GB 23200.57-2016 English PDF

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GB 23200.57-2016: Food safety national standard -- Determination of Acetochlor Residues in Foods
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Basic data

Standard ID: GB 23200.57-2016 (GB23200.57-2016)
Description (Translated English): Food safety national standard -- Determination of Acetochlor Residues in Foods
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Word Count Estimation: 12,114
Date of Issue: 2016-12-18
Date of Implementation: 2017-06-18
Older Standard (superseded by this standard): SN/T 2322-2009
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 23200.57-2016: Food safety national standard -- Determination of Acetochlor 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 Acetochlor Residues in Foods 1.1.1.1.1.2 GB National Standards of People's Republic of China Instead of SN/T 2322-2009 National standards for food safety Determination of Acetochlor Residues in Foods National food safety standards- Determination of acetochlor residue in foods 200 × - × - × release 200 × - × - × 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 2016-12-18 Release.2017-06-18 Implementation

Foreword

This standard replaces SN/T 2322-2009 "Method for the detection of acetochlor residues in food for import and export". Compared with SN/T 2322-2009, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name 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 2322-2009. National standards for food safety Determination of Acetochlor Residues in Foods

1 Scope

This standard specifies the determination of acetochlor residues in food by gas chromatography, gas chromatography - mass spectrometry and sample preparation methods. This standard applies to the determination of acetochlor residues in peanuts, soybeans, corn, wheat, onions, seaweed, chicken, pork, cashew nuts and pine Set, 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

The acetochlor residue in the sample was extracted with acetonitrile or ethyl acetate and purified by gel permeation chromatography (GPC) and/or silica gel SPE (SPE) Purification was carried out by gas chromatography (GC) and gas chromatography - mass spectrometry (GC - MS).

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 n-hexane (C6H14). 4.1.2 Ethyl acetate (C4H8O2). 4.1.3 Cyclohexane (C6H12). 4.1.4 Acetonitrile (C2H3N). 4.1.5 Acetone (C3H6O). 4.1.6 anhydrous sodium sulfate (Na2SO4). analytical pure; 650 ℃ burning 4 h, stored in a sealed container for use. 4.2 solution preparation 4.2.1 Ethyl acetate-n-hexane (3 97, V/V). Take 30 mL of ethyl acetate, add 970 mL of n-hexane and shake well. 4.2.2 Ethyl acetate - n-hexane (5 95, V/V). Take 50 mL of ethyl acetate, add 950 mL of n-hexane and shake well. 4.2.3 Ethyl acetate - cyclohexane (50 50, V/V). Take 500 mL of ethyl acetate, add 500 mL of n-hexane and shake well. 4.3 standards 4.3.1 Acetochlor standards (acetochlor, C14H20ClNO2, CAS No..34256-82-1). purity ≥ 98%. 4.4 standard solution preparation 4.4.1 Acetochlor standard solution. accurately weighed the amount of acetochlor standards, with acetone dubbed the concentration of 100 μg/mL standard stock solution. The standard stock solution is diluted with n-hexane to the standard working solution at the appropriate concentration. Standard stock solution and standard working fluid are protected from 0 ° C to 0 ° C 4 ℃ under the conditions of storage. Valid for 6 months.

5 instruments and equipment

5.1 Gas Chromatograph. Microspot Electronic Capture Detector (μ-ECD). 5.2 Gas Chromatography-Mass Spectrometer. Electronically challenged source (EI). 5.3 Gel Permeation Chromatography. 5.4 Rotary Evaporator. 5.5 Centrifuge. 5 000 r/min. 5.6 high speed homogenizer 5.7 silica gel solid phase extraction column. 6 mL/1 000 mg, or equivalent; before use with 10 mL n-hexane rinse. 5.8 Centrifuge tubes. 100 mL, plastic and glass. 5.9 Filtration. 0.45 μm, organic phase. 5.10 Analysis of balance. 0.01 g and 0.0001 g.

