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GB 23200.1-2016 English PDF

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GB 23200.1-2016: Food safety national standard -- Methods for the determination of herbicide residues -- Part 1: Determination of amide herbicides in grain and oilseeds by gas chromatography-mass spectrometry
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GB 23200.1: Evolution and historical versions

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GB 23200.1-2016English299 Add to Cart 3 days [Need to translate] Food safety national standard -- Methods for the determination of herbicide residues -- Part 1: Determination of amide herbicides in grain and oilseeds by gas chromatography-mass spectrometry Valid GB 23200.1-2016
GB/T 23200-2008EnglishRFQ ASK 3 days [Need to translate] Determination of 488 pesticides and related chemicals residues in mulberry twig, honeysuckle, barbary wolfberry fruit and lotus leaf -- GC-MS method Obsolete GB/T 23200-2008

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Basic data

Standard ID GB 23200.1-2016 (GB23200.1-2016)
Description (Translated English) Food safety national standard -- Methods for the determination of herbicide residues -- Part 1: Determination of amide herbicides in grain and oilseeds by gas chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 15,199
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 1737.1-2006
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 23200.1-2016: Food safety national standard -- Methods for the determination of herbicide residues -- Part 1: Determination of amide herbicides in grain and oilseeds 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 - Methods for the determination of herbicide residues - Part 1. Determination of amide herbicides in grain and oilseeds by gas chromatography-mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 1737.1-2006 National standards for food safety Method for determination of herbicide residue Part 1. Determination by gas chromatography - mass spectrometry Residues of amide herbicides in grain and oilseeds National food safety standards- Determination of acetanilide herbicide residues in cereals and oil seeds 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 1737.1-2006 "Method for the determination of herbicide residues Part 1. Determination of grain grains by gas chromatography-tandem mass spectrometry And residual residues of amide herbicides in oilseeds ". Compared with SN/T 1737.1-2006, 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 1737.1-2006. National standards for food safety Method for determination of herbicide residue Part 1. Determination of amide herbicides in grain and oilseeds by gas chromatography - mass spectrometry Agent residue

1 Scope

This standard specifies the sampling, sample preparation and method for the determination of amide herbicide residues in grain and oilseeds. This standard applies to rice, soybean amide herbicide residue quantitative determination of 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 herbicide in the sample was extracted with acetone and water. After removal of acetone from the extract, the sodium chloride solution was added, extracted with n-hexane, Concentrated n-hexane extract, and then extracted with acetonitrile, Florisil solid phase extraction column purification, sample gas supply gas chromatography - mass spectrometry, external standard Quantitative quantity.

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). chromatographic purity. 4.1.2 acetonitrile (CH3CN). pure chromatography. 4.1.3 Acetone (CH3COCH3). Chromatographic pure. 4.1.4 ether ((C2H5) 2O). chromatographic purity. 4.1.5 anhydrous sodium sulfate (Na2SO4). 650 ° C burning 4 h, after cooling placed in the dryer in reserve. 4.1.6 Sodium chloride (NaCl). Analytical purity. 4.2 solution preparation 4.2.1 Sodium chloride solution. 10% (m/v), 100 g of sodium chloride was dissolved in water and diluted to 1000 mL. 4.2.2 extract agent I. acetonitrile by adding a small amount of n-hexane saturation, shake. 4.2.3 extract agent Ⅱ. n-hexane by adding a small amount of acetonitrile saturation, shake. 4.2.4 N-Hexane - Ethyl Ether (85 15). Take 85 mL of n-hexane and 15 mL of ether and mix well. 4.3 standards 4.3.1 Chlorpyrifos, Atrazine, Acetochlor, Dimethalchenamine, Alachlor, Nitrazone, Propellaben, Propoxurine, Butachlor, Propane Amine, prednisamine standard (see Appendix A for specific information), purity greater than 98%. 4.4 standard solution preparation 4.4.1 accurately weighed 25 ± 0.1 mg standard in 50 mL volumetric flask, dissolved with acetone and volume, get the concentration of 500 g/mL Single standard stock solution, the solution in 0 ~ 4 ℃ can be stored for 3 months. According to the need to use acetone diluted stock solution, prepared into the appropriate concentration of mixed Standard solution, the solution in 0 ~ 4 ℃ can be stored for 1 month. 4.5 Materials 4.5.1 Florisil Solid Phase Extraction Column. 125 mg, 3 mL, or equivalent. Before use, use 5 mL n-hexane-ether solution and 5 mL N-hexane pre-leaching column at a flow rate of 1 d/sec.

