GB 23200.75-2016 English PDF

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GB 23200.75-2016: Food safety national standard -- Determination of Residual Potassium Amide Residues in Foods
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GB 23200.75-2016	279	Add to Cart	3 days	Food safety national standard -- Determination of Residual Potassium Amide Residues in Foods	Valid

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Basic data

Standard ID: GB 23200.75-2016 (GB23200.75-2016)
Description (Translated English): Food safety national standard -- Determination of Residual Potassium Amide Residues in Foods
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Word Count Estimation: 14,178
Date of Issue: 2016-12-18
Date of Implementation: 2017-06-18
Older Standard (superseded by this standard): SN/T 2796-2011
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 23200.75-2016: Food safety national standard -- Determination of Residual Potassium Amide Residues in Foods

---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 Residual Potassium Amide Residues in Foods ICS National Standards of People's Republic of China GB Instead of SN/T 2796-2011 National standards for food safety Determination of Residual Potassium Amide Residues in Foods National food safety standards- Determination of flonicamid 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

Foreword

This standard replaces SN/T 2796-2011 "Method for the determination of fluorosolane residues in food for import and export". Compared with SN/T 2796-2011, 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 "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 2796-2011. National standards for food safety Determination of Residual Potassium Amide Residues in Foods

1 Scope

This standard specifies the method of gas chromatography and liquid chromatography-mass spectrometry/mass spectrometry for the determination of diflufenamide residues in food. This standard applies to lettuce, carrots, cabbage, rice, citrus, grapes, chestnuts, beef, sheep liver, chicken, tilapia, Ketone, tea, honey, fluoride in the residual amount of fluoride determination and qualitative confirmation, other food can refer to the implementation.

2 normative reference documents

The 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 methods

3 principle

The samples were extracted with ethyl acetate and purified by gel permeation chromatography (GPC) and solid phase extraction (SPE). Quantitative determination of standard method, confirmed by liquid chromatography - mass spectrometry/mass spectrometry.

4 reagents and materials

Unless otherwise specified, the reagents are of analytical grade and the water is in accordance with the primary water specified in GB/T 6682. 4.1 Reagents 4.1.1 Cyclohexane (C6H12, CAS No. 110-82-7). 4.1.2 Ethyl acetate (C4H8O2, CAS No. 141-78-6). Chromatographic purity. 4.1.3 Methanol (CH3OH, CAS No. 67-56-1). Chromatographic Purification. 4.1.4 Sodium chloride (NaCl, CAS No. 7647-14-5). 4.1.5 anhydrous sodium sulfate (Na2SO4, CAS No. 15124-09-1). 650 ℃ burning 4 h, in the dryer to cool to room temperature, stored in Sealed in a bottle. 4.2 solution preparation 4.2.1 Ethyl acetate-cyclohexane solution (1 1). Take.200 mL of ethyl acetate, add.200 mL of cyclohexane and shake well. 4.2.2 methanol - water solution (9 1). take 900 mL of methanol, add 100 mL of water, shake back. 4.3 standards 4.3.1 Flonicamid (standard) (C9H6F3N3O, CAS number. 158062-67-0). purity ≥98.8%. 4.4 standard solution preparation 4.4.1 Fluoride insect amide standard stock solution (1.0 mg/mL). accurately weighed amount of fluoxetine amide, with ethyl acetate prepared into the concentration A standard stock solution of 1.0 mg/mL. The solution was stored in a refrigerator at -18 ° C. 4.4.2 Fluoride insect amide standard intermediate solution (100 μg/mL). Accurate to absorb the appropriate amount of standard stock solution, diluted with ethyl acetate to the concentration A standard intermediate solution of 100 μg/mL. The solution was stored in a refrigerator at -18 ° C. 4.4.3 Flutamide Amide Standard Working Solution. Standard intermediate solution is diluted with a blank matrix of various samples as appropriate before use. When the concentration of standard working fluid. 4.5 Materials 4.5.1 Amino solid phase extraction column..200 mg, 3 mL and 500 mg, 3 mL, or equivalent. Before use with 2 mL of ethyl acetate live 2 times. 4.5.2 XTR Diatomite Solid Phase Extraction Column. 3000 mg, 15 mL, or equivalent. 4.5.3 Microporous membrane. 0.45 μm, organic phase.

