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GB 23200.53-2016 English PDF

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GB 23200.53-2016: Food safety national standard -- Determination of fenosilazole residues in foodstuffs by gas chromatography-mass spectrometry
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PDF similar to GB 23200.53-2016


Standard similar to GB 23200.53-2016

GB/T 38211   GB/T 18418   GB/T 18419   GB 23200.46   GB 23200.47   GB 23200.45   

Basic data

Standard ID GB 23200.53-2016 (GB23200.53-2016)
Description (Translated English) Food safety national standard -- Determination of fenosilazole residues in foodstuffs by gas chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 11,148
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2236-2008
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 23200.53-2016: Food safety national standard -- Determination of fenosilazole residues in foodstuffs 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 fenosilazole residues in foodstuffs by gas chromatography - mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 2236-2008 National standards for food safety Determination of Fluorosilazole Residue in Food Gas chromatography - mass spectrometry National food safety standards- Determination of flusilazole 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

Foreword

This standard replaces SN/T 2236-2008 "Determination of Fluorosilicon Residue in Import and Export Food by Gas Chromatography-Mass Spectrometry". This standard compared with SN/T 2236-2008, 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 2236-2008. National standards for food safety Determination of fenosilazole residues in foodstuffs by gas chromatography - mass spectrometry

1 Scope

This standard specifies the method for the determination and confirmation of the content of fenosilazole residues in food by gas chromatography-mass spectrometry. This standard applies to rice, soybeans, small cabbage, fresh peas, pears, citrus, peanuts, tea, beef, chicken, shrimp, honey Determination and confirmation of fluorosilazole residues, 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 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 methods

3 principle

Samples were extracted with acetonitrile, fruits and vegetables were graphitized with carbon black and amino solid phase extraction tandem purification, grain, nuts, meat, tea And honey by Florian silica solid phase extraction column purification, gas chromatography - mass spectrometry detection and confirmation, external standard quantitative.

4 reagents and materials

Unless 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 Toluene (C7H8). Chromatographic pure. 4.1.3 n-hexane (C6H14). chromatographic purity. 4.1.4 ether (C4H10O). chromatographic purity. 4.1.5 sodium chloride (NaCl). analytical pure, 650 ℃ burning 4 h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve. 4.1.6 anhydrous sodium sulfate (Na2SO4). analytical pure, 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 n-Hexane - Ether (8 2). take 800 mL of n-hexane, add.200 mL of ether, shake and mix. 4.2.2 acetonitrile - toluene (7 3). take 700 mL of acetonitrile, add 300 mL of toluene, shake ready for use. 4.3 standards 4.3.1 Flusilazole, C16H15F2N3 Si, CAS No. 85509-19-9, molecular weight 315) Standard substance. purity > 99%. 4.4 standard solution preparation 4.4.1 Fenroxazole standard solution. accurately weighed the appropriate amount of fluorosilicone standard material, with acetonitrile dubbed the concentration of 100 g/mL standard reserve liquid. According to the need to use acetonitrile diluted to the appropriate concentration of standard working fluid. The standard stock solution is stored in 0 ℃ ~ 4 ℃ refrigerator, valid for 12 Month, the standard working fluid in 0 ℃ ~ 4 ℃ refrigerator to save, valid for 6 months. 4.5 Materials 4.5.1 Graphitized Carbon Black Solid Phase Extraction Column. Envi-Carb, 6 mL, 500 mg or equivalent. 4.5.2 Amino solid phase extraction column. Sep-Pak, 3 mL, 500 mg or equivalent. 4.5.3 Florisil Solid Phase Extraction Column. LC-Florisil, 6 mL, 1 g or equivalent. Before addition, add 5 mL of n-hexane-ether (8 2) Pre-leaching column. 4.5.4 Tandem Column. About 20 mm high anhydrous sodium sulphate was added to the graphitized carbon black solid phase extraction column, and the column was ligated to an amino solid phase extraction The top of the column was pre-leached with 5 mL of acetonitrile-toluene (7 3).

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. Equipped with an electron impact source (EI). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Centrifuge. speed greater than 5 000 r/mi. 5.4 nitrogen blowing instrument. 5.5 Rotary evaporator. 5.6 Homogenizer. 5.7 solid phase extraction device. 5.8 Multifunctional food mixers. 5.9 Shredder. 5.10 Vortex Mixer.