5 instruments and equipment

5.1 Gas Chromatography - Mass Spectrometer. 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Rotary Evaporator. 5.4 solid phase extraction device. 5.5 blowing nitrogen enrichment instrument. 5.6 vortex mixer. 5.7 homogenizer. 5.8 Centrifuge. 5.9 Eggplant bottle. 100 mL, 250 mL. 5.10 Centrifuge tube. 15 mL, 50 mL. 5.11 Microinjector. 10 μL.

6 Preparation and storage of samples

6.1 Preparation of the sample The samples were scaled to 1 kg by quarter, and the sample was taken according to GB 2763 Appendix A, and all were ground and passed through a 40 mesh sieve. Uniform, are divided into two, into a clean container, sealed, marked mark. 6.2 Sample storage Keep the sample below 5 ° C in dark. During sample and sample preparation, it is necessary to prevent contamination of the sample or change in the content of the residue The

7 Analysis steps

7.1 Extraction Weigh about 10 g (accurate to 0.01 g) sample in 50 mL centrifuge tube, add 10 mL of water and 20 mL of acetone, homogenized 3 min, Centrifuged at 4000 r/min for 4 min, the extract was transferred to 250 mL eggplant flask, the residue in the centrifuge tube was extracted with 30 mL  2 acetone, The extract is incorporated into an eggplant bottle. The acetone was removed by evaporation under reduced pressure at 38 ° C and the residue (about 10 mL) was transferred to another 50 mL centrifuge tube. The eggplant was washed with 10 mL of 10% sodium chloride solution and 15 mL of n-hexane, and the washing solution was transferred into a centrifuge tube and shaken for 3 min. 2500 r/min centrifugation 3 min, collecting n-hexane phase. Centrifuge tube in the water phase and then 15 mL  2 n-hexane extraction, combined with n-hexane phase. 7.2 liquid - liquid distribution purification The n-hexane phase was dehydrated by the addition of an appropriate amount of anhydrous sodium sulfate and the n-hexane phase was completely transferred to another 250 mL eggplant vial at 50 ° C Evaporated to dryness. The residue was dissolved in 5 mL of  2 extract II and transferred to a 50 mL centrifuge tube. Add 10 mL  3 extract I, mix, stratified, acetonitrile phase transferred to another 50 mL centrifuge tube. Add 10 mL of the extract Ⅱ, mix, stratified and discarded n-hexane Phase, the acetonitrile phase was transferred to a 100 mL eggplant flask and evaporated to dryness at 50 ° C. The residue was dissolved in 5 mL of n-hexane. 7.3 Solid phase extraction purification The above n-hexane solution was transferred to a Florisil solid phase extraction column with a liquid column flow rate of 0.5 d/sec, eluting with 15 mL of n-hexane - ether solution was rinsed with eggplant vials and transferred to a column for elution at a flow rate of 1 d/sec. The complete eluate was collected in a quantitative tube at 40 oC, In the nitrogen stream to the near dry, adding n-hexane dissolved residue and fixed to 1.0 mL for GC-MS determination. 7.4 determination 7.4.1 Gas Chromatographic Reference Conditions A) Column. HP-1701 MS, 30 m  0.25 mm (inner diameter)  0.25 m (film thickness), or equivalent; B) Carrier gas. helium (purity greater than 99.999%), flow rate. 1.0 mL/min. C) column temperature conditions. the initial temperature. 70 ℃ (keep 1 min); 15 ℃/min, heating to 160 ℃ (to maintain 1 min); 2 ℃/min, the temperature is raised to.200 ℃ (keep 2 min); 20 ℃/min, the temperature to 280 ℃ (to keep 8 min). D) Inlet temperature. 270 ° C. E) Injection method. splitless injection, 1 min after the opening of the diversion valve, split ratio of 100. 1. F) Injection volume. 1 μL; 7.4.2 Mass spectrometry reference conditions A) Ion source temperature. 230 ° C B) Transmission line temperature. 280 ° C C) Ionization mode. EI D) Scanning range. 50 - 400 amu E) Electron multiplier tube voltage. Auto tuning voltage.200 V; F) Test method. Select ion monitoring. 7.4.3 Determination and confirmation of chromatography 7.4.3.1 Quantitative determination According to the herbicide content in the sample solution, the standard working solution with similar peak area is selected, the standard working solution and the herbicide The values shall be within the linear range of the instrument detection. Quantitative method of single or multi-point external standard method, the standard working fluid and sample solution should be inserted into the sample set. 7.4.3.2 Qualitative determination Qualitative determination of the two basis. (1) the measured sample peak and the standard sample peak chromatographic retention time the same; (2) measured samples and standards The relative abundance of the monitored ions of the test sample shall be consistent with the standard sample, and the difference between the two is not greater than ± 10% (EI mode). See Annex A for monitoring ions and quantitation ions for each herbicide. Under the above chromatographic and mass spectrometric conditions, the effects of toxaphene, atrazine, acetochlor, dimethylphenols, alachlor, dicarbazone, metolachlor, The retention times of propanil, butachlor, propachlor and darior were 11.2 min, 13.2 min, 13.8 min, 14.9 min, 15.3 min, 15.7 min, 15.9 min, 16.9 min, 19.3 min, 20.6 min, 21.9 min. Select the ion chromatogram see Appendix B, Mass Spectrometry See Appendix C for C1 to C4. 7.5 blank experiment In addition to the sample, according to the above determination steps.

