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GB 23200.76-2016 English PDF

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GB 23200.76-2016: Food safety national standard -- Determination of residual amoxicillin residues in food by liquid chromatography-mass spectrometry / mass spectrometry
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GB 23200.76-2016English239 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of residual amoxicillin residues in food by liquid chromatography-mass spectrometry / mass spectrometry Valid GB 23200.76-2016

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Basic data

Standard ID GB 23200.76-2016 (GB23200.76-2016)
Description (Translated English) Food safety national standard -- Determination of residual amoxicillin residues in food by liquid chromatography-mass spectrometry / mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 12,169
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2581-2010
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 23200.76-2016: Food safety national standard -- Determination of residual amoxicillin 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 residual amoxicillin residues in food by liquid chromatography - mass spectrometry/mass spectrometry National standards for food safety Determination of residual amoxicillin residues in foods Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of flubendiamide residue in foods Liquid chromatography - mass spectrometry National Standards of People's Republic of China GB Replace SN/T 2581-2010 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 GB ×××× -xxxx

Foreword

This standard replaces SN/T 2581-2010 "Determination of fenapamide residues in food for import and export by liquid chromatography-mass spectrometry". Compared with SN/T 2581-2010, 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 2581-2010. National standards for food safety Determination of residual amoxicillin residues in food by liquid chromatography - mass spectrometry/mass spectrometry

1 Scope

This standard specifies a liquid chromatography-mass spectrometry/mass spectrometric method for the determination of florfenicol residues in foodstuffs. This standard applies to onions, radishes, tomatoes, orange, soybeans, apples, tea, walnuts, fish, pork, liver and milk Determination and confirmation of residues of amylamide, 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 dated edition applies to this file. 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 acetonitrile in acetonitrile, and the extract was extracted by graphite carbon-amino solid phase extraction column or Florisil solid phase extraction Column chromatography, liquid chromatography - mass spectrometry/mass spectrometry, external standard method.

4 reagents and materials

All reagents in addition to special instructions, are analytical pure, water for the GB/T 6682 of the provisions of a water. 4.1 Reagents 4.1.1 Acetonitrile (C2H3N). Chromatographic pure. 4.1.2 Toluene (C7H8). Chromatographic pure. 4.1.3 n-hexane (C6H14). chromatographic purity. 4.1.4 Acetone (C3H6O). Chromatographic pure. 4.1.5 Sodium chloride (NaCl). 4.1.6 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve. 4.2 solution preparation 4.2.1 acetonitrile saturated n-hexane. 250 mL of the separatory funnel by adding 150 ml of n-hexane and 50 mL of acetonitrile blending 5 min, take the upper spare. 4.2.2 acetonitrile - toluene (3 1, V/V). measuring the amount of 350 mL of acetonitrile and 150 mL of toluene mixed with spare. 4.2.3 Acetone-n-Hexane (1 1, V/V). Mix.200 mL of n-hexane and.200 mL of acetone in a graduated cylinder. 4.2.4 acetonitrile - water (7 3, V/V). with a measuring cylinder to take 350 mL of acetonitrile and 150 mL of water mixed spare. 4.3 standards 4.3.1 Flubendiamide standard. purity greater than or equal 99%, CAS number. 272451-65-7, molecular formula. C23H22F7IN2O4S, molecular weight 682.39. 4.4 standard solution preparation 4.4.1 Fenofibrate standard stock solution (100 g/mL). accurately weighed the appropriate amount of phenytoin amide standard, with acetonitrile dubbed Standard of 100 g/mL standard stock solution, the standard stock solution placed in a refrigerator at 4 ℃ in the dark sealed. 4.4.2 Fluorobenzene Amide Matrix Standard Working Solution. Standard stock solution is diluted with a blank matrix of various samples as needed before use. Appropriate concentration of standard working fluid. Matrix standard working fluid should be used with the current distribution. 4.5 Materials 4.5.1 Graphite Carbon-Amino Solid Phase Extraction Column. 500 mg/500 mg, 5 mL or equivalent. Pre-leaching with 5 mL of acetonitrile-toluene before addition column. 4.5.2 Florisil Solid Phase Extraction Column. 1000 mg, 5 mL or equivalent. Add 2 mL of acetone and 4 mL of n-hexane before addition Wash the column. 4.5.3 Microporous membrane. 0.2 m, general type.

5 instruments and equipment

5.1 Liquid Chromatography - Mass Spectrometry/Mass Spectrometer. Distribution Spray Ion Source (ESI). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Tissue crusher. 5.4 Homogenizer. 10000 r/min. 5.5 Centrifuge. 4000 r/min. 5.6 Teflon plastic centrifuge tube. 50 mL, with plug. 5.7 Rotary Evaporator. 5.8 nitrogen blowing instrument.