6 Preparation and storage of samples

6.1 vegetables, edible fungi 6.1.1 Take about 500 g of representative spicy vegetable samples onions and cut them into small pieces of about 4 cm2. Into a clean container, sealed And mark the mark. -18 ℃ below the preservation. 6.1.2 Take representative samples of vegetables (except spicy vegetables such as onions and other spicy vegetables) and pine velvet and other representative edible fungus samples about 500 g, The sample is processed into a slurry. Mix, fit into a clean container, sealed and marked. -18 ℃ below the preservation. 6.2 seaweed Take representative samples of seafood about 500 g, chopped, with a crusher to sample processed into a slurry. Mix well into a clean container Closed mark. -18 ℃ below the preservation. 6.3 Grains and nuts Take about 500 g of representative samples of peanuts, corn, wheat, soybeans, cashew nuts, etc., crushed and mixed with a pulverizer, packed in clean containers Inside, sealed and marked. 4 ℃ below the preservation 6.4 Animal source class Take about 500 g of representative samples of chicken, pork, etc., crushed with a meat grinder, mix well, into a clean container, sealed and marked. -18 ℃ below the preservation. Note. The above sample sampling site according to GB 2763 Appendix A implementation.

7 measurement steps

7.1 Extraction Grain, Nuts. Weigh 10 g (accurate to 0.1 g) in a 100 mL plastic centrifuge tube, add 50 mL of acetonitrile, Homogenize 2 min. Centrifuge at 4 000 r/min for 10 min. The supernatant was poured into a vial, concentrated to dryness, washed with 10 mL of ethyl acetate- Cyclohexane solution dissolves the residue, membrane, for gel permeation chromatography (GPC) purification. Poultry tissue. Weigh the sample 10 g (accurate to 0.1 g) in a 100 mL plastic centrifuge tube, add 5 g of anhydrous sodium sulfate, stir , Add 50 mL of acetonitrile and homogenize on a homogenizer for 2 min. Centrifuge at 4 000 r/min for 10 min, and supernatate the supernatant with anhydrous sodium sulphate After pouring into the concentrated flask, concentrated to dry, with 10 mL of ethyl acetate - cyclohexane solution to dissolve the residue, membrane, for gel permeation chromatography (GPC) Purification. Onion. Weigh the sample 5 g (accurate to 0.1 g) in a 100 mL glass centrifuge tube, digested at 700 wd digestion for 40 s. After returning to room temperature, add 50 mL of ethyl acetate and homogenize on a homogenizer for 2 min. Centrifuge at 4 000 r/min for 10 min, pour the supernatant Into the concentrated bottle, concentrated to dry, with 1 mL n-hexane dissolved residue, for solid phase extraction column purification. Seafood, Tricholoma matsuter. Weigh 5 g (accurate to 0.1 g) in a 100 mL glass centrifuge tube, add 50 mL of ethyl acetate, The slurry was homogenized for 2 min. Centrifuge at 4 000 r/min for 10 min. The supernatant was poured into a vial, concentrated to dryness, washed with 1 mL n-hexane The residue is purified by solid phase extraction column. 7.2 Purification 7.2.1 Gel permeation chromatography Purification conditions A) Column. S-X3 20 × 2 cm (inner diameter), or equivalent; B) Mobile phase. cyclohexane-ethyl acetate (1 1, V/V); C) Flow rate. 5.0 mL/min; D) Injection volume. 5.0 mL; E) elution volume. 40 mL; F) Collecting volume. 30 mL; G) Cleaning volume. 10 mL. 7.2.2 Gel permeation chromatography purification The filters of the extract of grain, nuts and poultry tissues in Section 7.1 were injected into a gel permeation chromatograph to collect 40 to 70 mL of the effluent, 40 ℃ water bath under reduced pressure to dry, with 1 mL n-hexane dissolved residue, for solid phase extraction column purification. 7.2.3 silica gel solid phase extraction column purification Mix the onion, seaweed, truffle extract and 7.2.2 purifying solution into the silica gel solid phase extraction column in section 7.1, then use 2 × 1 mL The flask was run in a silica gel column, washed with 10 mL of n-hexane, 5 mL of ethyl acetate-n-hexane solution and 5 mL of ethyl acetate - n-hexane solution eluted with 15 mL of ethyl acetate-n-hexane solution and the eluate was collected and concentrated to dryness under reduced pressure at 40 ° C. Hexane volume to 5 mL, for gas chromatography and gas chromatography-mass spectrometry. 