8 results are calculated and expressed

Use the chromatographic workstation or calculate the content of the herbicide in the sample by the following formula (1). The result of the calculation shall be deducted from the blank value. A  c  V X = (1) AS  m Where. X - Herbicide content in sample, mg/kg; A - the area of herbicide in the sample; AS - standard solution in the herbicide peak area; C - standard solution concentration, mg/L; V - the final volume of the sample solution, mL; M - sample weighing, 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) 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 toxaphene, atrazine, acetochlor, metolachlor, propachlor, droper, 0.02 mg/kg; alachlor, butachlor limit of quantification of 0.05 mg/kg. 10.2 Recovery rate 10.2.1 Experimental data on concentration and recovery of herbicides in rice. The recoveries were in the range of 0.02 mg/kg - 2.0 mg/kg, and the recoveries were 90.3% - 94.5%. The recoveries were 89.8% - 95.5% in the range of 0.02 mg/kg - 2.0 mg/kg. The recoveries were 84.5% - 93.5% in the range of 0.02 mg/kg - 2.0 mg/kg. The recoveries were 84.5% - 93.8% in the range of 0.02 mg/kg - 2.0 mg/kg. The recoveries were 83.7% - 93.9% in the range of 0.05 mg/kg - 2.0 mg/kg. The recoveries were 88.3% - 95.6% in the range of 0.02 mg/kg - 2.0 mg/kg. The recoveries were 88.1% - 93.8% in the range of 0.02 mg/kg - 2.0 mg/kg. The recovery rate was 83.7% - 95.8% in the range of 0.02 mg/kg - 2.0 mg/kg. The recoveries were 76.8% - 89.5% in the range of 0.05 mg/kg - 2.0 mg/kg. The recoveries were 86.9% - 97.5% in the range of 0.02 mg/kg - 2.0 mg/kg. The recoveries were in the range of 0.02 mg/kg - 2.0 mg/kg, and the recoveries were 94.2% - 101.9%. 10.2.2 Experimental data on the concentration and recovery of herbicides in soybean. The recoveries were in the range of 0.02 mg/kg - 2.0 mg/kg, and the recoveries were 78.1% - 92.0%. The recoveries were 80.8% - 92.8% in the range of 0.02 mg/kg - 2.0 mg/kg. The recoveries were 80.8% - 88.6% in the range of 0.02 mg/kg - 2.0 mg/kg. The recoveries were 78.7% - 90.9% in the range of 0.02 mg/kg - 2.0 mg/kg. The concentration of alachlor was between 0.05 mg/kg and 2.0 mg/kg, and the recovery was 76.1% - 86.4%. The recoveries were 81.7% -91.5% in the range of 0.02 mg/kg - 2.0 mg/kg. The recoveries were 81.6% -90.3% in the range of 0.02 mg/kg - 2.0 mg/kg. The recovery rate was 82.9% - 92.5% in the range of 0.02 mg/kg - 2.0 mg/kg. The concentration of butachlor was in the range of 0.05 mg/kg - 2.0 mg/kg, and the recovery was 72.8% - 83.6%. The recoveries were in the range of 0.02 mg/kg - 2.0 mg/kg, and the recoveries were 86.4% - 92.7%. The recoveries were in the range of 0.02 mg/kg - 2.0 mg/kg, and the recoveries were 88.4% - 96.0%.

