuric acid solution. in the amount of water slowly into the 54.3 mL concentrated sulfuric acid, while stirring and stirring, diluted with water to 1 L, so that With a period of 3 months. 4.2.3 10 mmol/L sulfuric acid solution. in the amount of water slowly into 10 mL 1 mol/L sulfuric acid, while stirring and stirring, diluted with water to 1 L, Use for 1 month. 4.2.4 acetonitrile aqueous solution. acetonitrile. water (3 7, V/V). 4.2.5 0.1% formic acid solution. 1 mL formic acid dissolved in water and fixed to 1 L. 4.3 standards 4.3.1 Pesticide standard (chlordimeform, C10H13ClN2, CAS. 6164-98-3. purity ≥99%) and 4-chloro-o-toluidine standard (4-chloro-o-toluidine, C7H8ClN, CAS. 95-69-2. purity ≥99%). 4.4 standard solution preparation 4.4.1 Preparation of standard stock solution. accurately weighed the appropriate amount of chlordimeform and 4-chloro o-toluidine standard, with acetonitrile prepared into a concentration of 1.0 Mg/mL standard stock solution. The solution was stored in a refrigerator at -18 ° C. Valid for 12 months. 4.4.2 Preparation of the standard intermediate solution. diluted the standard stock solution with acetonitrile to a final concentration of about 1.0 μg/mL, below 4 ° C. Save, valid for 6 months. 4.4.3 matrix standard working solution preparation. according to need, when used to absorb a certain amount of standard intermediate solution, with the matrix blank solution with Mix the standard working solution with the appropriate concentration. Less than 4 ℃ dark storage, is now available with. 4.5 Materials 4.5.1 HLB solid phase extraction column (hydrophilic lipophilic balance column). 60 mg (filler. polystyrene-divinylbenzene-pyrrolidone), 3 mL Or equivalent. Activate with 3 mL of methanol and 3 mL of water before use. 4.5.2 Microporous membrane. 0.22 μm, organic system.5 instruments and equipment5.1 Liquid Chromatography - Tandem Mass Spectrometer. Equipped with electrospray ion source (ESI). 5.2 Electronic balance. 0.01g and 0.0001g respectively. 5.3 vortex mixer. 5.4 solid phase extraction device. 5.5 nitrogen blowing instrument. 5.6 Centrifuge tube. 15 mL. 5.7 glass tube. 10 mL, with scale. 5.8 constant temperature water bath.6 Preparation and storage of samples6.1 Preparation of the sample Take about 500 g of the representative honey sample, the sampling site according to GB 2763 Appendix A implementation, the crystallization of honey samples will be evenly stirred. For samples of crystalline honey, in a sealed case, the vials are placed in a water bath of not more than 60 ° C and warmed and shaken until all the samples Melt and stir well, quickly cooled to room temperature, in the melting must pay attention to prevent moisture evaporation. Load a clean container, seal, mark the mark. 6.2 Sample storage The sample is stored at room temperature. 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 Weigh the sample 1 g (accurate to 0.01 g) in a 15 mL centrifuge tube, add 10 mL of 0.02 mol/L sodium hydroxide solution at.2000 r/min Under the vortex shock, mix. 7.2 Purification Transfer the extract to the HLB solid phase extraction column and add 3 mL of water to the centrifuge tube. Use 3 mL of water and 1 mL 10 mmol/L sulfuric acid solution leaching column, discard the leaching solution, dry. Eluted with 2 mL of acetonitrile and collected in 10 mL of the test tube At room temperature, nitrogen blowing near dry, accurately add 1.0 mL of acetonitrile. water (3 7, V/V), the oscillation dissolved, over 0.22 μm filter for determination. 7.3 Determination 7.3.1 Liquid Chromatography-Mass Spectrometry Reference Conditions. A) Column. C18 column length 50 mm, inner diameter 4.6 mm, particle size 1.8 μm, or equivalent; B) mobile phase. acetonitrile - 0.1% formic acid solution, gradient elution program in Table 1; Table 1 Mobile phase gradient elution program Time (min) 0.1% Formic acid solution (%) Acetonitrile (%) 0.0 70 30 2.0 70 30 4.0 5 95 7.0 5 95 7.1 70 30 13.0 70 30 C) Flow rate. 0.50 mL/min; D) Column temperature. 30 ° C; E) Injection volume. 