GB 23200.2-2016 English PDF

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GB 23200.2-2016: Food safety national standard -- Methods for the determination of herbicide residues -- Part 2: Determination of diphenyl ether herbicides in grain and oilseeds by gas chromatography-mass spectrometry
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 23200.2-2016	219	Add to Cart	3 days	Food safety national standard -- Methods for the determination of herbicide residues -- Part 2: Determination of diphenyl ether herbicides in grain and oilseeds by gas chromatography-mass spectrometry	Valid

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Basic data

Standard ID: GB 23200.2-2016 (GB23200.2-2016)
Description (Translated English): Food safety national standard -- Methods for the determination of herbicide residues -- Part 2: Determination of diphenyl ether herbicides in grain and oilseeds by gas chromatography-mass spectrometry
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Word Count Estimation: 11,167
Date of Issue: 2016-12-18
Date of Implementation: 2017-06-18
Older Standard (superseded by this standard): SN/T 1737.2-2007
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 23200.2-2016: Food safety national standard -- Methods for the determination of herbicide residues -- Part 2: Determination of diphenyl ether herbicides in grain and oilseeds by gas chromatography-mass spectrometry

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Food safety national standard - Methods for the determination of herbicide residues - Part 2. Determination of diphenyl ether herbicides in grain and oilseeds by gas chromatography National Standards of People's Republic of China GB Instead of SN/T 1737.2-2007 National standards for food safety Method for determination of herbicide residue Part 2. Determination by gas chromatography - mass spectrometry Residues of diphenyl ether herbicides in grain and oilseeds National food safety standards- Determination of diphenyl ether 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 1737.2-2007 "Methods for the determination of herbicide residues Part 2. Determination of grain and oil by gas chromatography/mass spectrometry The amount of diphenyl ether herbicide residues in seeds ". Compared with SN/T 1737.2-2007, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 1737.2-2007. National standards for food safety Method for determination of herbicide residue Part 2. Determination of diphenyl ethers in grain and oilseeds by gas chromatography - mass spectrometry Herbs Residue

1 Scope

This standard specifies the grain and oil seed in the ginger grass, methicillin ether, benzoyl ether, methylprednisolide, triflufen grass, Lecium grass Determination of 9 Diphenyl Ether Herbicide Residues by Gas Chromatography/Mass Spectrometry. This standard applies to rice and soybeans in the nine kinds of diphenyl ether herbicide residues in the detection and 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 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 samples were extracted with acetonitrile, cleaned up by Florian silica solid phase extraction column, gas chromatograph - mass spectrometer and external standard method.

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 Acetone (CH3COCH3). Chromatographic pure. 4.1.2 acetonitrile (CH3CN). excellent grade pure. 4.1.3 n-hexane (C6H14). chromatographic purity. 4.1.4 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, placed in the dryer in reserve. 4.2 standards 4.2.1 Diphenyl Ether Herbicide Standards. See Appendix A. 4.3 standard solution preparation 4.3.1 standard reserve solution. accurately weighed the right amount of benzoin ether, methylprednisolone ether, trifluoro-nitrofen, Lactobenzene, Herbicide, B Oxyfloxacin, Fluorofenoxylate, respectively, dissolved in acetone and fixed capacity to brown volumetric flask, the concentration is equivalent to 1 000 mg/L, stock solution storage Below -18 ° C. 4.3.2 mixed standard intermediate solution. accurate absorption of appropriate amount of benzoin, methylprednisolone, triflufen grass, lactoferrin, herbicidal ether, Ethoxifluorfen, Efloxacillin standard stock solution in brown volumetric flask, fixed with acetone to the scale, a variety of diphenyl ether herbicides concentrated The degree of 10 mg/L, the intermediate solution stored below -18 ℃. 4.3.3 Mixed standard working solution. Mix the standard intermediate solution with acetone as needed and dilute it with other diphenyl ether herbicides And other concentrations of cyclodextrin and methoxylated ether, with nine kinds of diphenyl ether herbicides mixed standard working solution, mixed standard work The solution is stored at 0 to 4 ° C. 4.4 Materials 4.4.1 Florisil Solid Phase Extraction Column. 500 mg, 3 mL.