Appendix A

(Informative) Table A.1 Quantitative ions and monitoring ions for herbicides * For the quantitative ions, for different mass spectrometry equipment, instrument parameters may be different, should be measured before the mass spectrometry parameters to optimize the best. Chinese name English name CAS number Molecular formula Molecular monitoring ion, m/z and its relative abundance Chlorpyrifos Propachlor 1918-16-7 C11H14ClNO 211.69 * 120 (100), 176 (37), 196 (10), 211 (8) Atrazine Atrazine 1912-24-9 C8H14ClN5 215.68 *.200 (100), 215 (62), 172 (15), 173 (35) Acetochlor 34256-82-1 C14H20ClNO2 269.80 * 146 (100), 223 (53), 174 (48), 162 (83) Dimethyl grass Dimethenamid 87674-68-8 C12H18ClNO2S 275.79 154 (100), 203 (42), 230 (58), 232 (20) Alachlor 15972-60-8 C14H20ClNO2 269.77 * 160 (100), 188 (93), 237 (24), 269 (6) Oxalcone metribuzin 21087-64-9 C8H14N4OS 214.28 * 198 (100),.199 (19), 144 (14), 214 (4) Isopropyl grass Metolachlor, Acetamide 51218-45-2 C15H22ClNO2 283.79 * 162 (100), 238 (47), 240 (15), 211 (7) Propanil 709-98-8 C9H9Cl2NO 218.08 * 161 (100), 163 (71), 217 (18), 219 (12) Butachlor 23184-66-9 C17H26ClNO2 311.85 * 176 (100), 160 (86), 188 (49), 237 (27) Pretilachlor 51218-49-6 C17H26ClNO2 311.85 162 (100), 202 (38), * 238 (69), 262 (27) Enantiose Napropamide 15299-99-7 C17H21NO2 271.36 72 (100), 100 (39), * 128 (63), 271 (26)

Appendix B

(Informative) Standard chromatogram Figure B.1 SIS chromatograms of standard mixtures of amide herbicides (concentrations of 0.1 mg/L) 1. Acetachlor. 11.2 min; 2. Atrazine. 13.2 min; 3. Acetochlor. 13.8 min; 4. Dimethalfen. 14.9 min; 5. Alachlor. 15.3 min; 6. Oxathione. 15.7 min; 7. metolachlor. 15.9 min; 8. propanil. 16.9 min; 9. butachlor. 19.3 min; 10. Propachlor. 20.6 min; 11. Dendrocaline. 21.9 min.

Appendix C

(Informative) Standard quality spectrum Figure C.1 SIM spectra of chloroxamine, atrazine and dimethylphenols Figure C.2 SIM spectra of oxalcone, propanil, acetochlor Figure C.3 SIM spectra of butachlor, alachlor, and metolachlor Figure C.4 SIM spectra of glyphosate and prednisone Diquat Napropamide

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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