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Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.56-2016: Food safety national standard -- Determination of Quinoxaline Residue in Food Status: Valid
Basic dataStandard ID: GB 23200.56-2016 (GB23200.56-2016)Description (Translated English): Food safety national standard -- Determination of Quinoxaline Residue in Food Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 14,120 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): SN/T 2319-2009 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.56-2016: Food safety national standard -- Determination of Quinoxaline Residue in Food---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 Quinoxaline Residue in Food National Standards of People's Republic of China GB Instead of SN/T 2319-2009 National standards for food safety Determination of Quinoxaline Residue in Food National food safety standards- Determination of quinoxyfen residue in foods 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 2319-2009 "Method for the detection of quinoxaline residues in food for import and export". Compared with SN/T 2319-2012, 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 2319-2009. National standards for food safety Determination of Quinoxaline Residue in Food1 ScopeThis standard specifies the method of liquid chromatography and liquid chromatography-mass spectrometry/mass spectrometry for the determination of quinoxaline residues in foodstuffs. This standard applies to soybean, cauliflower, cherry, fungus, wine, tea, honey, liver, chicken, eel quinoxyline residues The amount of the determination and confirmation, 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 quinoxaline in the sample was extracted with ethyl acetate or saturated sodium bicarbonate solution - ethyl acetate extraction, NH2 solid phase extraction column Or gel permeation chromatography combined with NH2 solid phase extraction column purification, liquid chromatography or liquid chromatography-mass spectrometry/mass spectrometry detection and confirmation, external 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 N-Hexane (C6H10). Chromatographic pure. 4.1.2 Ethyl acetate (C4H8O2). Chromatographic purity. 4.1.3 Acetonitrile (CH3CN). Chromatographic Purification. 4.1.4 Methanol (CH3OH). Chromatographic Purification. 4.1.5 Cyclohexane (C6H12). Chromatographic pure. 4.1.6 Acetone (C3H6O). Chromatographic pure. 4.1.7 Sodium bicarbonate (NaHCO3). 4.1.8 anhydrous sodium sulfate (Na2SO4). dried at 650 ℃ for 4 h before use, sealed and stored. 4.2 solution preparation 4.2.1 Cyclohexane-ethyl acetate solution (1 1, V/V). 50 mL of cyclohexane and ethyl acetate were mixed and mixed. 4.2.2 5% acetone-n-hexane solution. Remove 5 mL of acetone in 95 mL n-hexane and mix well. 4.2.3 50% acetonitrile - water solution. 50 mL of acetonitrile and 50 mL of water were collected and mixed. 4.2.4 saturated sodium bicarbonate solution. Weigh a certain amount of sodium bicarbonate dissolved in aqueous solution to saturation. 4.3 standards 4.3.1 Quinoxaline standard substance (English name Quinoxyfen, molecular formula C15H8Cl2FNO, CAS No.124495-18-7, molecular weight 308.14). purity ≥ 98%. 4.4 standard solution preparation 4.4.1 Quinoxaline standard stock solution (100 mg/L). accurately weighed 0.0100 g quinoxaline standard substance, dissolved in methanol and volume to 100 mL, the standard stock solution at 4 ℃ can be stored for three months. 4.4.2 quinoxaline standard working solution. according to the need to take appropriate standard stock solution, 50% acetonitrile aqueous solution diluted to the appropriate concentration of standard workers For liquid. The standard stock solution can be stored at 4 ° C for one month. 4.5 Materials 4.5.1 Amino (NH2) solid phase extraction column. 500 mg, 3 mL. 4.5.2 Filtration. 0.45 μm, 0.22 μm, organic.5 instruments and equipment5.1 Liquid Chromatograph with UV or Diode Array Detector. 5.2 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer, Distribution Spray (ESI) Source. 5.3 Analysis of balance. 0.01 g and 0.0001 g. 5.4 Gel Permeation Chromatography. 5.5 Centrifuge. 4 500 r/min with 100 mL stoppered plastic centrifuge tube. 5.6 pulverizer. 5.7 Tissue crusher. 5.8 Scroll Mixer. 5.9 Ultrasonic cleaner. 5.10 solid phase extraction device. 