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GB 23200.38-2016 English PDF

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GB 23200.38-2016: Food safety national standard -- Determination of Cyclohexenone Herbicide Residue in Plant-derived Food by Liquid Chromatography-Mass Spectrometry / Mass Spectrometry
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GB 23200.38-2016English259 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of Cyclohexenone Herbicide Residue in Plant-derived Food by Liquid Chromatography-Mass Spectrometry / Mass Spectrometry Valid GB 23200.38-2016

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Basic data

Standard ID GB 23200.38-2016 (GB23200.38-2016)
Description (Translated English) Food safety national standard -- Determination of Cyclohexenone Herbicide Residue in Plant-derived Food by Liquid Chromatography-Mass Spectrometry / Mass Spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 13,138
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 3035-2011
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 23200.38-2016: Food safety national standard -- Determination of Cyclohexenone Herbicide Residue in Plant-derived Food by Liquid Chromatography-Mass Spectrometry / Mass Spectrometry


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Food safety national standard - Determination of Cyclohexenone Herbicide Residue in Plant-derived Food by Liquid Chromatography-Mass Spectrometry/Mass Spectrometry National Standards of People's Republic of China GB Instead of SN/T 3035-2011 National standards for food safety Residual amount of cyclohexenyl ketone herbicide in plant - derived food Of the determination Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of cyclohexanedione herbicides residue in plant-derived foods Liquid 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 3035-2011 "Determination of Cyclohexenone Herbicide Residue in Exported Plant Foods by Liquid Chromatography-Mass Spectrometry / Tandem mass spectrometry ". Compared with SN/T 3035-2011, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name of the "export of plant-derived food" to "plant-derived food." - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 3035-2011. National standards for food safety Determination of Cyclohexanone Herbicide Residue in Plant - derived Food Liquid chromatography - mass spectrometry/mass spectrometry

1 Scope

This standard specifies rice, soybeans, corn, cabbage, potatoes, garlic, grapes and oranges, teproloxydim, Oxycodox, cycloxydim, methoxyphenone, sethoxydim and enx Determination of 6 Cyclohexanone Herbicides by Clethodim and Its Methods by Liquid Chromatography - Tandem Mass Spectrometry. This standard applies to rice, soybeans, corn, cabbage, potatoes, garlic, grapes and oranges in the pyrazone, Thiadenone, phenoxalone, ene-pyridine and enoxurone six kinds of cyclohexene ketone 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 file. 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 residual cyclohexenone herbicides were extracted with acetonitrile, and the extracts were purified by C18 and Envi-Carb solid phase extraction column. Spectrum - mass spectrometry/mass spectrometry detection 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 acetic acid (CH3COOH). pure chromatography. 4.1.4 Acetone (C3H6O). excellent grade pure. 4.1.5 Sodium chloride (NaCl). 4.2 solution preparation 4.2.1 n-Hexane - Acetone (6 4). Take 60 mL of n-hexane, add 40 mL of acetone and mix well. 4.2.2 acetonitrile - water solution (1 1). measure 500 mL of acetonitrile, water volume to 1 L, mix. 4.2.3 0.1% acetic acid aqueous solution. take 1.0 mL of acetic acid, diluted with water and set to 1000 mL. 4.3 standards 4.3.1 Reference substance. Pyrrione (CAS No. 79-41-9), Herbicide (CAS No. 565635-13-7), thiadenone (CAS No. (CAS No. 87820-88-0), olefenil (CAS No. 74051-80-2) and oleokinone (CAS No. 99129-21-2), purity ≥99% (see Appendix A, Appendix A.1 for chemical information). 4.4 standard solution preparation 4.4.1 Cyclohexenone pesticide standard stock solution. respectively, accurately weighed the right amount of cyclohexanone pesticide standard substances, with acetonitrile preparation Concentration of 1000 mg/L standard stock solution, the standard solution to avoid preservation at -18 ℃, the shelf life of 12 months. 4.4.2 Cyclohexenone Pesticide Mixed Intermediate Standard Solution. Absorb the appropriate amount of each standard stock solution and dilute with acetonitrile to a concentration of 1.0 mg/L Of the mixed standard solution, 0 ℃ ~ 4 ℃ dark preservation, the shelf life of 3 months. 4.4.3 matrix mixed standard working solution. absorb the appropriate amount of mixed intermediate standard solution, with blank sample extraction solution concentration of 0μg/L, 10.0 μg/L, 20.0 μg/L, 50.0 μg/L, 100 μg/L and.200 μg/L, respectively. The day of preparation. 4.5 Materials 4.5.1 Graphitized Carbon Black Solid Phase Extraction Column. 3 mL 250 mg, or equivalent. Activated with 3 mL n-hexane-acetone solution before use The column is moist. 4.5.2 C18 solid phase extraction column. Activate with 5 mL acetonitrile before use to keep the column moist. 4.5.3 Microporous membrane. 0.22 μm, organic phase type.