6 Preparation and storage of samples

6.1 tea, grain category Approximately 500 g of the representative sample was ground and pulverized by a pulverizer and passed through a 2.0 mm round hole sieve, mixed and sealed in a clean container. mark. 6.2 vegetables, fruits and nuts Replace the sample of about 500 g, chopped, the multi-functional food mixer fully mashed evenly, into a clean container sealed, marked the standard Remember. 6.3 livestock, poultry, aquatic products Replace the sample of about 500 g, chopped, with a multi-functional food mixer fully mashed uniform, sealed into a clean container, marked mark. 6.4 Bee products category To replace the sample about 500 g, the crystallization of the sample will be forced to stir evenly, the crystallization of the sample can be sealed after the sample cap, Placed in a water bath of not more than 60 ° C warm, and so the sample all melted and then stir, quickly cooled to room temperature. In the melting must pay attention to prevent water Points volatile. Sealed in a clean container and marked with a mark. Tea, cereals, bee products, nuts and other samples stored below 4 ℃; vegetables, fruits, livestock, poultry, aquatic products such as samples at -18 ℃ Save the following. In the sample preparation process, should prevent the sample contamination or the occurrence of florfenilazole residue changes. Note. The above sample sampling site according to GB 2763 Appendix A implementation.

7 Analysis steps

7.1 Extraction Grain, nuts and tea. Weigh 5 g (2 g of tea) (accurate to 0.01 g) in a 50 mL centrifuge tube, add 5 mL of water Placed for 0.5 h. Vegetables, fruits, meat and honey. Weigh 5 g (accurate to 0.01 g) sample in 50 mL centrifuge tube, add water 5 mL mix. Add 20 mL of acetonitrile, 10 000 r/min homogeneous 0.5 min (honey only need to vortex mixing 2 min), add 5 g sodium chloride, shake, And centrifuged at 4 000 r/min for 3 min. Absorb the upper organic phase in the concentrated flask, the residue by adding 15 mL of acetonitrile, repeat the extraction time, And the upper organic phase was concentrated in a 45 ° C water bath under reduced pressure to near dryness. Accurately add 5.0 mL of acetonitrile-toluene (7 3, volume ratio) (fruit, vegetables) Or hexane-ether (8 2, volume ratio) (grain, nuts, tea, meat and honey) to dissolve the residue for purification by solid phase extraction column. 7.2 Purification 7.2.1 Fruits and vegetables Accelerate the extraction of 2.5 mL of the extract into a tandem column, eluting with acetonitrile-toluene (7 3) at a flow rate of 2 mL/min, collecting 10 mL of eluent 10 mL glass centrifuge tube, in 45 ℃ below the water bath with a nitrogen blowing machine, add 0.5 mL of acetonitrile dissolved and constant volume, gas chromatography-mass spectrometry set. 7.2.2 Grains, nuts, meats, tea and honey Accurately remove the 2.5 mL extract into the Florisil solid phase extraction column, with 15 mL n-hexane - ether (8 2, volume ratio) Flow rate of 2 mL/min, discard the eluent. Elution with n-hexane-diethyl ether (3 7, by volume), 10 mL of eluent was collected in 10 mL of glass Glass centrifuge tube, in 45 ℃ below the water bath with a nitrogen blowing machine, add 0.5 mL of acetonitrile dissolved and volume, gas chromatography - mass spectrometry. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. DB-5ms quartz capillary column, 30 m x 0.25 mm (id) x 0.25 μm, or equivalent. B) Column temperature. 70 ° C (1 min) 20 ° C/min 300 ° C (10 min). C) Inlet temperature. 280 ° C. D) Interface temperature. 280 ° C. E) Carrier gas. helium, purity greater than or equal to 99.999%. Flow rate. 1.0 mL/min. F) Injection volume. 2 μL. G) Injection mode. pulse splitless injection, pulse pressure 25 psi, delay 0.75 min, 0.75 min after the valve. H) solvent delay time. 8 min. I) ion source. electron bombardment source (EI). J) Ionization energy. 70 eV. K) Detection method. Select the ion monitoring mode. L) Select the ion and relative abundance. see Table 1 Table 1 Select the ion and relative abundance Select ion (m/z) 233 (quant.) Relative abundance (%) 100 34.5 9.2 7.3.2 Quantitative determination According to the content of fluorosilazone in the sample solution, the standard working solution with the concentration of fenosilazole in the sample solution was selected. Standard working solution and sample The fluorosilazole response in the solution should be within the linear range of the instrument. Standard working solution and sample volume and other volume interspersed injection determination. In the above chromatogram The retention time of flusilazide is about 11.0 mim, and the total ion chromatogram of the standard is shown in Figure A.1 in Appendix A. 7.3.3 Qualitative determination The standard solution and sample solution are tested according to the conditions specified in 6.3.1, if the sample solution and the standard solution in the same retention time peak Now, it is confirmed by mass spectrometry, after deducting the background of the sample spectrum, the selected ions all appear, while the selected ion from the The abundance ratio is consistent with the relative abundance of the ions associated with the standard, and the fluctuation range is within the maximum allowable deviation of Table 2 (see Table 2) Fluorosilicon is present in the sample. The confirmed sample can be judged to be detected by fluorosilazole positive. The spectrum of the fluorosilazole standard is given in Appendix A. Figure A.2. Table 2 Mass Spectrometry Relative Ion Abundance Maximum Allowable Deviation 7.4 blank test In addition to the sample, according to the above test steps.

