GB 23200.66-2016 English PDFUS$219.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.66-2016: Food safety national standard -- Determination of Pseudo-mite Residue in Food by Gas Chromatography -- Mass Spectrometry Status: Valid
Basic dataStandard ID: GB 23200.66-2016 (GB23200.66-2016)Description (Translated English): Food safety national standard -- Determination of Pseudo-mite Residue in Food by Gas Chromatography -- Mass Spectrometry Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 11,169 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): SN/T 2646-2010 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.66-2016: Food safety national standard -- Determination of Pseudo-mite Residue in Food 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 Pseudo - mite Residue in Food by Gas Chromatography - Mass Spectrometry Replace SN/T 2646-2010 National standards for food safety Determination of Pyridine Residue in Food Gas chromatography - mass spectrometry National food safety standards- Determination of tebufenpyrad residue in foods 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 National Standards of People's Republic of China GB ForewordThis standard replaces SN/T 2646-2010 "Method for the determination of picamadine residues in food for import and export by gas chromatography-mass spectrometry" Compared with SN/T 2646-2010, 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 2646-2010. National standards for food safety Determination of Pseudo - mite Residue in Food by Gas Chromatography - Mass Spectrometry1 ScopeThis standard specifies the detection and preparation of picamadine residues in food, gas chromatography-mass spectrometry and confirmation methods. This standard applies to the amount of pyridine residues in spinach, lotus root, strawberry, peanut, chicken, pork, cod, honey, chestnut and tea 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 date of the note applies 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 samples were extracted with acetonitrile, washed with n-hexane liquid and magnesium silicate solid phase extraction column, and analyzed by gas chromatography-negative chemical mass spectrometry. 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 Acetone (C3H6O). Residue level. 4.1.2 acetonitrile (C2H3N). pesticide residues. 4.1.3 N-Hexane (C6H14). Pesticide Residue. 4.1.4 sodium chloride (NaCl). 650 ℃ burning 4 h, placed in a dryer cooling, standby. 4.2 solution preparation 4.2.1 Acetone - n-Hexane (3 7). Take 300 mL of acetone, add 700 mL of n-hexane and shake well. 4.3 standards 4.3.1 Pyridine standard (Tebufenpyrad, C18H24ClNO). purity ≥ 96.5%. 4.4 standard solution preparation 4.4.1 Preparation of Pymartamine Standard Solution. Accurately weigh the appropriate standard, dissolve with a small amount of acetone, and prepare the concentration of acetone 1.0 mg/mL of standard stock solution. According to the need to use acetone - n-hexane diluted to the appropriate concentration of standard working solution. Store at -18 ° C In the refrigerator, 4.5 Materials 4.5.1 Cleanert Florisil Solid phase extraction column. 500 mg, 3 mL or equivalent.5 instruments and equipment5.1 Gas Chromatography-Mass Spectrometer. A negative chemical source. 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Solid phase extraction device. 5.4 Homogenizer. 5.5 Rotary evaporator. 5.6 Nitrogen Concentrator. 5.7 with a plug centrifuge tube. 50 mL, 100 mL. 5.8 Concentrated bottles. 50 mL, 100 mL. 5.9 Pipettes. 1 mL, 2 mL, 5 mL, 10 mL.6 Preparation and storage of samples6.1 Preparation of the sample 6.1.1 Grain Take a representative sample volume of 500 g, grind all with an attritor and pass through a 2.0 mm round hole screen. Mix, are divided into two as a test Kind, divided into a clean container, sealed, marked mark. 6.1.2 fruit or vegetables Take a representative sample 500 g, chopped, followed by the use of food mashed the sample processed into a slurry. Mix well into a clean capacity Inside, sealed, marked mark. 6.1.3 Meat and meat products Take a representative sample 500 g, fully mashed by the crusher, into a clean container as a sample. Sealed, marked. 