5 instruments and equipment

5.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer. Equipped with an electrospray ion source (ESI). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Tissue crusher. 5.4 pulverizer. 5.5 Scroll Mixer. 5.6 Solid phase extraction unit with vacuum pump. 5.7 nitrogen blowing concentrator. 5.8 Centrifuge. speed of not less than 5 000 r/min. 5.9 Centrifuge tube. 50 mL. 5.10 scale test tube. 15 mL.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 corn, soybeans and rice Take about 500 g of sample, crush and mix thoroughly with a pulverizer. Samples are divided into two copies, into a clean container, sealed, and marked the standard Remember. 6.1.2 cabbage, potatoes, garlic, grapes and oranges Take the sample about 500 g, will be (not available to wash) chopped, with a mashed machine processed into a slurry, mix. The samples are divided into two Copies, into a clean container, sealed, and marked with a mark. Frozen at -18 C. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue. Corn, soy and rice samples Save at room temperature. Chinese cabbage, potato, garlic, grape and orange samples are stored at -18 C.

7 Analysis steps

7.1 Extraction 7.1.1 Corn, soybeans and rice Weigh 5 g (accurate to 0.01 g) sample in a 50 mL stoppered centrifuge tube, add 10 mL of water, whirlpool and mix for 1 h. Then add Into the 4.0 g sodium chloride, then add 15 mL of acetonitrile high-speed homogeneous extraction 3 min, shake extraction 15 min, centrifuged at 5 000 r/min 5 min, The acetonitrile layer was transferred to a 25 mL volumetric flask. The residue was extracted again with 10 mL of acetonitrile and the extracts were combined and bound to 25 with acetonitrile ML. 7.1.2 cabbage, potatoes, garlic, grapes and oranges Weigh 5 g (accurate to 0.01 g) sample in 50 mL stoppered centrifuge tube, then add 2.0 g of sodium chloride, then add 15 mL of acetonitrile high speed Homogenized extraction for 3 min, shaking extraction for 15 min, centrifugation at 5 000 r/min for 5 min, and the acetonitrile layer was transferred to a 25 mL volumetric flask. Residue again With 10 mL of acetonitrile repeated extraction time, combined extract, and acetonitrile constant volume to 25 mL. 7.2 Purification 7.2.1 Soybeans and maize Extraction of 5.0 mL of extract in the C18 solid phase extraction column, at about 1.5 mL/min flow rate of all the sample through the solid phase extraction column, and then The solid phase was extracted with 3 mL of acetonitrile and the whole extract was collected in a 15 mL centrifuge tube and purged with nitrogen at 40 ° C. The residue was dissolved in 3.0 mL of n-hexane-acetone and the solution was added to a treated Envi-Carb solid phase extraction column at about 1.5 mL/min The flow rate was passed through a solid phase extraction column and the sample tubes were rinsed with 5 mL of n-hexane-acetone and the rinsing solution was added to Envi-Carb The solid extract was collected and the whole effluent was collected in a 15 mL centrifuge tube and the nitrogen was blown to near dryness in a 40 ° C water bath. The residue was washed with 1.0 mL of acetonitrile - water dissolved, vortex after mixing, through the microporous membrane, for liquid chromatography - mass spectrometry/mass spectrometry. 7.2.2 Rice, cabbage, potatoes, garlic, grapes and oranges Take 5.0 mL of the extract in 15 mL centrifuge tube, 40 ℃ with N2 blowing to near dry. The residue was dissolved in 2.0 mL of n-hexane-acetone The solution was added to the treated Envi-Carb solid phase extraction column and the sample solution was passed through a solid phase extraction column at a flow rate of about 1.5 mL/min. The sample tubes were rinsed with 5 mL of n-hexane-acetone and the rinsing solution was added to the Envi-Carb solid phase extraction column to collect the whole effluent in 15 ML centrifuge tube, in a 40 ° C water bath, nitrogen blowing to near dry, the residue with 1.0 mL acetonitrile - water dissolved, vortex mixing, the microporous filter Membrane for liquid chromatography - mass spectrometry/mass spectrometry. 7.3 Determination 7.3.1 Liquid Chromatographic Reference Conditions A) Column. Waters Acquity BEH C18 column, 50 mm × 2.1 mm (id), 1.7 μm, or equivalent; B) Column temperature. 40 ° C; C) Injection volume. 10 μL; D) The mobile phase, flow rate and gradient elution conditions are shown in Table 1. Table 1 Mobile phase, flow rate and gradient elution conditions time Min Flow rate ML/min 0.1% acetic acid aqueous solution Acetonitrile 0 0.30 50 50 5.0 0.30 10 90 6.0 0.30 10 90 7.5 0.30 50 50 7.3.2 Mass spectrometry reference conditions A) ionization mode. electrospray ion source; B) Scanning mode. positive ion scanning; C) Detection method. Multiple reaction monitoring (MRM); D) Resolution. Unit resolution; See Appendix B for other reference mass spectrometry conditions. 7.3.3 Determination and confirmation of chromatography 7.3.3.1 Qualitative determination Each selected component selected one parent ion, two or more child ions, in the same experimental conditions, the sample retention of the test substance And the retention time of the matrix standard solution is within ± 2.5%. The relative abundance of the qualitative ions in each sample is close to the concentration Of the matrix of mixed standard working solution corresponding to the relative abundance of qualitative ions were compared, the deviation does not exceed the range specified in Table 2, As there is a corresponding sample in the sample. Table 2 shows the maximum allowable error for relative ion abundance when qualitatively by liquid chromatography-tandem mass spectrometry Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% 7.3.3.2 Quantitative determination Under the optimum working conditions of the instrument, the standard working solution of the matrix was mixed with the peak area as the ordinate and the matrix mixed standard work Solution concentration for the abscissa to draw the standard working curve, with the standard working curve to calculate the sample solution solution concentration (C), sample The response value of the analyte in the solution shall be within the linear range of the instrument determination. If the linear response range is exceeded, the blank matrix solution is applied Line proper dilution. A multi-reaction monitoring (MRM) chromatogram of the six cyclohexene ketone reference materials is shown in Figure C.1 in Appendix C. 7.4 blank experiment In addition to the sample, according to the above determination steps.