6 Sample preparation and storage

6.1 Preparation of the sample 6.1.1 Tea, soybeans, walnuts Approximately 500 g of the representative sample, crushed by a tissue crusher and passed through a 2.0 mm round hole sieve, mixed, sealed in a clean container, Mark the mark. 6.1.2 onions, radish, tomatoes, orange, apples, fish, pig lean meat, liver To replace the sample about 500 g, chopped, by the tissue crusher fully mashed evenly, into the clean container sealed, marked mark. 6.1.3 Milk Replace the sample with about 500 g, sealed into a clean container, marked with a mark. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Tea, grain, nuts and other samples stored at 0 ℃ ~ 4 ℃; vegetables, fruits, livestock, poultry and other samples at -18 ℃ frozen preservation. In the sample preparation process, should prevent the sample contamination or the occurrence of flunaramide residues in the amount of change.

7 Analysis steps

7.1 Extraction 7.1.1 onions, radishes, tomatoes, orange, soybeans, apples, tea, walnuts Soybeans, walnuts and tea. Weigh 2 g (accurate to 0.01 g) sample in 50 mL centrifuge tube, add 5 mL of water for 0.5 h; Radish, tomato, orange, apple. Weigh 2 g (accurate to 0.01 g) sample in 50 mL centrifuge tube. Add 20 mL of acetonitrile to 10,000 R/min homogenization 1 min, adding 2 g sodium chloride, shake, and centrifuged at 4000 r/min 3 min. Absorb the upper organic phase in the concentrated bottle, the residual Add 15 mL of acetonitrile in the slag, repeat the extraction time, merge the upper organic phase, in 40 ℃ water bath under reduced pressure to near dry, to be purified. 7.1.2 fish, pig lean meat, liver, milk Weigh the sample after 2 g (accurate to 0.01 g) in a 50 mL centrifuge tube, add 2 g of anhydrous sodium sulfate, 20 mL of acetonitrile and 10 mL Acetonitrile saturated n-hexane, homogenized at 10,000 r/min for 1 min, centrifuged at 4000 r/min for 3 min, and the lower organic phase was taken into a concentrated flask. Add 15 mL of acetonitrile residue, repeat extraction time, combined with the lower organic phase, in 40 ℃ water bath under reduced pressure to near dry, to be purified. 7.2 Purification 7.2.1 onions, radishes, tomatoes, orange, soybeans, apples, tea, walnuts The residue was concentrated in 3 x 2 mL acetonitrile-toluene and transferred to a graphite carbon-amino solid phase extraction column and then washed with 15 mL B Nitrile - toluene elution column, control the flow rate of not more than 2.0 mL/min, collecting the whole effluent, concentrated in a 40 ° C water bath under reduced pressure, Near dry, with acetonitrile - water dissolved residue and set to 2.0 mL, filter membrane for analysis. 7.2.2 fish, pig lean meat, liver, milk The residue in the concentrated flask was washed with 3 x 2 mL of n-hexane and transferred to a Florisil solid phase extraction column until all of the solution Phase extraction after adding 2 mL of n-hexane leaching, discard all the effluent. And then 10 mL of acetone - n-hexane elution, control flow rate does not exceed 2.0 mL/min, the whole eluate was collected, concentrated in a water bath at 40 ° C under reduced pressure, and the nitrogen was blown to near dryness. The residue was dissolved in acetonitrile-water and allowed to settle 2.0 mL, filter membrane for analysis. 7.3 Determination 7.3.1 Liquid Chromatography - Mass Spectrometry/Mass Spectrometry Reference Conditions A) Column. C18 column, 2.1  50 mm, 1.7 m or equivalent; B) mobile phase and gradient elution program. see Table 1. Table 1 Mobile phase gradient elution program Time/(min) acetonitrile/(%) water/(%) 0.00 60 40 2.00 100 0 3.00 60 40 C) Flow rate. 0.20 mL/min; D) Column temperature. 35 ° C; E) Injection volume. 2 μL; F) Please refer to Appendix B for mass spectrometry conditions. 7.3.2 Determination and confirmation of chromatography According to the content of fluoxynol in the sample solution, the standard working solution with similar peak area was selected. Standard working solution and sample solution of fluorobenzene The amylose response should be within the linear range of the instrument. If the residue exceeds the standard curve range, the sample extract is applied with acetonitrile (7.1) for proper dilution. Standard working solution and sample solution volume measurement. Under the above chromatographic conditions, florfenicol amide The retention time is about 1.75 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 material and standard The corresponding retention time deviation in the solution is within ± 2.5%; and the relative abundance of the qualitative ions of each component in the sample spectrum is close to the concentration The relative abundance of the corresponding qualitative ions in the quasi-solution spectrum is compared, and the deviation does not exceed the range specified in Table 2. Determination of florfenonamide positive detection. The spectrum of the standard is shown in Appendix A, Figures A.1, A.2. Table 2 The 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 Except that the sample is not weighed, according to the above determination conditions and steps.