5 instruments and equipment

5.1 Gas Chromatograph. with ECD detector. 5.2 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer. Equipped with electrospray ion source. 5.3 gel permeation chromatography. equipped with automatic concentration equipment. 5.4 Analytical balance. 0.01 g and 0.0001 g. 5.5 high speed homogenizer. 5.6 high-speed low-temperature freeze centrifuge. 10000 r/min. 5.7 Polytetrafluoroethylene plastic centrifuge tube. 50 mL, with lid. 5.8 heart-shaped bottle. 50 mL. 5.9 Test tube. 15 mL. 5.10 Rotary Evaporator. 5.11 Nitrogen Drying Concentrator. 5.12 glass scale tube. 5 mL, 10 mL, with plug.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 lettuce, carrots, cabbage, citrus, grapes, chestnut Take a representative sample of about 500 g, chopped, processed with a crusher into a slurry or fine particles. Mix well into a clean container, close Seal, mark. 6.1.2 Rice, tea Approximately 500 g of representative sample was pulverized and pulverized through a pulverizer and passed through a 1.2 mm round hole. Mix well into a clean container, close Seal, mark. 6.1.3 beef, chicken, sheep liver, tilapia Take a representative sample of about 500 g, minced with a meat grinder, mix well, fit into a clean container, seal, mark the mark. 6.1.4 tomato sauce Take a representative sample of about 500 g, mix, mix into a clean container, seal, mark the mark. 6.1.5 honey To replace the sample of about 500 g, the crystallization of honey samples will be evenly stirred; on the crystallization of honey samples, in the dense In the case of closed, the vials were placed in a water bath of not more than 60 ° C and warmed and shaken until the samples were completely melted and stirred and cooled rapidly Room temperature, in the melting must pay attention to prevent moisture evaporation. Load a clean container, seal, mark the mark. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Tea, honey, grain and nuts and other samples stored at 0 ~ 4 ℃; fruits and vegetables and animal-derived food samples at -18 ℃ The following frozen storage. During sample and sample preparation, the sample should be protected from contamination or changes in the residue content.

