GB 23200.28-2016 English PDF

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GB 23200.28-2016: Food safety national standard -- Determination of residues of various herbicides in foodstuffs -- Gas chromatographic-mass spectrometry
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GB 23200.28-2016	279	Add to Cart	3 days	Food safety national standard -- Determination of residues of various herbicides in foodstuffs -- Gas chromatographic-mass spectrometry	Valid

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Basic data

Standard ID: GB 23200.28-2016 (GB23200.28-2016)
Description (Translated English): Food safety national standard -- Determination of residues of various herbicides in foodstuffs -- Gas chromatographic-mass spectrometry
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Word Count Estimation: 14,124
Date of Issue: 2016-12-18
Date of Implementation: 2017-06-18
Older Standard (superseded by this standard): SN/T 3541-2013
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 23200.28-2016: Food safety national standard -- Determination of residues of various herbicides in foodstuffs -- Gas chromatographic-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 residues of various herbicides in foodstuffs - Gas chromatographic - mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 3541-2013 National standards for food safety Determination of Residues of Various Ether Herbicides in Food Gas chromatography - mass spectrometry National food safety standards- Determination of multiple ether herbicides residues 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 3541-2013 "Method for the determination of residues of various herbicides in foodstuffs for import and export. Gas Chromatography - Negative Chemistry Ion source - mass spectrometry ". Compared with SN/T 3541-2013, 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 3541-2013. National standards for food safety Determination of Residues of Various Ether Herbicides in Food Gas chromatography - mass spectrometry

1 Scope

This standard specifies the method for the determination of phenylether herbicides in food by gas chromatography-negative chemical ion source-mass spectrometry. This standard applies to rice, soybeans, spinach, green onions, peppers, strawberries, sweet peas, green tea, lobster, eel, pork, honey, And other 12 kinds of food ether herbicide residue determination 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/T 6682 Analytical laboratory water specifications and test methods GB 2763 National Standard for Food Safety - Maximum Residue Limit of Pesticides in Foodstuffs

3 principle

The samples were extracted with n-hexane saturated acetonitrile (containing 1% glacial acetic acid), dispersed by solid phase extraction, gas chromatography - negative chemical ion source Spectral method for determination and confirmation, external standard method 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 n-hexane (C6H14). pure chromatography. 4.1.3 Acetone (C3H6O). Chromatographic pure. 4.1.4 glacial acetic acid (C2H4O2). 4.1.5 anhydrous magnesium sulfate (MgSO4). 4.1.6 anhydrous sodium acetate (C2H3ONa). 4.2 solution preparation 4.2.1 Extraction solvent (1% acetic acid in n-hexane saturated acetonitrile solution). add 10 mL of glacial acetic acid to 990 mL of acetonitrile (prior Saturated with n-hexane). 4.3 standards 4.3.1 Reference material. Fluorodafen (CAS. 15457-05-3), Oxyfluorfen, CAS. 42874-03-3), herbicidal ether (Nitrofen, CAS. 1836-75-5), benzoyl ether (Aclonifen, CAS. 74070-46-5), piccon Lt;/RTI & (Ethoxyfen-ethyl, CAS. 131086-42-5), methicillin ether (Chlomethoxyfen, CAS. 32861-85-1), Ether (Bifenox, CAS. 42576-02-3), Lactofen (CAS. 77501-63-4) and Fenflufen (Fluoroglycofen-ethyl, CAS. 77501-90-7). purity ≥98.0%. 4.4 standard solution preparation 4.4.1 Pesticide standard stock solution. accurately weighed the appropriate amount of the standard, diluted with acetone prepared into 1.00 mg/mL single The standard stock solution is stored at 4 ° C (valid for 6 months). 4.4.2 mixed standard stock solution. respectively, the exact removal of the appropriate amount of the above standard stock solution, diluted with acetone prepared into 50 μg/mL mixture The standard stock solution is stored at 4 ° C (valid for 6 months). 4.4.3 mixed standard working solution. according to the need to use acetone diluted to the appropriate concentration of the standard working solution, stored at 4 ℃ (valid for 3 Month). 4.5 Materials 4.5.1 Graphitized carbon black filler. 40 μm. 4.5.2 PSA (N-2 aminoethyl) filler. 40 μm. 4.5.3 C18 Filler. 40 μm. 4.5.4 Microporous membrane. 0.45 μm, organic phase.

