GB 23200.73-2016 English PDFUS$239.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.73-2016: Food safety national standard -- Determination of rotenone and azadirachtin residues in food by liquid chromatography-mass spectrometry / mass spectrometry Status: Valid
Basic dataStandard ID: GB 23200.73-2016 (GB23200.73-2016)Description (Translated English): Food safety national standard -- Determination of rotenone and azadirachtin residues in food by liquid chromatography-mass spectrometry / mass spectrometry Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 12,162 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): SN/T 3264-2012 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.73-2016: Food safety national standard -- Determination of rotenone and azadirachtin residues 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 rotenone and azadirachtin residues in food by liquid chromatography - mass spectrometry/mass spectrometry National Standards of People's Republic of China GB Replace SN/T 3264-2012 National standards for food safety Determination of the residue of rotenone and azadirachtin in food Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of rotenone and azadirachtin 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 3264-2012 "Detection methods of rotenone and azadirachtin residues in export food by liquid chromatography-mass spectrometry Spectrum method ". Compared with SN/T 3264-2012, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name and scope of the "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 3264-2012. National standards for food safety Determination of rotenone and azadirachtin residues in food by liquid chromatography - mass spectrometry/mass spectrometry1 ScopeThis standard specifies methods for the determination of rotenone and azadirachtin residues in food by liquid chromatography-mass spectrometry/mass spectrometry. This standard applies to rice, cauliflower, apple, fungus, tea, honey, liver, fish, shrimp, chicken, milk rotenone And azadirachtin residues in 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 rotenone and azadirachtin in the sample were extracted with acetonitrile, and the extract was salted out by sodium chloride and degreased with n-hexane. The polystyrene- Dimethylbenzene-pyrrolidone polymer filler solid phase extraction column purification, liquid chromatography - mass spectrometry/mass spectrometry detection and confirmation, external standard statutory 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). Chromatographically pure. 4.1.2 n-hexane (C6H10). pure chromatography. 4.1.3 Methanol (CH3OH). 4.1.4 Formic acid (HCOOH). Chromatographic pure. 4.1.5 Sodium chloride (NaCl). 4.1.6 Ammonium acetate (CH3COONH4). 4.1.7 Sodium bicarbonate (NaHCO3). 4.2 solution preparation 4.2.1 Saturated sodium bicarbonate solution. Weigh a certain amount of sodium bicarbonate dissolved in water to saturation. 4.2.2 5mmol/L ammonium acetate buffer. Weigh 0.38 g of ammonium acetate dissolved in 800 mL of water, add 2 mL of formic acid, the water volume to 1000 ML. 4.3 standards 4.3.1 Reference substance (rotenone. English name Rotenone, molecular formula C23H22O6, CAS No. 83-79-4, molecular weight 394.42; Azadirachtin. English name Azadirachtin, molecular formula C35H44O16, CAS No.11141-17-6, molecular weight 720.71). purity ≥98%. 4.4 standard solution preparation 4.4.1 rotenone and azadirachtin standard stock solution (100 mg/L). accurately weighed 0.0100 g of rotenone and azadirachtin standard substance, with a The alcohol was dissolved and set to 100 mL, and the standard stock was kept at 4 ° C for no more than one month. 4.4.2 rotenone and azadirachtin standard working solution. according to the need to take appropriate standard stock solution, 20% acetonitrile aqueous solution diluted to the appropriate concentration Of the standard working fluid, temporary with the distribution. 4.5 Materials 4.5.1 Solid phase extraction column of polystyrene-divinylbenzene-pyrrolidone polymer filler. 60 mg, 3 mL. Use 3 mL before use Methanol, 3 mL water pretreatment. 4.5.2 Filtration. 0.22 μm, organic.5 instruments and equipment5.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer, Distribution Spray (ESI) Source. 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Centrifuge. 4 500 r/min with 50 mL stoppered plastic centrifuge tube. 5.4 pulverizer. 5.5 Tissue crusher. 5.6 Scroll Mixer. 5.7 Ultrasonic Cleaner. 5.8 solid phase extraction device. 5.9 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, chopped (not washed), with the tissue crusher to sample processed into a slurry, mix, divided into 2, 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 sieve having a diameter of 2.0 mm, mixed, divided into 2 portions, packed in a clean container Inside, 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 milk Take a representative sample of 500 g, mix thoroughly, divide it into 2, into a clean vial, seal and mark it. 