GB 23200.27-2016 English PDFUS$179.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.27-2016: Food safety national standard -- Determination of 4,6-dinitro-o-cresol Residue in Fruits by Gas Chromatography -- Mass Spectrometry Status: Valid
Basic dataStandard ID: GB 23200.27-2016 (GB23200.27-2016)Description (Translated English): Food safety national standard -- Determination of 4,6-dinitro-o-cresol Residue in Fruits by Gas Chromatography -- Mass Spectrometry Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 9,910 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): SN/T 1734-2006 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.27-2016: Food safety national standard -- Determination of 4,6-dinitro-o-cresol Residue in Fruits by Gas Chromatography -- 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 4,6 - dinitro - o - cresol Residue in Fruits by Gas Chromatography - Mass Spectrometry National Standards of People's Republic of China GB Instead of SN/T 1734-2006 National standards for food safety Determination of 4,6 - dinitro - o - cresol Residue in Fruits Gas chromatography - mass spectrometry National food safety standards- Determination of 4, 6-dinitro-cresol residue in fruits Gas 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 1734-2006 "Test Method for Residue of 4,6-Dinitro-o-cresol in Import and Export Fruits Gas Chromatography-Mass Spectrometry law". Compared with SN/T 1734-2006, 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 fruit" to "fruit". - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 1734-2006. National standards for food safety Determination of 4,6 - dinitro - o - cresol Residue in Fruits by Gas Chromatography - Mass Spectrometry1 ScopeThis standard specifies the method for the determination of 4,6-dinitro-o-cresol residues in fruit by gas chromatography-mass spectrometry. This standard applies to the apple, pear 4,6 6-dinitro-o-cresol residue test, 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 methods.3 principleFruit sample 4,6-dinitro-o-cresol residue extracted with dichloromethane, blowing nitrogen to dry after acetonitrile dissolved, with N- (p-butyl dimethyl (MTBSTFA), which was determined by gas chromatography-mass spectrometry and quantified by external standard method.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 dichloromethane (CH2Cl2). excellent grade pure. 4.1.2 acetonitrile (CH3CN). pure chromatography. 4.1.3 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, placed in the dryer in the spare. 4.1.4 Derivative reagent N- (tert-butyldimethylsilyl) -N-methyltrifluoroethylphthalide (MTBSTFA). 99% purity. 4.2 standards 4.2.1 4,6-dinitro-o-cresol standard (C7H6N2O5, CAS No .. 534-52-1). purity 99%. 4.3 standard solution preparation 4.3.1 4,6-dinitro-o-cresol standard stock solution. accurately weighed 10 mg 6,6-dinitro-o-cresol standard, dissolved in acetonitrile and prepared Into the concentration of 100 rng/L of the standard stock solution, can be stored in the refrigerator 0 ℃ ~ 4 ℃ for 3 months. 4.3.2 4,6-dinitro-o-cresol standard working solution. according to the need for acetonitrile will be 4,6-dinitro-o-cresol standard stock solution diluted to the appropriate concentration Degree of standard working fluid, can be stored in the refrigerator 0 ℃ ~ 4 ℃ for 1 month.5 instruments and equipment5.1 Gas Chromatography - Mass Spectrometer, with electron bombardment source. 5.2 Analysis of balance. 0.0001 g and 0.01 g. 5.3 Crusher. 5.4 Centrifuge..2000 r/min. 5.5 Scroll Mixer. 5.6 blowing nitrogen enrichment instrument. 5.7 incubator. 5.8 Polypropylene centrifuge tube. 15 mL, with plug.6 Preparation and storage of samples6.1 Preparation of the sample Replace the sample of about 500 g, the sampling site according to GB 2763 Appendix A implementation, (not available washing) chopped, with a crusher will sample The product is processed into a slurry, mixed, packed into a clean container, sealed and marked. 6.2 Sample storage Samples stored at -5 ° C in the dark. During sample preparation, the sample should be protected from contamination or changes in the residue content.7 Analysis steps7.1 Extraction Weigh 1 g (accurate to 0.01 g) of the prepared homogeneous sample in a 15 mL centrifuge tube, add 3 g of anhydrous sodium sulfate and 5 mL of dichloromethane, Mix thoroughly for 3 min on a vortex mixer and centrifuge at 2 000 r/min for 5 min. Transfer the dichloromethane to another 15 mL centrifuge tube, With 5 mL of methylene chloride repeated extraction time, combined extract, 50 ℃ nitrogen blowing concentrated to near dry. 7.2 Derivatization After drying in nitrogen, add 0.4 mL of acetonitrile to the centrifuge tube and add 100 μL of MTBSTFA, sealed at 80 ° C Derived 1 h. Standard working fluid also added 100 μL MTBSTFA, sealed, under the above conditions for derivatization. After derivatization 0.22 μm microporous membrane was determined by gas chromatography-mass spectrometry. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. HP-5MS quartz capillary column. 30 m × 0.25 mm (inner diameter) × 0.25 μm film thickness, or equivalent. B) Column temperature. 100 ° C (1 min) 30 ° C/min 180 ° C (1 min) 50 ° C/min 205 ° C 10 ° C/min 260 ° C (20 min). C) Inlet temperature. 210 ° C. D) Transmission line temperature. 250 ° C. E) Carrier gas. helium, purity 99.999%, flow rate 1.0 mL/min. F) Injection volume. 1 μL. G) Injection method. no split injection, 1 min, open the diverter valve, split ratio of 20. 1. H) ionization mode. EI. I) Ionization energy. 70 eV. J) Measurement method. Select the ion monitoring mode (SIM). K) monitoring of ions. m/z 255,209,239,179, quantitative ion m/z 255. L) solvent delay. 5 min. 7.3.2 Determination and confirmation of chromatography According to the content of 4,6-dinitro-o-cresol in the sample, the standard working solution with similar concentration of sample peak area was selected. Derivatized The response values of the 4,6-dinitro-o-cresol derivative in the standard working solution and the sample should be within the linear range of the instrument. Derivative After the standard working solution and sample volume to participate in the measurement. The retention time of the 4,6-dinitro-o-cresol derivative under the above chromatographic conditions About 9.31 min. Under the same experimental conditions, the chromatographic retention time of the test substance in the sample was the same as that of the standard working solution and after subtracting the background Of the selected ions in the sample mass chromatogram, the abundance of the selected ions is compared to the abundance ratio of the corresponding ions of the standard, Within the allowable range (see Table 1) allows you to determine the corresponding sample in the sample. Standard SIM chromatograms and full scan spectra See Appendix A, Figure A.1, Figure A.2. Table 1 Maximum allowable error for relative ion abundance using gas chromatography-mass spectrometry 7.4 blank experiment In addition to the sample, according to the above determination steps.8 results are calculated and expressedThe content of 4,6-dinitro-o-cresol in the sample was calculated according to the following formula (1) MΑs VCsA .. (1) Where. The content of 4,6-dinitro-o-cresol in the X-sample, in milligrams per kilogram, mg/kg; The peak area of 4,6 - dinitro - o - cresol derivative in A - AS - standard working solution 4,6 - dinitro - o - cresol derivative peak area; Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% C - Concentration of 4,6 - dinitro - o - cresol in standard working solution in milligrams per liter, mg/L; M - the final sample quality of the sample, in grams, g; V - the final volume of the sample solution, in milliliters, mL. 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 The quantitation limit of this method 4, 6-dinitro-o-cresol is 0.01 mg/kg. 10.2 Recovery rate The recoveries of 4, 6 - dinitro - o - cresol were between 74.0% and 105.0% at the concentration of 0.01 mg/kg. The recoveries of 4, 6 - dinitro - o - cresol were between 72.0% and 101.0% at the concentration of 0.05 mg/kg. The recoveries of 4, 6 - dinitro - o - cresol were between 81.1% and 105.0% at the concentration of 0.10 mg/kg.Appendix A(Informative) 4, 6-dinitro-o-cresol standard-MTBSTFA derivative gas chromatography-mass spectrometry Figure A.2 SIM spectra of 4, 6-dinitro-o-cresol-MTBSTFA derivatives Figure A.1 SIM chromatogram of 0.5 mg/L 4,6-dinitro-o-cresol-MTBSTFA derivativeAppendix 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 23200.27-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.27-2016_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of GB 23200.27-2016_English with my colleagues?Answer: Yes. The purchased PDF of GB 23200.27-2016_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet.Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to Sales@ChineseStandard.net. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay. |