7 Analysis steps

7.1 Extraction 7.1.1 lettuce, carrots, cabbage, citrus, grapes, chestnuts, beef, sheep liver, chicken, tilapia, tomato sauce Weigh 10 g (accurate to 0.01 g) sample in 50 mL centrifuge tube, add 15.0 mL ethyl acetate, homogeneous extraction 1 min; Another 50 mL centrifuge tube, add 10 mL of ethyl acetate wash homogenizer knife head, combined homogeneous solution. Add 10 g of anhydrous sodium sulfate, Cover, shake for 10 min. Centrifuge the extract at 10,000 r/min for 5 min, draw 10 mL supernatant, place the refrigerator below 0 ° C. H, then 0.45 μm organic filter, to be gel permeation chromatography purification. 7.1.2 Rice Weigh 10 g (accurate to 0.01 g) sample in a 50 mL centrifuge tube, add 10.0 mL of water, soak for 20 min, add 15.0 mL B Ethyl acetate, homogeneous extraction 1 min, another take a 50 mL centrifuge tube, add 10 mL of ethyl acetate wash homogenizer knife head, combined homogeneous solution. Add 10 g of anhydrous sodium sulfate, cover, shake 10 min. Centrifuge the sample at 10,000 r/min for 5 min, draw 10 mL supernatant, fridge 0 ℃ below placed 10 h, then 0.45 μm organic filter, to be gel permeation chromatography purification. 7.1.3 Tea Weigh 2 g (accurate to 0.01 g) sample in 50 mL centrifuge tube, add 10 mL of water soak for 20 min; add 1 g of anhydrous sulfuric acid sodium. Add 10.0 mL of ethyl acetate, shock extraction 1 0 min, extraction 2 times. Samples were centrifuged at 4000 r/min for 5 min Liquid, constant volume to 20 mL; take 10 mL of 0.45 μm organic phase filter, to be gel permeation chromatography purification. 7.1.4 honey Weigh 2 g sample (accurate to 0.01 g) in 50 mL centrifuge tube, add 3 mL of water, 0.5 g sodium chloride, shake and mix The solid phase extraction column was allowed to stand for 5 min and rinsed with 35 mL of ethyl acetate. The flow rate was controlled at 1 mL/min. The filtrate was collected in 50 mL Concentrated in the bottle, spin at 45 ℃ below the concentration of about 1 mL, to be purified. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 7.2 Purification 7.2.1 lettuce, carrots, cabbage, citrus, grapes, chestnut, rice, beef, sheep liver, chicken, tilapia, tomato sauce, tea The solution obtained in 7.1.1, 7.1.2 and 7.1.3 was taken into 10 mL supergel permeation chromatography to collect 7 to 14 min effluent, 2 mL Ethyl acetate constant volume, as the primary purification solution. After the primary purification solution was passed through the amino column, the flask was washed three times with 1 mL of ethyl acetate, and the washing solution was also passed through the column and the flow rate was controlled to 1 ML/min, the whole eluate was collected in a test tube, concentrated at 45 ° C to near dryness, and the residue was swollen with ethyl acetate to dissolve the residue. Constant volume 1.0 mL, to be tested. 7.2.2 Honey 0.5 g of anhydrous sodium sulfate was filled on the amino column before activation. After the column was purified, the residue was eluted with 2 mL of ethyl acetate And the flow rate was controlled to 1 mL/min. The whole eluate was collected in a test tube and concentrated at about 45 ° C to about 0.5 mL. Ester volume to 1.0 mL, to be tested. 7.3 Determination 7.3.1 Gel Chromatographic Purification Reference Conditions A) gel cleaning column. 300 mm × 25 (id) mm; filler. Bio-Beads, S-X3, 38 μm to 75 μm. B) Concentration temperature. 45 ° C. C) mobile phase. cyclohexane-ethyl acetate (1 1, volume ratio). D) constant volume reagent. ethyl acetate. E) Flow rate. 5 mL/min. F) Injection volume. 5 mL. 7.3.2 Gas Chromatographic Reference Conditions A) Column. DB-1701 capillary column, 30 m × 0.32 mm (id), 0.25 μm, or equivalent. B) heating process. the initial temperature of 80 ℃, keep 1 min, to 15 ℃ per minute rose to 240 ℃, keep 1 min, Clock 10 ℃ up to 260 ℃, keep 10 min. C) Inlet temperature. 260 ° C. D) Detector temperature. 320 ° C. E) Carrier gas. nitrogen (purity 99.999%), flow rate 2.5 mL/min. F) Injection mode. Splitless injection. G) Injection volume. 1.0 μL. 7.3.3 Determination of gas chromatography According to the content of fluoride in the sample solution, the standard working solution with similar peak area was selected. Standard working solution and sample solution The value of the fluphenamide response should be within the linear range of the instrument. Standard working solution and sample solution volume measurement. above Under the conditions of chromatographic conditions, the retention time of flutamide was about 13.1 min. The chromatogram of the standard is shown in Figure A.1 in Appendix A. 7.3.4 LC-MS/MS mass spectrometry reference conditions 7.3.4.1 Liquid Chromatographic Reference Conditions A) Column. Waters Atlantis Hilic Silica Column, 3 μm, 3.0 mm (id) x 50 mm, or equivalent; B) Column temperature. 40 ° C; C) mobile phase. methanol - water (9 1, volume ratio); D) Flow rate. 0.30 mL/min; E) Injection volume. 10 μL. 7.3.4.2 Mass Spectral Reference Conditions See Appendix B. 7.3.5 Determination by liquid chromatography mass spectrometry Ethyl acetate volume of the sample solution for solvent conversion to methanol - water (9 1, volume ratio) and then on the machine. According to the sample in the fluorine The content of the solution was similar to that of the standard working solution. Standard working solution and sample solution of fluoride acid amide reaction value are Should be within the linear range of the instrument. Standard working solution and sample solution volume measurement. Under the above chromatographic conditions, The retention time of the amide was about 1.03 min. The selected component selected one parent ion, two or more child ions, under the same experimental conditions, if the sample to be detected in the sample with the standard The corresponding retention time deviation in the quasi-solution is within ± 2.5%; and the relative abundance of the qualitative ions of each component in the sample spectrum is The relative abundance of the corresponding qualitative ions in the standard solution spectrum is compared with the range specified in Table 1, The samples can be judged to be positive for fluphenectam amide. The spectrum of the standard is shown in Appendix C, C.1, C.2. 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 test In addition to the sample, according to the above determination steps.

8 results are calculated and expressed

Use the chromatographic data processor or (1) to calculate the residual content of the fluoroacetamide in the sample. The result is deducted from the blank. MA VcA S    (1) Where. X - The content of the fluoroacetamide in the sample, in ng/g g/g; The chromatographic peak area of flutamide in A - sample solution; C - the concentration of flutamide in the standard working solution, in ng/ml for ng/mL; V - Final volume of the final solution, in milliliters, mL; AS - standard chromatographic peak area of flutamide in standard working solution; M - the amount of sample that the final sample represents, 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 precision

9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) Comply with the requirements of Appendix E. 9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) Comply with the requirements of Appendix F. 10% limit and recovery rate 10.1 Quantitation limits In this method, the fluconamide in lettuce, carrots, cabbage, citrus, grapes, tea, beef, chicken, sheep liver, tomato sauce The limit of quantitation was 20 μg/kg, and the limit of quantitation in rice, chestnut, tilapia, and honey was 10 μg/kg. 10.2 Recovery rate When the levels were 0.02 mg/kg, 0.04 mg/kg, 0.4 mg/kg, 4 mg/kg, the addition recoveries of flutamide See Appendix D.