5.11 nitrogen blowing instrument.6 Preparation and storage of samples6.1 Preparation of the sample 6.1.1 Fruits and vegetables Take a representative sample 500 g, cut it (not water wash), with the tissue crusher to sample processed into a slurry, mix, divided into 2 copies, into a clean container, sealed and identified. 6.1.2 Tea, grain and nuts Take a representative sample of 500 g, crushed by a pulverizer and passed through a 2.0 mm round hole sieve, mixed, divided into 2 portions, packed in a clean container, Sealed and identified. 6.1.3 Meat and meat products Take a representative sample 500 g, chopped after the use of tissue crusher sample processed into a slurry, mix, into a clean container, divided into 2 Part, sealed and identified. 6.1.4 honey Take a representative sample of 500 g, and stir the honey sample without crystallization. For crystalline samples, in confined cases, Placed in a water bath of not more than 60 ℃ in the warm, shaking, until the sample all melt and stir well, quickly cooled to room temperature, divided into 2, into the clean Net vial, sealed and identified. 6.1.5 Juice, wine and so on All the original samples were poured into a clean mix bucket, stirred thoroughly and mixed, and the mixed samples were dispensed into two portions, each about 500 ML, sealed and identified. In the sample preparation process, should prevent the sample contamination or the occurrence of residue content changes. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Tea, wine, honey, milk, grain stored at 0 ~ 4 ℃, vegetables, fruits, meat and meat products stored at -18 ℃.7 Analysis steps7.1 Extraction 7.1.1 samples of tea, cereals and nuts Weigh 5 g (accurate to 0.01 g) sample, placed in a 100 mL stoppered plastic centrifuge tube, add 15 mL of saturated sodium bicarbonate solution Shake for 10 min, add 20 mL of ethyl acetate, vortex 30 s after ultrasonic extraction 20 min, 4 500 r/min centrifugation 3 min, shift The organic phase was added and the residue was further extracted with 20 mL of ethyl acetate. The extracts were combined, dried over anhydrous sodium sulfate and rotated at 50 ° C Evaporated to near dry, add 5 mL n-hexane, vortex 30 s dissolved residue, according to 7.2.2 purification steps. 7.1.2 Vegetables and fruit samples Weigh 10 g (accurate to 0.01 g) sample, placed in a 100 mL stoppered plastic centrifuge tube, add 30 mL of ethyl acetate, shake all After centrifugation for 20 min, 4 500 r/min centrifugation 3 min, remove the organic phase, the residue and then add 20 mL of ethyl acetate repeat extraction 1 The combined extracts were dried over anhydrous sodium sulfate and evaporated to near dryness at 50 ° C. After addition, 5 mL of n-hexane and vortex Slag, according to 7.2.2 steps purification. 7.1.3 Juice, honey, wine and so on Weigh 10 g (accurate to 0.01 g) The sample was placed in a 250 mL stoppered flask with 10 mL of saturated sodium bicarbonate solution, 30 mL Ethyl acetate, shake evenly after ultrasonic extraction 20 min, 4 500 r/min centrifugal 5 min, remove the organic phase, the residue and then add 20 mL B Ethyl acetate repeated extraction 1 times, combined extract, dried over anhydrous sodium sulfate after 50 ° C rotary evaporation to near dry, add 5 mL n-hexane, Vortex 30 s dissolved residue, according to 7.2.2 steps purification. 7.1.4 Meat and meat products Weigh 10 g (accurate to 0.01 g) The sample was placed in a 100 mL stoppered plastic centrifuge tube, 10 mL of saturated sodium bicarbonate solution was added, 30 mL of ethyl acetate, homogenized at 10 000 r/min homogenously 30 s, 4 500 r/min centrifugal 5 min, remove the organic phase, residual Slag and then add 20 mL of ethyl acetate repeated extraction 1 times, combined extract, dried over anhydrous sodium sulfate after 50 ° C rotary evaporation to near dry, Add 10 mL of cyclohexane-ethyl acetate, shake the residue for 30 s, centrifuge at 4 500 r/min for 5 min, press 7.2.1 and 7.2.2 Sequence of purification. 