8 results are calculated and expressed

Use the chromatographic data processor or (1) to calculate the residual content of florfenicol in the sample, the calculation results need to deduct the blank value. 1000    MA VcA (1) Where. The residual amount of florfenicol in the X-sample, in milligrams per kilogram (mg/kg); The peak area or peak height of florfenicanamide in A sample solution; AS-standard working area of the peak area or peak of fenfenamide; C - the concentration of florfenicanamide in standard working fluid, in ng/ml (ng/mL); M - the mass of the sample represented by the final sample, in grams (g); The final volume of the V-sample solution in milliliters (mL). 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) 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 limit of quantification of this method is 0.005 mg/kg. 10.2 Recovery rate See Appendix C for the recovery of florfenicol.

Appendix A

(Informative) Fluorobenzene Amine Standard LC/MSMS Mass Spectrometry M/z 100 120 140 160 180.200 220 240 260 280 300 320 340 360 380 400 420 440 460 480 500 520 540 560 580 600 620 640 660 680 700 JISU 94 (0.892) Cm (85.94) Daughters of 681ES- 1.85e5254.1 274.1 272.0 681.3 Figure A.1 Ion Full Scanning Mass Spectrometry (Concentration. 5 ng/mL) Min 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 MRM of 2 channels, ES- 681.1 > 254.1 090123-083 Smooth (Mn, 1x2) 3.196e 003 FCXA 1.76 285.49 Min 0.25 0.50 0.75 1.00 1.25 1.50 1.75 2.00 2.25 2.50 2.75 3.00 3.25 3.50 3.75 4.00 4.25 4.50 4.75 5.00 MRM of 2 channels, ES- 681.1 > 274.1 090305-005 Smooth (Mn, 1x2) 3.422e 003 FCXA-2 1.73 326.28 A) b) Figure A.2 Multi-reaction monitoring (MRM) chromatogram of florfenonamide standard (concentration 5 ng/mL)

Appendix B

(Informative) Fluoresuin Amide Liquid Chromatography - Tandem Mass Spectrometry Conditions A) ion source. electrospray ionization source (ESI), anion scanning; B) Detection method. multiple reaction selection ion detection (MRM); C) electrospray voltage (IS). 2500V; D) atomization gas, air curtain gas, auxiliary heating gas, collision gas are high purity nitrogen and other suitable gas; before use should adjust the gas Flow to make the mass spectrometry sensitivity to the detection requirements; E) Auxiliary gas temperature (TEM). 250 ° C; F) ion source temperature. 110 ° C; G) Qualitative ion pair, quantitative ion pair, acquisition time, deblocking voltage and collision energy are shown in Table 1. Table B.1 Fluorobenzene amide monitoring ion pair, quantitative ion pair, deblocking 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) Fenfenamide 681.1/254.1 681.1/254.1 500 -35 -30 681.1/274.1 -20

Appendix C

(Informative) Addition recovery of flumethasone in different substrates Table C.1 Concentration, Recovery and Variation Coefficients of Fenfenamide in Different Matrices (n = 10) Sample name Add concentration (mg/kg) Recovery rate range (%) RSD% 0.005 70.0 to 99.6 14.0 1.50 88.5 to 98.1 4.6 3.00 77.6 ~ 100.4 8.4 radish 0.005 68.0 to 95.6 12.0 0.015 77.5 to 107.8 15.5 0.030 91.0 to 108.7 7.9 tomato 0.005 92.6 ~ 108.9 7.2 0.300 68.0 to 86.0 11.1 0.700 73.0 ~ 86.6 5.6 0.005 61.8 ~ 95.3 17.6 0.010 76.4 ~ 109.6 13.4 0.020 78.6 ~ 110.0 12.8 Soybeans 0.005 68.4 to 91.2 10.7 0.150 78.7 ~ 100.2 9.8 0.300 68.4 ~ 95.4 11.6 apple 0.005 71.7 to 88.4 7.1 0.700 66.3 ~ 72.4 3.1 1.000 91.1 to 94.9 1.4 0.005 68.4 to 97.8 13.7 20.00 75.4 ~ 91.1 7.2 40.00 84.0 ~ 91.5 3.2 walnut 0.005 74.7 to 95.8 8.5 0.030 81.7 ~ 100.7 8.2 0.060 87.8 ~ 98.7 4.5 0.005 88.3 ~ 99.4 4.7 0.010 79.6 ~ 109.6 10.8 0.020 83.6 ~ 110.8 11.8 Pig lean meat 0.005 82.0 ~ 107.1 8.9 0.050 66.6 to 83.4 7.8 0.100 74.6 ~ 81.5 3.2 Liver 0.005 70.8 to 96.1 10.5 0.300 81.7 to 94.3 5.6 0.600 84.3 ~ 101.0 9.7 milk 0.005 87.5 to 100.8 5.2 0.100 74.8 ~ 89.6 7.7 0.200 84.0 ~ 94.5 4.3

Appendix D

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

Appendix 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

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