5 instruments and equipment

5.1 Gas Chromatography - Mass Spectrometer, with electron bombardment source. 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Centrifuge. 5.4 blowing nitrogen enrichment instrument. 5.5 Solid phase extraction device. 5.6 Scroll Mixer.

6 Preparation and storage of samples

Respectively, representative of the rice and soy samples of about 500 g, the sample sampling site according to GB 2763 Appendix A implementation, full crushing, mixing, Into a clean container, sealed and marked with, stored at 4 ℃ cold storage.

7 Analysis steps

7.1 Extraction Weigh 5 g (accurate to 0.01 g) sample in 50 mL centrifuge tube, add 2 mL of water and 20 mL of acetonitrile, then add 2 g of anhydrous sodium sulfate, Mixed in a vortex mixer for 3 min, centrifuged at 5000 r/min for 5 min, transferred to 10 mL of acetonitrile in the upper layer to another 15 mL centrifuge tube. 40 ° C water bath blowing nitrogen to dry, with n-hexane volume to 1 mL. 7.2 Purification A 1 cm high anhydrous sodium sulphate was filled above the Fryborough Silica Solid Phase Extraction Column packing, pre-leached with 6 mL of acetone and 6 mL of n-hexane, respectively. The extract was transferred to a solid phase extraction column, the column was discarded at a rate of 1 d/s, the effluent was discarded, and 5 mL of n-hexane-acetone (60 40, V/V) Followed by elution at a flow rate of 1 d/s. The eluate was collected in a 15 mL centrifuge tube and concentrated in a 40 ° C water bath to dryness, dissolved with n-hexane and Constant volume to 1.0 mL, gas chromatographic - mass spectrometry. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. HP-5MSI quartz capillary column. 30 m × 0.25 mm (inner diameter), film thickness 0.25 μm, or equivalent. B) Column temperature. 70 ° C (2 min) 50 ° C/min 180 ° C 10 ° C/min.200 ° C 2 ° C/min 220 ° C 10 ° C/min 280 ° C (10 min). C) Inlet temperature. 270 ° C. D) Carrier gas. helium, purity greater than 99.999%, flow rate 1.0 mL/min. E) Injection volume. 1 μL. F) Injection method. no split injection, 1.5 min after the valve. G) ion source temperature. 230 ° C. H) Transmission line temperature. 280 ° C. I) ionization mode. EI. J) Ionization energy. 70 eV. K) Monitoring mode. Select ion monitoring (SIM) and monitor ions See Appendix A. L) solvent delay. 5 min. 7.3.2 Determination and confirmation of chromatography According to the sample solution of diphenyl ether herbicide residue content, selected peak height similar to the standard working solution. Standard working solution and sample solution The residual response value of the diphenyl ether herbicide residue should be within the linear range of the instrument. The standard working solution and sample solution volume mixed injection Determination. If the sample solution is in the selective ion chromatogram of the standard working solution, a chromatographic peak appears at the same retention time, and the ion The abundance ratio is consistent with the relative abundance of the ions associated with the standard sample, and the similarity is within the tolerance (see Table 1), according to the selective ion Quantitative method. Under the above conditions of gas chromatography/mass spectrometry, cyproterone, trifluoroacetate, ethoxifen, herbicides, The retention times of oxygen herbicides, methylprednisolides, lactofenfen, and fenflufen are shown in Appendix A. 0.02mg/L mixed standard solution total separation Subflow Chromatogram See Appendix B, Figure B.1. Table 1 Maximum allowable error for relative ion abundance using gas chromatography-mass spectrometry 7.4 blank experiment In addition to the sample, according to the above determination steps.