6.1.4 honey and bee products Take a representative sample volume of 500 g, the crystallization of honey samples will be evenly stirred; on the crystallization of honey samples, in the Sealed, the sample bottle placed in not more than 60 ℃ in the water bath in the warm, shaking, until the sample all melted and stir well, quickly cooled To room temperature, in the melting must pay attention to prevent moisture evaporation. Load a clean container, sealed, marked with a mark. 6.1.5 Tea Take a representative sample of 500 g, grind all with an attritor and pass through a 2.0 mm round hole screen. Mix well and clean the clean container Inside, sealed, marked mark. 6.1.6 nuts Take a representative sample 500 g, all grinding with an attritor. Mix, are divided into two as a sample, into the clean clean Container, enclosed, marked mark. 6.1.7 Aquatic products Take a representative sample of 500 g, remove about 1 kg from the sample, take the edible part of the crusher fully mashed evenly Into two copies, respectively, into the clean container as a sample. Sealed and marked. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Grain samples are stored at 0-4 ° C; fruits and vegetables and other samples are cryopreserved at -18 ° C or lower. In sampling and sample preparation During the operation, the sample should be protected from contamination or changes in the content of the residue.7 Analysis steps7.1 Extraction Weigh 10 g of sample (accurate to 0.1 g) in a 100 mL stoppered centrifuge tube, add 10 mL of water, add 50 mL of saturated Acetonitrile, homogenized high-speed homogenate extraction 2 min (soy sauce and honey only violent oscillation 10 min), then add 5 g sodium chloride, violent Shock 10 min, 3000 r/min centrifugal 10 min. 7.2 Purification 7.2.1 Liquid/liquid distribution purification Take 20 mL of extract (spinach, lotus root, strawberry) or 10 mL (peanut, chicken, pork, cod, honey, chestnut and tea) Leaves) transferred to 50 mL with a plug centrifuge tube, add 10 mL of saturated n-hexane, shaking 3 min, standing stratified, abandoned the upper And the mixture was repeated with 10 mL of n-hexane. The n-hexane phase was discarded and the lower acetonitrile phase was collected in a 100 mL concentrated flask. 40 ℃ water bath concentrated to nearly 1 mL. 7.2.2 Solid phase extraction (SPE) purification Before use with 5 mL of acetone - n-hexane pre-sprayed Florisil column. The sample was poured into a column and washed with 12 mL of acetone-n-hexane Off, control flow rate less than or equal to 2 mL/min. The whole eluate was collected in a 50 mL concentration flask, concentrated in a 40 ° C water bath to near dryness, Nitrogen blown dry. With acetone - n-hexane dissolved and set to 1.0 mL, gas chromatography - mass spectrometry. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. HP-5 MS quartz capillary column, 30 m × 0.25 mm (id), film thickness 0.25 μm, or equivalent; B) column temperature. the initial temperature of 70 ℃, 30 ℃/min program temperature to.200 ℃, keep 10 min, then 50 ℃/min The program was heated to 270 ° C for 4 min. C) Inlet temperature. 250 ° C; D) chromatographic - mass spectrometer interface temperature. 280 ° C; E) Carrier gas. helium, purity greater than or equal to 99.999%, constant pressure mode, column head pressure 1.45 Mpa); F) Injection volume. 1 μL; G) Injection method. no split injection, 0.65 min after the opening valve; H) ionization mode. negative chemical ionization; I) ion source temperature. 150 ° C; J) quadrupole temperature. 150 ° C; K) reactant gas. methane, purity ≥99.99%; L) Determination of the way. select the ion monitoring mode; M) select the monitoring ion (m/z). quantitative 318, qualitative 320,333,335; N) solvent delay. 