10 μL; F) ion source. electrospray ion source (ESI); G) Scanning mode. positive ions; H) Monitoring methods. Multiple reaction monitoring (MRM); I) Mass spectrum conditions are given in Appendix A. 7.3.2 Determination and confirmation of chromatography According to the content of the test compound in the sample solution, the standard working solution with similar peak area is selected, and the standard working solution and sample solution The reaction values of the test compounds in the standard working solution and the sample solution shall be within the linear range of the instrument detection, and the standard working curve According to external standard method. The reference retention times of chlordimeform and 4-chloro-o-toluidine were 1.3 and 4.4 min, respectively, under the above chromatographic conditions, And 4-Chloro-o-toluidine standard Multi-reaction detection (MRM) chromatograms are given in Appendix B, Figure B.1. The sample and standard working solution were determined according to the liquid chromatography-mass spectrometry conditions. The mass retention time of the sample was corresponding to that of the standard The retention time deviation is within ± 2.5%; and the relative abundance of the qualitative ions of each component in the sample is corresponding to the standard working solution in close proximity The relative abundance of qualitative ions is compared, the deviation does not exceed the range specified in Table 2, it can be determined that there is a corresponding analyte in the sample. Table 2 The maximum allowable deviation of relative ion abundance when qualitative confirmation Relative ion abundance > 50% > 20% ~ 50% > 10% ~ 20% ≤10% Allowable relative 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 expressedUse the chromatographic data processor or calculate the amount of chlordimeform or 4-chloro-o-toluidine in the sample by the following formula (1). MΑsi VCsiAi X .. (1) Where. The residual content of chlordimeform or 4 - chloro - o - toluidine in the sample, in milligrams per kilogram (mg/kg); Ai - the peak area of chlordimeform or 4-chloro-o-toluidine in the sample solution; V - the final volume of the sample solution in milliliters (mL); Asi - the standard working solution of the peak area of chlordimeform or 4-chloro-o-toluidine; Csi - the concentration of chlordimeform or 4-chloro-o-toluidine in standard working solution in micrograms per milliliter (μg/mL); M - the amount of sample that the final sample represents, 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 this method is 5 μg/kg. 10.2 Recovery rate The addition rates of chlordimeform and 4-chloro-o-toluidine in different matrices are shown in Appendix C when the level is 5,10,20 μg/kg.Appendix A(Informative) Electrospray ionization source Reference conditions. A) ionization source mode. electrospray ionization; B) ionization source polarity. positive mode; C) Detection method. multiple reaction monitoring; D) atomization gas. nitrogen; E) Atomizing gas pressure. 0.207 MPa (30 psi); F) Capillary voltage. 4000 V; G) Dry gas temperature. 350 ° C; H) Dry gas flow rate. 9 L/min; I) Resolution. Unit resolution; (E), qualitative ion pairs (m/z), and quantitative ion pairs (m/z) are shown in Table A.1; Table A.1 Qualitative ion pairs of chlordimeform and 4-chloro-o-toluidine, quantitative ion pair, fragmentation voltage, collision energy name Qualitative ion pair (M/z) Quantitative ion pair (M/z) Fragmentation voltage (V) Collision energy (EV) Chlordimeform 197.1/117.1 197.1/117.1 130 197.1/125 33 4-Chloro-o-toluidine 142/106.7 21 Non-commercial declaration. The reference mass spectrometry conditions listed in Appendix A are performed on an Agilent 6410B LC/MS/MS LC/MS, where the test instrument The model is for reference only and does not involve commercial purposes and encourages standard users to try different manufacturers or models of instruments.Appendix B(Informative) Chlordime and 4-chloro-o-toluidine standard multi-reaction detection (MRM) chromatograms Figure B.1 Chlordimeform and 4-Chloro-o-toluidine Standard Multi-Reaction Monitoring (MRM) Mass Chromatogram (5 ng/mL)Appendix C(Informative) The recovery of chlordimeform and 4-chloro-o-toluidine in different matrices Table C.1 Recovery range of the method (n = 10) sample name Add concentration (Μg/kg) 4 - Chloro - o - toluidine Recovery rate range (%) Coefficient of variation% Recovery rate range (%) Coefficient of variation% Acacia honey 5 86.4 ~ 102.0 7.5 86.2 ~ 105.3 8.6 10 88.3 ~ 110.3 8.3 87.1 ~ 111.4 7.0 20 86.9 to 111.2 7.6 88.8 to 111.4 8.3 Vitex 5 86.7 ~ 109.6 8.6 86.2 ~ 109.3 8.7 10 76.2 ~ 100.5 7.5 92.3 ~ 108.8 9.8 20 81.5 to 110.2 10.2 88.0 to 114.3 9.0 Honeycomb honey 5 86.3 ~ 109.8 9.0 85.6 ~ 112.2 9.9 10 75.8 ~ 101.0 10.2 90.8 ~ 110.8 10.0 20 82.6 ~ 109.8 9.7 90.7 ~ 105.0 6.7 Mango 5 86.9 to 99.7 4.8 87.4 to 107.6 6.2 10 82.6 ~ 101.5 7.9 87.9 ~ 112.5 9.7 20 83.0 to 112.2 9.7 89.5 to 106.9 6.4 Wild honey 5 86.1 to 113.8 9.2 86.2 to 112.2 9.8 10 81.4 ~ 101.2 8.1 93.4 ~ 110.5 8.6 20 83.1 to 101.1 7.4 87.8 to 110.6 8.0Appendix 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 23200.96-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.96-2016_English as soon as possible, and keep you informed of the progress. 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