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Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.74-2016: Food safety national standard -- Determination of Jinggangmycin Residue in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry Status: Valid
Basic dataStandard ID: GB 23200.74-2016 (GB23200.74-2016)Description (Translated English): Food safety national standard -- Determination of Jinggangmycin Residue in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 12,190 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): SN/T 2387-2009 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.74-2016: Food safety national standard -- Determination of Jinggangmycin Residue 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 - Determination of Jinggangmycin Residue in Food by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry GB National standards for food safety Determination of Jinggangmycin Residue in Food Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of effectiveamycin residue 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 National Standards of People's Republic of China Instead of SN/T 2387-2009 ForewordThis standard replaces SN/T 2387-2009 "Determination of Jinggangmycin Residue in Import and Export Food by Liquid Chromatography-Mass Spectrometry/Mass Spectrometry". Compared with SN/T 2387-2009, 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"; - "liquid chromatography - mass spectrometry/mass spectrometry" in the standard name to "liquid chromatography - tandem mass spectrometry"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 2387-2009. National standards for food safety Determination of Jinggangmycin Residue in Food by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry1 ScopeThis standard specifies the method for the determination of Jinggangmycin residues in food by liquid chromatography-mass spectrometry/mass spectrometry. This standard applies to rice, cabbage, onions, carrots, tomatoes, cucumbers, spinach, fungus, pear, lemon, almonds, tea, pork, Pig liver, tilapia, shrimp in the detection and confirmation of Jinggangmycin residues, 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 document. 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 of Jinggangmycin residues in methanol aqueous solution extraction, by HLB solid phase extraction column or ethyl acetate liquid extraction and purification, with liquid chromatography - Mass spectrometry/mass spectrometer detection and confirmation, external standard method quantitative.4 reagents and materialsUnless otherwise specified, the reagents used in this method are pure liquid chromatography, water in line with GB/T 6682 in the provisions of a water. 4.1 Reagents 4.1.1 Ammonium acetate (CH3COONH4, CAS number. 631-61-8). 4.1.2 Methanol (CH3OH, CAS No. 67-56-1). 4.1.3 Acetonitrile (CH3CN, CAS No. 75-05-8). 4.1.4 Ethyl acetate (CH3COOCH2CH3, CAS number. 141-78-6). 4.1.5 glacial acetic acid (CH3COOH, CAS number. 64-19-7). 4.2 solution preparation 4.2.1 methanol solution (9 1). the amount of 90 mL of methanol by adding 10 mL of water, mix. 4.2.2 5 mmol/L ammonium acetate buffer solution. Weigh 0.385 g of ammonium acetate, dissolved in water and fixed to 1 000 mL, adjusted with glacial acetic acid PH to 4.5 ± 0.1. 4.3 standards 4,3.1 Jinggangmycin standard (Validamycin A, molecular formula. C20H35NO13, CAS. 37248-47-8). purity ≥ 91.0%. 4.4 standard solution preparation 4.4.1 Jinggangmycin standard stock solution. Weigh 2 mg (accurate to 0.1 mg) the standard of Jinggangmycin, dissolved in water and set to 25 mL of a brown volumetric flask to prepare a standard stock solution at a concentration of 80 mg/L. 4.4.2 Jinggangmycin matrix standard working solution. according to the need, with blank samples in accordance with the sample treatment steps to get the extract, preparation is not With the concentration of the matrix standard solution, is now available. 4.5 Materials 4.5.1 HLB column. 6 mL /.200 mg or equivalent; activated with 6 mL of methanol and 6 mL of water before use. 4.5.2 Filtration. 0.22 m, biphasic.5 instruments and equipment5.1 Liquid Chromatography - Mass Spectrometry/Mass Spectrometer. Atmospheric Pressure Chemical Ionization Source (APCI). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 vortex mixer. 5.4 Homogenizer. 5.5 Centrifuge. speed greater than 3 000 r/min. 5.6 nitrogen blowing concentrator. 