Appendix A

(Informative) Gas Chromatographic Spectrum of Flutamide Amide Standard Figure A.1 Gas chromatogram of the fluoroacetamide standard (10 μg/kg) (GC-ECD)

Appendix B

(Informative) Determination of the conditions for the determination of fluoxetine amide mass spectrometry Mass spectrum reference conditions. A) ion source. electrospray ion source (ESI), temperature 500 ° C; B) scanning mode. negative ion scanning; C) Detection method. Multi-reaction selective ion detection (MRM); D) electrospray voltage (IS). 4500 V; E) atomization gas, air curtain gas, auxiliary heating gas, collision gas are high purity nitrogen and other suitable gas; before use should adjust the gas Body flow to make the mass spectrometry sensitivity to meet the testing requirements; F) Auxiliary gas temperature (TEM). 500 ° C; G) Monitoring of ion pairs, doping ions, dwell time, deblocking voltage and collision energy are shown in Table B.1. Table B.1 Fluorinated butanamide monitoring ion pair, quantitative ion pair, dwell time, de-cluster voltage and collision energy Name of the test object Monitor ion pairs / (M/z) Quantitative ion pair / (M/z) Dwell time / (Ms) To cluster voltage / (V) Collision energy / (V) Flutamide amide 228.0/81.1 228.0/81.1 100 -64 -14 228.0/146.0 -30 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. Non-commercial statement. The reference mass spectrometry conditions listed in Appendix B are performed on the API3000 LC/MS, where the test instrument model is only Provide reference, does not involve commercial purposes, to encourage standard users to try different manufacturers or models of equipment.

Appendix C

(Informative) Fluethanone Amide Standard LC/MS-MS Mass Spectrometry Figure C.1 Fluoride insect amide standard ion ion full scan mass spectrometry Figure C.2 Fluoride Amide Standard Multi-Reaction Monitoring (MRM) Chromatogram (20 μg/L)

Appendix D

(Informative) The addition of fluoxetine amide and the recovery rate Table D.1 Fluorinated butyramide addition levels and added recovery sample name Add level (Μg/kg) Recovery rate (%) lettuce 20 92.5 to 112.5 40 87.3 ~ 95.3 400 83.0 ~ 87.8 4000 84.7 to 94.1 Cabbage 20 102.0 to 108.5 40 94.0 ~ 114.5 400 92.9 ~ 100.6 4000 92.5 ~ 106.4 carrot 20 83.0 to 91.5 40 84.3 ~ 95.0 400 90.4 to 95.5 4000 86.7 ~ 100.6 Rice 10 85.0 ~ 99.0 20 82.0 to 90.5 100 90.1 to 98.7 Tangerine 20 101.0 to 116.0 40 90.8 to 107.0 400 101.7 ~ 105.6 grape 20 87.5 to 92.5 40 88.8 ~ 94.3 400 89.4 ~ 106.5 Chestnut 10 89.0 ~ 109.0 20 83.5 ~ 97.0 100 91.1 to 99.3 tea 20 83.0 ~ 99.5 40 83.0 ~ 98.5 500 96.8 ~ 98.7 40000 95.0 ~ 109.9 beef 20 74.5 to 92.5 50 80.2 ~ 95.4 100 87.2 ~ 92.6 Sheep liver 20 78.5 ~ 86.5 80 82.8 to 91.4 200 83.7 to 98.2 chicken 20 80.5 to 91.0 40 80.3 ~ 91.8 100 87.5 ~ 89.6 Tilapia 10 89.0 ~ 97.0 20 80.0 to 85.0 100 84.4 ~ 93.5 ketchup 20 80.5 to 99.5 40 84.8 ~ 98.3 500 84.4 ~ 95.3 2000 96.8 ~ 104.9 honey 10 87.0 to 91.0 20 83.0 to 96.5 100 85.0 to 91.4

Appendix E

(Normative appendix) Laboratory repeatability requirements Table E.1 Laboratory repeatability requirements Measured component content Mg/kg Precision 0.001 36 > 0.01 > 1 14

Appendix 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 ......

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