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. Configure a negative chemical ion source (NCI source). 5.2 Analysis of balance. 0.1 mg and 0.01 g. 5.3 Rotary Evaporator. 5.4 Tissue crusher 5.5 Crusher. 5.6 Homogenizer. 5.7 Oscillator.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 Spinach, green onions, peppers, strawberries and sweet peas 10 g of the sample was taken, and after shredding (without washing with water), the sample was processed into a slurry by a mashing machine. Mix, are divided into two As a sample, into the container, sealed and marked. 6.1.2 Green tea, rice and soybeans 500 g of the representative sample was taken, pulverized by a pulverizer and passed through a 2.0 mm round hole sieve. Mix well, into the container, sealed and marked. 6.1.3 lobster, eel and pork After picking 500 g of the sample, it was chopped, and the sample was successively crushed and mixed with a crusher, packed into a container, sealed and marked mark. 6.1.4 honey Take a representative sample volume of 500g, the crystallization of honey samples will be evenly stirred; on the crystallization of honey samples, in a closed situation Condition, the sample bottle placed in not more than 60 ℃ in the water bath in the warm, shaking, until the sample all melt and stir well, quickly cooled to room temperature, in the melt Must pay attention to prevent the evaporation of water. The prepared samples were divided into two separate sections, sealed into the vials, sealed and marked. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Rice, soybeans, green tea, honey and other samples stored at 0 ~ 4 ℃; spinach, green onions, peppers, strawberries, sweet peas, lobster, eel Fish and pork and other samples in -18 ℃ below the frozen storage. During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue.