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 1 g (accurate to 0.01 g) sample, placed in a 50 mL stoppered plastic centrifuge tube, add 5 mL of saturated sodium bicarbonate solution Shake and soak for 10 min, add 15 mL of acetonitrile, vortex 30 s after ultrasonic extraction 10 min, 4 500 r/min centrifugal 3 min, shift The organic phase, the residue and then add 10 mL of acetonitrile repeated extraction 1 times, combined extract, add about 3 g sodium chloride salting out, 4 500 r/min Centrifuge 3 min centrifugation, take the supernatant, add 2 mL by acetonitrile saturated n-hexane, shaking 1 min, 4 500 r/min centrifugal 3 min Centrifuged, discarded n-hexane layer, acetonitrile layer at 45 ℃ under reduced pressure evaporation to near dry, with 5 mL of 20% methanol water to dissolve the residue, according to 7.2 steps Purification. 7.1.2 Vegetables and fruit samples Weigh 2 g (accurate to 0.01 g) sample, placed in 50 mL stoppered plastic centrifuge tube, add about 2 g sodium bicarbonate and 15 mL Acetonitrile, shake evenly after ultrasonic extraction 10 min, 4 500 r/min centrifugal 3 min, remove the organic phase, the residue and then add 10 mL of acetonitrile weight Extraction of the extraction 1, combined extract, add about 3 g sodium chloride salting out, 4 500 r/min centrifugal 3 min, the supernatant, at 45 ℃ by Pressure rotation to near dry, with 5 mL of 20% methanol water to dissolve the residue, according to 7.2 steps purification. 7.1.3 honey Weigh 2 g (accurate to 0.01 g) The sample was placed in a 50 mL stoppered plastic centrifuge tube, 5 mL of saturated sodium bicarbonate solution was shaken, Add 15 mL of acetonitrile, vortex 30 s after ultrasonic extraction 10 min, 4 500 r/min centrifugal 3 min, remove the organic phase, the residue and then add 10 mL of acetonitrile was repeated 1 times, the combined extract, add about 3 g sodium chloride salting out, 4 500 r/min centrifugation 3 min, take the supernatant, At 45 ° C under reduced pressure rotary evaporation to near dry, with 5 mL of 20% methanol water to dissolve the residue, according to 7.2 steps purification. 7.1.4 milk, fruit juice and wine Weigh 2 g (accurate to 0.01 g) The sample was placed in a 50 mL stoppered plastic centrifuge tube, about 2 g of sodium bicarbonate and 15 mL of acetonitrile was added, After centrifugation for 30 s, the mixture was centrifuged at 4 500 r/min for 3 min, and the organic phase was removed. The residue was added with 10 mL of acetonitrile. Take 1, the combined extract, add about 3 g sodium chloride salting out, 4 500 r/min centrifugal 3 min, take the supernatant, at 45 ℃ under pressure Evaporated to near dry, with 5 mL of 20% methanol water to dissolve the residue, according to 7.2 steps purification. 7.1.5 Fish, meat and meat products Weigh 2 g (accurate to 0.01 g) The sample was placed in a 50 mL stoppered plastic centrifuge tube, 5 mL of saturated sodium bicarbonate solution was shaken, Add 15 mL of acetonitrile, vortex 30 s after ultrasonic extraction 10 min, 4 500 r/min centrifugal 3 min, remove the organic phase, the residue and then add 10 mL of acetonitrile was repeated 1 times, the combined extract, add about 3 g sodium chloride salting out, 4 500 r/min centrifugation 3 min, take the supernatant, Add 5 mL n-hexane, shaking 1 min, 4 500 r/min centrifugal 3 min, discard the n-hexane layer, acetonitrile layer at 45 ℃ under reduced pressure steam Sent to near dry, with 5 mL of 20% methanol water to dissolve the residue, according to 7.2 steps purification. 7.2 Purification The sample extract was rinsed with 5 mL of water and the whole eluent was discarded, dried, eluted with 5 mL of acetonitrile to maintain a flow rate of about 1 ML/min, the eluent was collected and blown to near dry at 45 ° C. The mixture was allowed to settle 1 mL in 20% aqueous acetonitrile and tested for 0.22 μm. 7.3 Determination 7.3.1 Liquid Chromatographic Reference Conditions A) Column. Phenomenex Luna C18 column, 150 mm x 2.0 mm (id), 3 [mu] m, or equivalent; B) Column temperature. 35 ° C; C) mobile phase. acetonitrile - 5 mmol/L ammonium acetate buffer (35 65, V/V); D) Flow rate. 400 μL/min; E) Injection volume. 10 μL. 7.3.2 Mass spectrometry reference conditions A) ion source. electrospray source (ESI), positive ion mode; B) scanning mode. multiple reaction monitoring (MRM); Refer to Table A.1 in Appendix A for other reference mass spectrometry conditions. 