4.0 min. 7.3.2 Determination and confirmation of chromatography According to the sample content of the sample, the selected concentration of similar standard working solution, the standard working solution and sample volume and other volume The response value of pyridoxamine in standard working solution and sample solution should be within the linear range of instrument detection. If the sample solution is in the selective ion chromatogram of the standard working solution, a chromatographic peak appears at the same retention time, In the sample quality chromatogram, the selected ions are present, the abundance of the selected ions is greater than the abundance ratio of the corresponding ions Within the allowable range (see Table 1). Under the condition of 7.3.1, the retention time of pyridoxamine was 16.18 min, and the monitoring ion (m/z) Which was confirmed by m/z318,320,333,335 (its abundance ratio was 100. 39. 95. 33). According to the quantitative ion m/z318 The amount of external standard method. The total ion chromatogram and full scan mass spectrometry of the gas chromatographic-mass spectrometry of the pyramidamine standard under 7.3.1 Appendix A, Figures A.1 and A.2. Table 1 Maximum qualitative error of relative ion abundance when qualitative gas chromatography-mass spectrometry Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50%8 results are calculated and expressedUse the chromatographic data processor or (1) to calculate the amount of tetrafluoroether residues in the sample. H × c × V X = ------------------------------. (1) Hs × m In formula (1). X - the amount of diclofenam residues in milligrams per kilogram (mg/kg); H - the peak of pyrrolidazole in the sample solution; Hs - standard chromatographic peak of picarbamate; C - the concentration of pyridoxamine in standard working fluid in micrograms per milliliter (μg/mL); 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 reproducibility and its arithmetic mean (percentage) Together with the requirements of Appendix C. 9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) Together with the requirements of Appendix D. 10% limit and recovery rate 10.1 Quantitation limits The quantification limit of this method is 2 μg/kg. 10.2 Recovery rate When adding levels of 0.002 mg/kg, 0.004 mg/kg, 0.01 mg/kg, see Table B for the recovery of picamines.Appendix A(Informative) The total ion chromatogram of picarbamate standard substance 1 5 .5 0 1 6 .0 0 1 6 .5 0 1 7 .0 0 1 7 .5 0 1 8 .0 0 1 8 .5 0 Time - - > Abundance TIC. 1 0 0 PPB .D \\ data .ms 1 6 .1 8 5 Min Figure A.11 Total ion chromatogram of picidamine standard Mass Spectrometry of Pyridine Acetate Reference Substance 3 0 8 3 1 0 3 1 2 3 1 4 3 1 6 3 1 8 3 2 0 3 2 2 3 2 4 3 2 6 3 2 8 3 3 0 3 3 2 3 3 4 3 3 6 3 3 8 3 4 0 3 4 2 3 4 4 M/z - - > Abundance Scan 1 5 7 5 (1 6. 2 1 0 points). 1 0 0 PPB .D \\ data .ms Figure A.2 Pymartamine Standard Substance Mass SpectrometryAppendix B(Informative) The recovery rate in different matrices Table B.1 Addition recovery in different matrices Sample concentration (μg/kg) Recovery rate range (%) Sample addition concentration (μg/kg) Recovery rate range (%) spinach 2 90.0 ~ 110.0 Codfish 2 90.0 ~ 110.0 4 95.0 to 107.5 4 92.5 to 107.5 10 97.0 to 112.0 10 97.0 to 119.0 2 95.0 to 110.0 honey 2 90.0 ~ 110.0 4 97.5 to 110.0 4 92.5 to 107.5 10 96.0 to 112.0 10 96.0 to 112.0 Strawberry 2 81.5 ~ 100.8 Chestnut 2 95.0 ~ 115.0 4 92.5 to 107.5 4 92.5 to 107.5 10 96.0 to 112.0 10 95.0 to 114.0 peanut 2 90.0 ~ 110.0 tea 2 90.0 ~ 110.0 4 90.0 to 112.5 4 97.5 to 112.5 10 94.0 to 117.0 10 97.0 to 113.0 chicken 2 90.0 ~ 110.0 pork 2 90.0 ~ 110.0 4 95.0 to 107.5 4 92.5 to 112.5 10 94.0 to 112.0 10 94.0 to 112.0Appendix C(Normative appendix) Laboratory repeatability requirements Table C.1 Laboratory repeatability requirements Measured component content Mg/kg Precision 0.001 36 > 0.01 > 1 14Appendix D(Normative appendix) Inter-laboratory reproducibility requirements Table D.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 23200.66-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.66-2016_English as soon as possible, and keep you informed of the progress. 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