5.7 Centrifuge tube. 50 mL Teflon centrifuge tube and 50 mL stopper glass centrifuge tube. 5.8 scale tube. 30 mL, the smallest scale of 0.1 mL. 5.9 pH meter. the amount of 0.1.6 Sample preparation and storage6.1 Sample requirements During sample preparation, the sample should be protected from contamination or changes in residue content. 6.2 Tea and cereals Approximately 500 g of the representative sample, ground and ground through the mill and passed through a 2.0 mm round hole screen, mixed and sealed in a clean container. Remember, stored at 0 ℃ ~ 4 ℃ refrigerated. 6.3 vegetables and fruits To replace the sample of about 500 g, chopped, the multi-functional food mixer fully mashed evenly, into a clean container sealed, marked mark, Frozen at -18 ℃ below the storage. 6.4 nuts Approximately 500 g of the sample was taken and ground thoroughly with an attritor and passed through a 20 mm round hole screen, mixed, sealed in a clean container, marked with a mark, Store at 0 ℃ ~ 4 ℃. 6.5 animal muscle, liver, fish, shrimp Replace the sample part of about 500 g, chopped, by the multi-functional food mixer fully mashed evenly, into a clean container sealed, marked Note, in -18 ℃ below the frozen storage. Note. The above sample sampling site according to GB 2763 Appendix A implementation.7 Analysis steps7.1 Extraction 7.1.1 Rice, edible fungus, almonds Weigh 2.5 g sample (accurate to 0.01 g), placed in 50 mL polytetrafluoroethylene centrifuge tube, add 20 mL of methanol solution, with homogenizer high Rapid homogenate extraction 2 min, 3 000 r/min centrifugation 5 min, collecting supernatant in a scale tube. The residue after centrifugation was dissolved in 5 mL of methanol The supernatant was combined once the above extraction step was repeated and the nitrogen was concentrated to 2.5 mL below the nitrogen bath at 45 ° C to be purified. 7.1.2 cabbage, onions, carrots, tomatoes, cucumber, spinach, pear, lemon, pork, liver, fish, shrimp Weigh 2.5 g sample (accurate to 0.01 g), placed in 50 mL polytetrafluoroethylene centrifuge tube, add 20 mL of methanol, homogenizer high speed uniform Pulp extraction 2 min, 3 000 r/min centrifugation 5 min, collecting supernatant in a scale tube. The residue after centrifugation was diluted with 5 mL of methanol solution Repeat the above extraction step 1, the supernatant, in 45 ℃ water bath blowing nitrogen concentrated to 2.5 mL below, to be purified. 7.1.3 Tea Weigh 1 g of sample (accurate to 0.01 g), add 1.5 mL of water, mix, and the rest according to 7.1.1. 7.2 Purification 7.2.1 Solid phase extraction (SPE) purification The resulting solution from 7.1 was transferred to a pretreated HLB solid phase extraction column and the sample solution was passed through solid phase extraction at a flow rate of about 1 drop/s Column, rinse the column with 2 mL of water, collect all the effluent and eluent to a scale tube, add water to a volume of 5.00 mL, mix, over 0.22 m Filter for determination. 7.2.2 liquid - liquid distribution purification The resulting solution in 7.1 was fixed to 5.00 mL with water, mixed into a 50 mL stoppered glass centrifuge tube, 5 mL of ethyl acetate was added, Vortex oscillation 3 min, 3 000 r/min centrifugal 5 min, discard the upper ethyl acetate phase, and then 5 mL ethyl acetate repeated operation once. Too 0.22 m filter for liquid chromatography-tandem mass spectrometry. 7.3 Determination 7.3.1 Liquid Chromatographic Reference Conditions Column. HILIC (250 mm × 4.6 mm, particle size 5 m), or equivalent. Mobile phase. acetonitrile 5 mmol/L ammonium acetate buffer solution, gradient elution (see Table 1). Flow rate. 1 000 L/min. A) Column temperature. 35 ° C. B) Injection volume. 10 μL. Table 1 Gradient elution conditions for liquid chromatography Time/min 5 mmol/L ammonium acetate buffer solution /% acetonitrile /% 0.0 20 80 4.0 45 55 10.0 45 55 10.1 20 80 16.0 20 80 7.3.2 Mass spectrometry reference conditions See Appendix A for the mass spectrometric conditions. 