8 results are calculated and expressed

The content of the diphenyl ether herbicide in the sample was calculated according to the following formula (1) Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% MΑs VCsA   .. (1) Where. X-sample Diphenyl ether herbicide content in milligrams per kilogram, mg/kg; The peak area of diphenyl ether herbicide in A sample solution; As - standard working solution of diphenyl ether herbicide peak area; Cs - Concentration of diphenyl ether herbicides in standard working solutions in milligrams per liter, mg/L; M - the final sample quality of the sample, in grams, g; V - the final volume of the 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 quantification limit of this method was 0.025 mg/kg. 10.2 Recovery rate When the levels were 0.025 mg/kg, 0.050 mg/kg, 0.100 mg/kg, the recoveries of diphenyl ether herbicides in rice and soybeans See Appendix C.

Appendix A

(Informative) Diphenyl ether herbicide basic information, retention time and monitoring of ion abundance ratio Table A.1 Basic information on the diphenyl ether herbicide, retention time and monitoring of the ion abundance ratio Serial number Pesticide Chinese name Pesticide English name CAS number Molecular formula Molecular retention time Min Monitor the ion abundance ratio 1 Cyclohexyl ether cinmethylin 87818-31-3 C18H26O2 270.40 10.041 105 * (100), 123 (44), 154 (15), 169 (16) 2 Trifluorobenzoate Fluorodifen 15457-05-3 C13H7F3N2O5 328.20 14.229 190 * (100), 126 (31), 162 (18), 309 (9), 328 (9) 3 oxyfluorfen oxyfluorfen 42874-03-3 C15H11ClF3NO4 361.70 15.177 252 * (100), 280 (16), 300 (31), 361 (38) 4 herbicides nitrofen 1836-75-5 C12H7Cl2NO3 284.09 15.680 283 * (100), 139 (27), 202 (49), 253 (18), 285 (77) 5 benzoate aclonifen 74070-46-5 C12H9ClN2O3 264.66 16.694 264 * (100), 77 (49), 183 (38), 194 (32), 212 (38) 6 Methoxy herbicides chlomethoxyfen 32861-85-1 C13H9Cl2NO4 314.12 19.584 313 * (100), 232 (36), 266 (79), 283 (33) 7 A Carboxylated Herbicide Bifenox 42576-02-3 C14H9Cl2NO5 342.13 20.404 341 * (100), 173 (18), 189 (17), 310 (26), 343 (71) 8 lactofen grass lactofen 77501-63-4 C19H15ClF3NO7 461.77 21.616 344 * (100), 207 (24), 223 (26), 346 (40)

9 Fluorofenoxylate

Fluoroglycofen-et Hyl 77501-90-7 C18H13ClF3NO7 447.75 21.880 344 * (100), 207 (63), 223 (59), 315 (31) Note. "*" mark ions as quantitative ions

Appendix B

(Informative) Total ion chromatograms of nine kinds of diphenyl ether herbicides Figure B.1 Diphenyl ether herbicide standard solution Total ion chromatogram 2. trifluoro-nitro-grass; 3. ethoxifen herb; 4. herbicidal ether; 5. 6. methoxylated herbicides; 7. methylprednisolide ether; 8. lactofen grass spirit; 9.

Appendix C

(Informative) Addition recovery of diphenyl ether herbicides in rice and Table C.1 Recovery of Diphenyl Ether Herbicides in Rice and Soybeans No. Compound Name Sample Substrate Rice and soybeans 1 Cyclohexanone 72.0% ~ 100.0% 72.0% ~ 104.0% 2 Trifluorobenzoate 74.0% ~ 110.0% 70.0% ~ 108.0% 3 ethoxifluorfen 70.0% ~ 98.0% 70.0% ~ 106.0% 4 Herbicide 72.0% ~ 107.0% 70.0% ~ 106.0% 5 benzoate 72.0% ~ 105.0% 71.0% ~ 102.0% 6 Oxygen Herbicide 70.0% ~ 107.0% 72.0% ~ 96.0% 7 A Carboxylated Herbicide 72.0% ~ 107.0% 72.0% ~ 108.0% 8 Lactobenzene Cream 70.0% ~ 106.0% 71.0% ~ 104.0% 9 Fluorofenoxides 72.0% ~ 104.0% 70.0% ~ 104.0%

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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