7.3.3 Determination and confirmation of chromatography 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 values of rotenone and azadirachtin in the solution should be within the linear response range of the instrument. According to the formula 8 under the results of the calculation. In this method The retention time of rotenone and azadirachtin was about 5.6 min and 4.2 min, and the multi-reaction monitoring (MRM) of rotenone and azadirachtin standards, See Appendix B for chromatograms. Qualitative criteria For sample determination, if the detected chromatographic peak retention time is consistent with the standard sample, and after deducting the background In the spectrum, the relative abundance of each qualitative ion is close to the standard solution spectrum obtained under the same conditions, and the maximum allowable relative deviation The difference does not exceed the range specified in Table 1, it can be judged that there is a corresponding analyte 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% 7.4 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 samples of rotenone and azadirachtin drug residues, the results need to deduct the blank value. X = C × (1) Where. Residue of rotenone or azadirachtin in the sample, in micrograms per kilogram, μg/kg; The concentration of rotenone and azadirachtin solution from the standard working curve, in micrograms per liter, μg/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 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 limits of quantification of rotenone and azadirachtin were 0.0005 mg/kg and 0.002 mg/kg, respectively. 10.2 Recovery rate The added recoveries of rotenone and azadirachtin when added at levels of 0.0005 mg/kg, 0.001 mg/kg, 0.005 mg/kg Record C. Appendix A (1) (Informative) Reference to mass spectrometry conditions Reference mass spectrometry conditions. Capillary voltage. 4 kV; Shielding gas temperature. 320 ℃; Shielding air flow. 10 L/min; Dry air flow. 3 L/min; Collision pressure. 50 psi; Other mass spectral parameters are shown in Table B.1 Table A.1 The main reference mass spectra of rotenone and azadirachtin Compound Monitoring Ion Dwell Time (ms) Voltage (V) Collision Energy (eV) Rotenone 395 > 213 50 160 24 395 > 192 25 Azadirachtin 743 > 725 50 140 28 743 > 625 36 Note. The figures shown in the boldface in the table are quantitative ions. For different mass spectrometry instruments, the instrument parameters may be different and the mass spectrometry parameters should be optimized before the measurement To the best. (1) Non-commercial declaration. The reference mass spectrometry conditions listed in Appendix C are performed on an Agilent 6460 LC/MS, where the test instrument model is only listed For reference, does not involve commercial purposes, encourage standard users to try different manufacturers or models of equipment.Appendix B(Informative) Multi - reaction monitoring chromatogram of rotenone and azadirachtin standard solution Figure B.1 Multi-reaction monitoring chromatograms of rotenone and azadirachtin standard solutionsAppendix C(Informative) The recovery of rotenone and azadirachtin in different matrices Table C.1 Data on the recovery of rotenone and azadirachtin residues Sample name rotenone azadirachtin Add concentration (μg/kg) Recovery rate range (%) Add concentration (μg/kg) Recovery rate range (%) Rice 0.5 83.5 to 102.0 2 75.2 to 104.5 1 84.6 ~ 101.8 4 79.6 ~ 105.2 5 79.3 ~ 97.8 20 80.5 ~ 101.3 cauliflower 0.5 81.0 to 103.0 2 84.8 to 106.5 1 79.4 to 96.8 4 80.1 to 102.4 5 80.8 ~ 108.7 20 78.9 ~ 100.3 apple 0.5 81.0 to 96.0 2 81.4 to 102.8 1 79.6 ~ 98.4 4 86.6 ~ 106.5 5 78.4 ~ 100.3 20 90.1 ~ 102.4 Fungus 0.5 81.0 to 99.0 2 82.1 to 108.2 1 79.0 ~ 99.8 4 85.6 ~ 104.4 5 81.4 ~ 104.5 20 81.4 ~ 104.8 tea 0.5 78.0 to 103.0 2 74.6 to 107.6 1 78.8 ~ 102.2 4 76.2 ~ 100.3 5 77.4 ~ 99.7 20 78.9 ~ 104.8 honey 0.5 84.0 to 101.0 2 79.4 to 102.8 1 80.2 ~ 97.6 4 80.5 ~ 103.2 5 80.5 to 99.7 20 80.5 to 100.5 milk 0.5 76.2 ~ 104.3 2 78.6 ~ 109.6 1 76.4 ~ 106.6 4 76.2 ~ 95.5 5 76.2 ~ 102.8 20 81.9 ~ 106.8 Liver 0.5 75.0 to 98.0 2 77.2 to 106.5 1 78.4 ~ 103.2 4 76.3 ~ 101.5 5 76.8 ~ 100.1 20 81.8 ~ 100.7 Fish 0.5 79.0 to 105.0 2 77.5 to 100.3 1 79.6 ~ 101.2 4 76.2 ~ 101.7 5 80.7 to 103.0 20 80.9 to 98.4 Shrimp 0.5 81.0 to 97.0 2 77.2 to 102.8 1 80.6 ~ 101.8 4 79.2 ~ 105.3 5 80.3 ~ 96.3 20 82.7 ~ 101.4 chicken 0.5 83.0 to 97.0 2 78.6 to 104.5 1 80.4 ~ 104.2 4 79.3 ~ 93.8 5 81.2 ~ 96.9 20 81.9 ~ 106.8Appendix 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 23200.73-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.73-2016_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 23200.73-2016_English with my colleagues?Answer: Yes. The purchased PDF of GB 23200.73-2016_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. |