7.2 Purification 7.2.1 Gel permeation chromatography For the extract obtained in 7.1.4, take 5 mL into the gel column through the sample loop and operate according to the following conditions. A) Purification column. Bio-Beads S-X3 filler, 25 (id) ×.200 mm (id); B) Mobile phase. cyclohexane-ethyl acetate (1 1, V/V); C) Flow rate. 4.2 mL/min; The effluent from 9.5 to 21.5 min was collected and evaporated to near dry at 50 ° C. Add 5 mL of n-hexane to solid phase extraction. The Note. If the amount of fat contained in the sample of 5.00 g is greater than 0.5 g, the volume of the sample extract should be adjusted so that it is injected into the 5 mL sample of the gel chromatogram Of the amount of fat is not greater than 0.5 g. 7.2.2 solid phase extraction column purification Pre-leach the column with 3 mL of methanol and 3 mL of n-hexane before use. The sample extract was washed with 5 mL of n-hexane and discarded The eluent was eluted with 5 mL of 5% acetone-n-hexane to maintain a flow rate of about 1 mL/min. The eluate was collected and blown at 50 ° C to near- With 50% acetonitrile - aqueous solution volume 1 mL, over 0.45 μm filter for high performance liquid chromatography determination; or 50% acetonitrile aqueous solution volume 5 mL, 0.22 μm filter for liquid chromatography-mass spectrometry/mass spectrometry. Determination of liquid chromatography 7.3.1 Liquid Chromatographic Reference Conditions A) Column. Waters Symmetry C18 column, 4.6 x 250 mm (id), 5 μm, or equivalent; B) Mobile phase. acetonitrile - water (75 25, V/V); C) Flow rate. 1.0 mL/min; D) Detection wavelength. 235 nm; E) Injection volume. 40 μL; 7.3.2 Determination by liquid chromatography The standard working curve was drawn with the standard working solution of quinoxaline standard, and the standard working curve was drawn with the peak area as the ordinate and the working solution concentration as the abscissa. The working curve is used to quantify the sample. The response values of quinoxaline in standard working fluid and sample solution should be within the linear response range of the instrument. Press 8 Under the provisions of the results of the calculation. Under the present method, the retention time of quinoxaline was about 8.0 min. Refer to Appendix A for standard chromatograms Figure A.1. 7.4 Determination by liquid chromatography - mass spectrometry/mass spectrometry 7.4.1 Liquid Chromatography - Mass Spectrometry/Mass Spectrometry Reference Conditions A) Column. Acquity UPLC BEH C18 column, 2.1 x 55 mm (id), 1.7 μm, or equivalent; B) Column temperature. 30 ° C; C) mobile phase. acetonitrile - water (70 30, V/V); D) Flow rate. 300 μL/min; E) Injection volume. 10 μL. 7.4.2 Mass spectrometry reference conditions A) ion source. electrospray source (ESI), positive ion mode; B) scanning mode. multiple reaction monitoring (MRM); Other reference mass spectrometry conditions are given in Table B.1 in Appendix B. 7.4.3 Determination by liquid chromatography-mass spectrometry/mass spectrometry According to the sample content of the sample, select the appropriate response value of the standard working solution for chromatographic analysis. Standard working fluid and sample to be tested The response value of quinoxaline in the solution should be within the linear response range of the instrument. According to the provisions of 8 to calculate the results. Under the conditions of this method, Oxygen retention time of about 1.5 min, the cone voltage of 30 V, the standard secondary mass spectrometry and multi-reaction monitoring (MRM) chromatography See Figure C.1 and Figure C.2 in Appendix C, respectively. 7.4 Qualitative determination When the sample is measured, if the detected chromatographic peak retention time is consistent with the standard sample, and in the sample spectrum after subtracting the background, The relative abundance of the qualitative ions is close to the standard solution of the standard solution obtained under the same conditions compared to the maximum allowable relative deviation does not exceed the table 1 in the range, you can determine the existence of the corresponding sample in the sample. Table 1 Maximum allowable deviation of relative ion abundance when qualitative confirmation Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% 7.5 blank experiment In addition to the sample, according to the above steps.8 results are calculated and expressedUse the data processing software or according to formula (1) to calculate the residual amount of quinoxylin in the sample, the calculation results need to deduct the blank value. X = C × (1) Where. The residual amount of quinoxaline in the sample is in milligrams per