7 Analysis steps

7.1 7.1.1 Soybean, lobster, eel and pork and other samples Weigh 5 g sample (accurate to 0.01 g). 7.1.2 Spinach, green onions, peppers, strawberries and sweet peas and other samples Weigh 10 g sample (accurate to 0.01 g). 7.1.3 rice, green tea and honey and other samples Weigh 5 g of sample (accurate to 0.01 g) and add 4 mL of water, mix, soak or dissolve. Tea to be soaked for 30 min. 7.2 Extraction Place the weighed sample in a 250 mL stoppered conical flask, add 20 mL of the extraction solvent, add 15 g of anhydrous magnesium sulfate and 6 g of anhydrous vinegar Acid, the extraction of 40 min (beef, eel, lobster, chicken and other meat products should be homemade extraction 5 min), filtered in 150 mL concentrated bottle in. And then add 20 mL of extraction solvent to extract once again, the combined extract, 40 ° C spin concentrated to dry. The residue was dissolved in 2 mL of acetonitrile, To be purified. 7.3 Solid phase dispersion extraction purification 7.3.1 Spinach, green onions, peppers, strawberries, sweet peas and green tea extract The corresponding sample extract of 7.2 was transferred to a small tube containing 50 mg of PSA filler and.200 mg of graphitized carbon black filler in advance. Sub-vortex 1 min, until the pigment is completely eliminated, the filter membrane, gas chromatography-mass spectrometry and confirmation. 7.3.2 Rice, soybeans, lobster, eel, pork and honey extract The corresponding sample extract of 7.2 was transferred to a solution containing 100 mg of PSA filler, 50 mg of graphitized carbon black filler and 100 mg of C18 filler in advance Tube, full vortex 1 min, filter membrane, gas chromatography - mass spectrometry determination and confirmation. 7.4 determination 7.4.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. DB-17ms quartz elastic capillary column, 30 m × 0.25 mm (id), film thickness 0.25 μm, or equivalent; B) Column temperature. 90 ℃ 15 ℃/min 270 ℃ 2 ℃/min 276 ℃ 48 ℃/min 300 ℃ (2.5 min); C) Inlet temperature. 300 ° C; D) chromatographic-mass spectrometer interface temperature. 250 ° C; E) Carrier gas. helium, purity greater than or equal to 99.999%; flow rate, 1.0 mL/min; F) Injection volume. 1 μL; G) Injection method. splitless injection, 1.5 min after the opening valve; H) ionization mode. NCI; I) ionization energy. 184 eV; J) ion source temperature. 150 ° C; K) quadrupole temperature. 150 ° C; L) Reaction gas. methane, purity greater than or equal 99.99%, reaction gas flow rate. 2 mL/min; M) Detection mode. Select the ion monitoring mode (SIM), see Table 1; N) solvent delay time. 5.5 min. Table 1 Segment Select ion table Pesticide retention time window (min) Retention time (min) Qualitative ion (m/z) Trifluorobenzoate 5.50-7.10 6.50 138 *, 190,298 Ethoxyphenanthrene ether 6.64 296,361 *, 363 Herbicide 6.83 283 *, 284,285 Benzoate 7.02 211 *, 228,264 Picolinate 7.11-7.85 7.26 349,376,412 * Quinoxaline 7.29 271 *, 272,273 Fluorinated Milk Ethers 7.64 378 *, 415,450 Oxygen herbicides 7.72 262,313 *, 315 Achaferrone 7.86-End 8.04 341 *, 342,343 Lactobacillus cerevisiae 8.66 461 *, 462,463 Fluorofenoxylate 8.68 294,447 *, 449 Note. The standard "*" is a quantitative ion. 7.4.2 Determination and confirmation of chromatography According to the amount of pesticide residues in the sample solution, select the standard area similar to the standard working solution, the standard working fluid and sample volume Particle injection. The corresponding values of the pesticide to be tested in the standard working solution and the sample solution shall be within the linear range of the instrument. 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 after subtracting the background After the sample quality chromatogram, the selected ions are present, the abundance of the selected ions is higher than the abundance ratio of the corresponding ions of the standard. Within the allowable range (see Table 2). According to quantitative ions (see Table 1 marked * debris) on its external standard quantitative. Diphenyl ether pesticide mix The total ion chromatogram of gas chromatography-mass spectrometry for standard solutions is shown in Figure A.1 in Appendix A. Table 2 shows the maximum allowable error of relative ion abundance using gas chromatography-mass spectrometry 7.5 blank experiment In addition to the sample, according to the above determination steps.

8 results are calculated and expressed

Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 10% ± 15% ± 20% ± 50% Use the chromatographic data processor or (1) to calculate the amount of pesticide residues in the sample. (1) Where. X - the amount of pesticide residues in the sample solution, in milligrams per kilogram (mg/kg); Ax - the quantitative ion peak area of the pesticide to be tested in the sample solution; Cs ---- the concentration of pesticide in the standard working fluid, in micrograms per milliliter (μg/mL); Vx - the final volume of the sample solution, in milliliters (m L); As - the peak area of the quantified ions in the standard working fluid. M - the quality of the sample represented by the final sample, in grams (g). Note. The result of the calculation must be deducted from the blank value. The result of the measurement is expressed as the arithmetic mean of the parallel measurement, and the two valid digits are retained.

9 precision

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 the requirements of D. 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 E. 10% limit and recovery rate 10.1 Quantitation limits The limit of quantification of 11 kinds of diphenyl ether pesticides in various substrates was 0.01 mg/kg. 10.2 Recovery rate See Appendix C for the recovery range at the additional concentration levels in the different matrices. X = As × m Ax × Cs × Vx

Appendix A

(Informative) Figure A.1 Alkaloid herbicide standard solution GC-MSD/NCI Select ion chromatogram 6.00 6.50 7.00 7.50 8.00 8.50 9.00 9.50 10.00 10.50 11.00 11.50 Tim e - > Abundance TIC. Diphenyl ether-std-3.D \\ data.ms Figure A.1 Total ion chromatogram of GC-MS/NCI mixed standard solution of ether herbicide Among them, 1 trifluoro-nitro-grass; 2 ethoxifluorfen; 3 herbicides; 4 phenylephrine; 5 piccones; 6 quinoxaline; 8 Methoxy herbicides; 9 A Carboxylated Herbicides; 10 Lacto Fen Grass; 11 Fluorofenoxides.