7.3 Determination 7.3.1 Gas Chromatographic Reference Conditions A) Column. DB-5 quartz capillary column, 30 m x 0.32 mm (inner diameter), film thickness 0.25 μm, or equivalent; 15 ° C/min B) column temperature. 60 ℃ (1min) 260 ℃ (5min), 300 ℃ (after running 15min); C) Inlet temperature. 250 ° C; D) detector temperature. 325 ° C; E) Carrier gas. helium, purity ≥99.995%, 1.8 mL/min; F) Injection volume. 1 μL; G) Injection method. no split injection, 0.75 min after the opening valve; 7.3.2 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. DB-5MS quartz capillary column, 30 m × 0.25 mm (inner diameter), film thickness 0.25 μm, or equivalent; B) column temperature. 60 ℃ (1min) 260 ℃ (5min), 300 ℃ (after running 15min); C) Inlet temperature. 250 ° C; D) chromatographic - mass spectrometer interface temperature. 280 ° C; E) Carrier gas. helium, purity ≥99.995%, 1.0 mL/min; F) Injection volume. 1 μL; G) Injection method. no split injection, 0.75 min after the opening valve; H) ionization mode. EI; I) ionization energy. 70 eV; J) Measurement method. Select the ion monitoring mode (SIM); K) monitoring of ions (m/z). quantitation 162, qualitative 174,234,269; L) solvent delay. 3 min. 7.3.3 Determination of gas chromatography According to the sample solution of acetochlor content, selected concentrations similar to the standard working solution. Standard Working Solution and Acetochlor Response in Samples Should be within the linear range of the instrument. Standard working solution and sample solution volume measurement. Under the above chromatographic conditions, acetochlor The retention time is about 12.3 min. The chromatogram of the standard is shown in Appendix A, Figure A.1. 7.3.4 Gas Chromatography - Mass Spectrum Confirmation The standard solution and sample solution of acetochlor are determined according to the conditions specified in Section 7.3.2. If the same retention time as the sample solution is the same as that of the standard solution Appears, then it is confirmed by mass spectrometry. The sample retention time of the measured sample was consistent with that of the standard sample, and the background After the selected spectra, the selected ions appear; the ions m/z162, 174, 234, 269 (the abundance ratio of 100. 54. 24. 8) The relative abundance of the standard sample-related ions is consistent and the similarity is within the allowable deviation (see Table 1), then the acetochlor is present in the sample. The total ion chromatogram, selective ion spectrum and full scan mass spectrum of the acetochlor standard are shown in Appendix A, Figures A.2, A.3 and A.4. Table 1 GC-MS confirms the maximum allowable deviation of relative ion abundance 7.4 blank test In addition to the sample, according to the above steps.

8 results are calculated and expressed

Use the chromatographic data processor or calculate the content of acetochlor in the sample according to formula (1). The calculation result must be deducted from the blank value. A × c × V AS x m Where. X - the content of acetochlor in the sample, mg/kg, mg/kg; C - the concentration of acetochlor in standard working fluid, in micrograms/ml, μg/mL; A - the peak area of acetochlor in sample solution; AS - standard working area of acetochlor in the peak area; V - the final volume of the sample solution, in milliliters, mL; M - the amount of 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 precision

Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% 15 ° C/min X = (1) 9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the Record 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 the Record the requirements of D. 10% limit and recovery rate 10.1 Quantitation limits The limit of quantification of this method is 0.01 mg/kg. 10.2 Recovery rate The addition and recovery of the sample by gas chromatography are shown in Appendix B (Table B.1). Gas Chromatography-Mass Spectrometry Concentration and recovery data are given in Appendix B (Table B.2).