kilogram, mg/kg; Concentration of quinoxaline solution from standard working curve in milligrams per liter, mg/L; The final volume of the sample solution, in milliliters, mL; The mass of the 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 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, recovery rate 10.1 Quantitation limits The limit of quantification for liquid chromatography was 0.01 mg/kg. The quantitation limit of the liquid chromatography-mass spectrometry/mass spectrometry is 0.001 mg/kg. 10.2 Recovery rate When the levels were 0.01 mg/kg, 0.02 mg/kg, 0.04 mg/kg, the recovery of quinoxaline was measured by liquid chromatography. Appendix D (Table D.1). When the levels were 0.001 mg/kg, 0.005 mg/kg, 0.01 mg/kg, the concentration of quinoxaline was determined by liquid chromatography-mass spectrometry The recovery is shown in Appendix D (Table D.2).Appendix A(Informative) The chromatogram of quinoxaline Figure A.1 Liquid chromatogram of quinoxaline Appendix B (1) (Informative) Reference to mass spectrometry conditions Reference mass spectrometry conditions. Capillary voltage. 0.5 kV; Source temperature. 120 ° C; Solvent temperature. 450 ° C; Taper hole air (nitrogen). 45 L/Hr; Solvent gas stream (nitrogen). 900 L/Hr; Collision air pressure (argon). 2.20 × 10-6 Pa; Duration. 0.20 s Other mass spectral parameters are shown in Table C.1 Table B.1 Basic reference mass spectra of quinoxaline (M/z) ion (m/z) dwell time (s) taper hole voltage (V) collision energy (eV) Quinoxaline 308.2 272.1 197.1 * 0.2 0.2 Note. the table with * ions for the quantitative ions; for different mass spectrometry equipment, instrument parameters may be different, should be measured before the mass spectrometry The number of optimization to the best. (1) Non-commercial declaration. The reference to the mass spectrometric conditions listed in Appendix C is performed on a Waters UPLC/Priemer 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) The secondary spectrum of quinoxaline and the multi - reaction monitoring (MRM) ion chromatogram Figure C.1 The quaternary spectrum of quinoxaline Figure C.2 Quinoxyline Multiple Reaction Monitoring (MRM) Ion Chromatography ---------Appendix D(Informative) Sample concentration and recovery of the experimental data Table D.1 Data on the recovery of quinoxaline residues by liquid chromatography Sample Name Add Concentration (mg/kg) Recovery (%) Soybeans 0.010 75.2 ~ 104.5 0.020 76.2 to 92.9 0.040 81.8 ~ 93.0 cauliflower 0.010 76.6 ~ 106.5 0.020 90.1 to 102.4 0.040 94.9 to 100.3 Cherry 0.010 81.4 ~ 102.8 0.020 83.2 ~ 98.0 0.040 86.6 ~ 98.4 Fungus 0.010 89.6 ~ 108.2 0.020 84.2 to 104.4 0.040 88.9 to 104.8 wine 0.010 77.2 to 102.8 0.020 79.2 ~ 98.2 0.040 82.8 to 97.2 tea 0.010 74.6 ~ 107.6 0.020 76.2 ~ 100.3 0.040 78.9 to 94.8 honey 0.010 79.4 ~ 102.8 0.020 91.9 to 99.7 0.040 84.8 ~ 95.6 Liver 0.010 74.6 ~ 106.5 0.020 76.3 to 101.5 0.040 80.7 to 96.9 eel 0.010 74.6 to 100.3 0.020 76.2 to 97.7 0.040 80.9 to 98.3 chicken 0.010 74.6 ~ 104.5 0.020 78.3 ~ 93.8 0.040 81.6 to 94.1 Table D.2 Liquid Chromatography Quirgine Ling Drug Residue Recovery Recovery Data Sample Name Add Concentration (mg/kg) Recovery (%) Soybeans 0.001 83.5 to 102.0 0.005 84.6 ~ 101.8 0.010 79.3 ~ 97.8 cauliflower 0.001 81.0 to 103.0 0.005 79.4 ~ 96.8 0.010 78.7 to 97.7 Cherry 0.001 81.0 to 99.0 0.005 79.6 ~ 98.4 0.010 78.4 to 100.3 Fungus 0.001 81.0 to 96.0 0.005 79.0 to 99.8 0.010 81.4 ~ 104.5 wine 0.001 81.0 to 97.0 0.005 80.6 ~ 100.8 0.010 81.3 to 96.3 tea 0.001 78.0 to 106.0 0.005 78.8 ~ 103.8 0.010 77.4 to 99.7 honey 0.001 84.0 to 101.0 0.005 80.2 ~ 97.6 0.010 77.1 to 99.7 Liver 0.001 75.0 to 98.0 0.005 78.4 to 103.2 0.010 76.8 to 100.1 eel 0.001 79.0 to 96.0 0.005 79.6 ~ 101.2 0.010 76.2 to 103.0 chicken 0.001 84.0 to 97.0 0.005 77.8 to 96.6 0.010 81.2 to 96.9Appendix E(Normative appendix) Laboratory repeatability requirements Table E.1 Laboratory repeatability requirements Measured component content Mg/kg Precision 0.001 36 > 0.01 > 1 14Appendix F(Normative appendix) Inter-laboratory reproducibility requirements Table F.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 23200.56-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.56-2016_English as soon as possible, and keep you informed of the progress. 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