Appendix B

(Informative) Molecular structural information of pesticides to be tested

1 Oxyfluorfen ethoxylate

CAS Number. 42874-03-3 Molecular formula. C15H11ClF3NO4

2 Lactofen Lactoflavones

CAS No.. 77501-63-4 Molecular formula. C19H15ClF3NO7

3 aclonifen

CAS Number. 74070-46-5 Molecular formula. C12H9ClN2O3

4 Fluorodifen

CAS Number. 15457-05-3 Molecular formula. C13H7F3N2O5

5 Bifenox Methyl Carboxylate

CAS Number. 42576-02-3 Molecular formula. C14H9Cl2NO5

6 Fluoroglycofen ethyl fluoride

CAS No.. 77501-90-7 Molecular formula. C18H13ClF3NO7

7 Nitrofen Herbicide

CAS Number. 1836-75-5 Molecular formula. C12H7Cl2NO3

8 Ethoxyfen ethyl fluoride

CAS Number. 131086-42-5 Molecular formula. C19H15Cl2F3O5

9 Ethoxyfen

CAS. 188634-90-4 Molecular formula. C17H11Cl2F3O5 10 Chlomethoxyfen Methoxylated ether CAS Number. 32861-85-1 Molecular formula. C13H9Cl2NO4 11 quinoxyfen CAS Number. 124495-18-7 Molecular formula. C15H8Cl2FNO 12 Paraflufen ethyl CAS Number. 129630-19-9 Molecular formula. C15H13Cl2F3N2O4

Appendix C

(Informative) The range of recovery of various diphenyl ether pesticides in the concentration of different concentrations of matrix Table C.1 Average recovery rates for various diphenyl ether pesticides in food under three added levels sample name 0.01 mg/kg 0.02 mg/kg 0.04 mg/kg 0.10 mg/kg RSD (%) Recovery rate range (%) Recovery rate range (%) Recovery rate range (%) Recovery rate range (%) Rice 80.6 ~ 87.8 96.9 ~ 106.1 87.8 ~ 100.4 97.3 ~ 109.1 5.2 ~ 10.2 Soybean 91.1 ~ 114.5 87.4 ~ 97.3 85.3 ~ 99.0 88.7-107.6 3.2 ~ 10.7 Spinach 86.3 ~ 105.4 98.3 ~ 108.6 91.3 ~ 99.4 86.7-104.1 4.0 ~ 10.2 Green onion 92.1 ~ 106.7 101.4 ~ 116.4 90.2 ~ 103.7 84.5-96.5 3.7 ~ 10.6 Pepper 94.4 ~ 102.3 96.2 ~ 106.9 93.3 ~ 106.0 87.5-117.8 5.0 ~ 10.6 Strawberry 95.0 ~ 114.3 105.2 ~ 111.1 92.0 ~ 101.7 87.7-103.9 5.7 ~ 10.4 Sweet peas 99.0 ~ 119.4 79.3 ~ 92.2 97.4 ~ 102.2 94.4-101.3 5.8 ~ 10.7 Green tea 96.5 ~ 118.9 114.3 ~ 121.5 98.8 ~ 118.9 93.9-101.8 4.1 ~ 10.6 Long shrimp 105.7 ~ 109.8 97.6 ~ 109.1 98.3 ~ 105.9 95.1-106.0 2.6 ~ 10.6 Eel 92.5 ~ 113.5 92.1 ~ 108.7 87.6 ~ 99.0 94.4-102.7 2.2 ~ 9.7 Pork 99.7 ~ 108.5 94.4 ~ 101.6 97.8 ~ 100.3 92.6-111.0 2.9 ~ 10.8 Honey 93.8 ~ 103.3 100.3 ~ 108.5 98.6 ~ 106.2 104.0-117.2 4.1 ~ 10.3

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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