Appendix A

(Informative) Standard Chromatography and Mass Spectrometry Min 8 9 10 11 12 13 14 15 Hz Figure A.1 Acetochlor Standard Gas Chromatogram 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 Time - > Abundance TIC..2007120712.D. Figure A.2 Acetochlor Standard Total Ion Flow Chromatogram (TIC) Acetochlor Acetochlor 160 170 180 190.200 210 220 230 240 250 260 270 M/z - > Abundance Scan 4496 (12.581 m in)..2007120712.D Figure A.3 Acetochlor Standard Selective Ion (SIM) Mass Spectrometry 50 100 150.200 250 300 350 400 450 M/z - > Abundance Scan 980 (12.591 min)..2007120702.D 242 341 420305 401381360 446 Figure A.4 Acetochlor Standard Full Scanning (SCAN) Mass Spectrometry

Appendix B

(Informative) Sample concentration and recovery of the experimental data Table B.1 Determination of the concentration and recovery of samples by gas chromatography sample name Add concentration (Mg/kg) Recovery rate range (%) Precision RSD (%) sample name Add concentration (Mg/kg) Recovery rate range (%) Precision RSD (%) peanut 0.01 71.3  91.2 9.8 seaweed 0.01 86.795.9 8.3 0.02 77.2  91.5 6.0 0.02 81.8  96.7 4.4 0.05 78.1  96.4 9.1 0.05 79.1  93.2 6.9 Soybeans 0.01 76.2 88.7 5.1 chicken 0.01 82.094.6 7.4 0.02 74.5 86.9 3.1 0.02 80.3 88.8 4.1 0.05 76.0  94.2 8.6 0.05 80.1 97.2 6.3 corn 0.01 75.786.0 6.9 pork 0.01 76.086.7 5.3 0.02 73.9 86.8 4.9 0.02 77.1  85.5 3.5 0.05 76.8  92.3 6.9 0.05 78.9 98.8 6.5 wheat 0.01 75.9 88.2 6.7 Cashew nuts 0.01 74.3  87.7 5.5 0.02 78.3  91.6 3.4 0.02 75.4  89.2 4.9 0.05 76.7  89.1 7.4 0.05 75.4  92.7 7.8 onion 0.01 76.6  93.1 9.4 Matsutake 0.01 81.5  97.6 8.3 0.02 82.6  93.7 4.3 0.02 83.1 96.5 4.4 0.05 80.0  93.2 6.9 0.05 79.3  95.3 6.9 Table B.2 Gas Chromatography-Mass Spectrometry Detection of Sample Concentration and Recovery Data sample name Add concentration (Mg/kg) Recovery rate range (%) Precision RSD (%) sample name Add concentration (Mg/kg) Recovery rate range (%) Precision RSD (%) peanut 0.01 71.5  88.3 8.6 seaweed 0.01 79.0  93.7 6.8 0.02 77.5  94.0 5.9 0.02 76.1  93.5 5.8 0.05 70.1  90.2 8.3 0.05 81.9  97.8 7.1 Soybeans 0.01 74.9 85.2 6.9 chicken 0.01 80.0  97.7 6.7 0.02 82.5  90.3 4.7 0.02 84.1  95.5 5.2 0.05 76.2  96.2 6.7 0.05 79.9 98.8 7.5 corn 0.01 70.9  85.8 4.4 pork 0.01 77.4  89.2 4.6 0.02 75.988.8 4.0 0.02 74.986.2 4.6 0.05 78.1  96.4 6.0 0.05 80.4  94.2 7.5 wheat 0.01 71.386.2 4.4 Cashew nuts 0.01 76.4 90.2 7.3 0.02 84.392.6 4.1 0.02 77.4  87.2 6.4 0.05 74.7  90.2 6.8 0.05 77.4  97.9 6.7 onion 0.01 82.6  91.1 4.6 Matsutake 0.01 82.0  96.5 6.8 0.02 78.6  89.7 5.5 0.02 83.9  100.3 5.8 0.05 79.0  95.2 8.7 0.05 87.6  101.5 7.1

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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