7.3.3 Determination and confirmation of chromatography Under the optimum working condition of the instrument, according to the content of the compound in the sample solution, the substrate standard working solution with similar peak height is selected, Quality standard working solution and sample solution volume measurement. With the peak area as the ordinate, the concentration of abscissa to draw the standard working curve, with The standard working curve is used to quantify the sample, and the response values of the test compound to be tested in the working solution and the sample solution should be measured linearly Within range. In the above instruments, the reference retention time of Jinggangmycin is about 8.10 min; the calibration curve for the calibration product of Jinggangmycin is given in Appendix B Figure B.1. Table 2 in the same experimental conditions, the sample solution to be tested material retention time, and the matrix standard working solution retention time deviation of ± 2.5% And the relative abundance of the qualitative ion pairs in the sample solution is compared with the matrix standard working solution close to the concentration. The deviation does not exceed the standard It is determined that there is a corresponding analyte in the sample. Table 2 Maximum allowable deviation of relative ion abundance using liquid chromatography-mass spectrometry/mass spectrometry Relative ion abundance 50% 20% to 50% 10% to 20% 10% Permissible relative deviation 20% 25% 30% 50% 7.4 blank test In addition to the sample, according to the above determination steps.8 results are calculated and expressedUsing the external standard method, according to formula (1) to calculate the sample of Jinggangmycin residues, the results should be deducted blank value. Vc X (1) Where. X - the amount of Jinggangmycin residues in micrograms per kilogram (g/kg); C - the concentration of the component to be measured in the sample from the standard working curve, in micrograms per liter (g/L); V - the final volume of the sample solution in milliliters (mL); M - 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 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 limit of quantification of this method was 10 μg/kg. 10.2 Recovery rate When adding levels of 10 μg/kg, 25 μg/kg, 50 μg/kg, the recovery rates of Jinggangmycin in different substrates are given in Appendix C.Appendix A(Informative) Reference to mass spectrometry conditions Reference mass spectrometry conditions. A) Ionization mode. Atmospheric pressure Chemical ionization positive ion mode (APCI). B) Mass Spectrometry. Multiple Reaction Monitoring (MRM). C) Resolution. Unit resolution. D) air curtain gas pressure (CUR). 207 KPa (nitrogen). E) Corona discharge current (NC). 5.00 μA. F) Atomization temperature (TEM). 600 ° C. G) Atomizing gas pressure. 138 KPa (nitrogen). H) Impact air pressure (CAD). 34.5 KPa (nitrogen). I) Other mass spectral parameters are shown in Table A.1. Table A.1 Main reference mass spectrometry parameters Compounds Ion pair (M/z) Dwell time Ms To cluster voltage (DP)/V Inlet voltage (EP)/V Collision energy (CE)/eV Collision cell outlet voltage (CXP)/V Jinggangmycin 498.3/336.3 100 75 3 31.74 12.08 498.3/178.1a 100 75 3 38.57 12.08 498.3/142.2 100 75 3 48.77 12.08 Note. For different mass spectrometry instruments, the instrument parameters may be different, before the determination of the mass spectrometry parameters should be optimized to the best. A ion pair is a quantitative ion pairAppendix B(Informative) Standard multi-reaction monitoring (MRM) chromatograms Figure B.1 Multi-reaction monitoring (MRM) chromatogram of Jinggangmycin standard solution Ion pair 498.3/336.3 Ion pair 498.3/178.1 Ion pair 498.3/142.2Appendix C(Informative) Addition Recovery of Jinggangmycin in Different Substrates Table C.1 Recovery of Jinggangmycin in Different Substrates Sample Concentration/μg/kg Recovery Range /% Sample Concentration/μg/kg Recovery Range /% Rice 10 87.2 ~ 101.8 10 86.6 ~ 111.0 25 92.8 ~ 101.6 25 87.2 ~ 108.8 50 89.2 ~ 100.8 50 87.2 ~ 113.6 cabbage 10 96.8 to 109.4 lemon 10 86.2 to 111.6 25 94.4 ~ 108.0 25 89.6 ~ 102.4 50 96.0 ~ 108.0 50 87.6 ~ 106.8 10 94.6 ~ 108.4 almond 10 90.6 ~ 105.4 25 93.6 ~ 109.6 25 87.2 ~ 111.2 50 93.6 ~ 108.0 50 99.6 ~ 113.2 carrot 10 91.6 ~ 109.2 tea 10 86.0 to 107.8 25 91.2 ~ 105.6 25 87.2 ~ 106.4 50 91.2 ~ 108.4 50 86.8 ~ 104.0 tomato 10 91.6 ~ 107.2 pork 10 89.4 ~ 105.6 25 91.2 ~ 111.2 25 87.2 ~ 108.0 50 94.8 ~ 111.6 50 88.0 ~ 101.6 cucumber 10 98.6 ~ 111.4 Liver 10 90.0 to 106.4 25 89.6 ~ 108.8 25 92.0 ~ 106.4 50 95.2 ~ 111.6 50 87.2 ~ 106.4 spinach 10 87.0 ~ 104.2 Tilapia 10 88.8 ~ 107.2 25 92.8 ~ 108.8 25 96.8 ~ 112.8 50 89.6 to 108.0 50 88.4 to 113.2 Fungus 10 92.8 to 107.2 10 93.4 ~ 106.2 25 92.8 ~ 109.6 25 93.6 ~ 113.6 50 89.2 ~ 108.8 50 88.0 ~ 112.0 IXAppendix 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 23200.74-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.74-2016_English as soon as possible, and keep you informed of the progress. 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