8 results calculated

Use the chromatographic data processing software or calculate the residual content of flusilazole in the sample according to formula (1). A × c × V X = (1) AS x m Where. X - the amount of fluorosilazazole residues in milligrams per kilogram mg/kg; The peak area of fluorosilazazole in A - sample solution; C - the concentration of fluorosilazazole in standard working fluid, expressed in micrograms per milliliter of g/mL; V - final volume of volume in milliliters of mL; AS - standard working area of fluorosilazazole peak area; M - the amount of sample represented by the final sample, in grams. 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 C 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 D requirements. 10% limit and recovery rate Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% 10.1 Quantitation limits The quantification limit of this method is. 0.01 mg/kg. 10.2 Recovery rate The experimental data on the concentration, recovery and precision of the sample are given in Appendix B.

Appendix A

(Informative) Chromatograms and spectra Figure A.1 Total ion chromatogram of the fluorosilicone target substance Figure A.2 Mass spectrum of fluorosilazole standard substance

Appendix B

(Informative) Sample concentration and recovery of the experimental data Table B.1 Experimental data on the concentration and recovery of the sample Sample added concentration (Mg/kg) Recovery rate range% precision range% Sample added concentration (Mg/kg) Recovery rate range% precision range Rice 0.01 65.7 to 81.1 7.88 Tea 0.01 63.1 to 85.1 11.0 0.02 72.5 to 86.0 5.74 0.02 69.0 to 76.0 6.73 0.05 79.0 to 100.8 10.7 0.05 73.6 to 84.2 5.03 Fresh pea 0.01 71.2 ~ 82.3 6.83 Beef 0.01 63.8 ~ 85.3 10.4 0.02 72.5 to 86.0 5.79 0.02 74.5 to 90.0 7.47 0.05 78.6 to 86.4 5.03 0.05 83.0 to 102.2 9.3 Komatsu 0.01 66.9 ~ 86.1 10.0 Chicken 0.01 66.6 ~ 87.3 10.1 0.02 69.0 to 85.5 8.18 0.02 73.5 to 88.5 7.02 0.05 75.6 to 88.2 5.49 0.05 79.2 to 101.0 10.7 Pear 0.01 66.3 ~ 84.0 8.72 Shrimp 0.01 65.3 ~ 88.6 11.9 0.02 72.5 to 86.0 6.78 0.02 75.5 to 93.0 9.03 0.05 73.4 ~ 87.2 5.89 0.05 79.6 ~ 102.4 9.67 Citrus 0.01 72.3 ~ 85.2 8.88 Honey 0.01 66.5 ~ 82.3 8.82 0.02 74.0 to 88.0 6.12 0.02 75.5 to 93.5 7.43 0.05 79.8 to 97.4 7.57 0.05 77.8 to 100.2 9.93 Peanut 0.01 67.8 ~ 80.1 7.79 Soybean 0.01 63.7 ~ 80.6 12.5 0.02 76.0 to 91.5 6.61 0.02 66.5 to 86.0 14.1 0.05 77.4 to 90.6 6.73 0.05 75.0 to 90.0 11.8

Appendix C

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

Appendix 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 ------------------------------------------------

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