8 results are calculated and expressed

Use the chromatographic data processor or calculate the content of each cyclohexanone pesticide in the sample according to the following formula (1). MΑsi VCsiAi   .. (1) Where. Xi - Residual content of each cyclohexanone pesticide in the sample in milligrams per kilogram, mg/kg; The peak area of each cyclohexanone pesticide in sample solution; V - the final volume of the sample solution, in milliliters, mL; Asi - the peak area of each cyclohexene ketone pesticide in standard working fluid; Csi - the concentration of each cyclohexene ketone pesticide in standard working fluid in micrograms per milliliter, g/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

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 E. 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 F requirements. 10% limit and recovery rate 10.1 Quantitation limits The limit of quantification of cyclohexyl ketone pesticides is 0.005 mg/kg. 10.2 Recovery rate The data on the concentration and recovery of the sample are given in Appendix D.

Appendix A

(Informative) Cyclohexenone pesticides Table A.1 Related information about cyclohexanone pesticides Compound name English name Cas No. molecular formula molecular weight molecular structure Pyramidone Teproloxydim 149979-41-9 C17H24ClNO4 341.83. CH2 Cl OH CH2 CH3 Herbs off. Alloxydim 55635-13-7 C17H25NO5 323.37 CC CH2 CH2 CH3 O CH2 CH CH2 OH OCH3 CH3 CH3 Thioketone Cycloxydim 101205-02-1 C17H27NO3S 325.47 CH2 CH2 CH3 CH2 OH CH3 Oxalcone Clethodim 99129-21-2 C17H26ClNO3S 359.91 OH CH2 CH3 O CH2 C Cl CH2CHCH3 CH2CH3 Olefinic acid Sethoxydim 74051-80-2 C17H29NO3S 327.48 OH CH3 O CH3 CH3 CH3 Phenacetone Methoxypheno Ne 87820-88-0 C20H27NO3 329.43 CH2 CH2 CH3 CH3 OH CH3 H3C CH3

Appendix B

(Informative) Mass spectrometry conditions A) electrospray voltage. 3000 V; B) Auxiliary gas flow rate. 750 L/h; C) collision gas. argon; D) curtain air flow rate. 50 L/h; E) ion source temperature. 105 ° C; F) Auxiliary gas temperature. 350 ° C; G) Qualitative ion pair, quantitative ion pair, acquisition time, cone hole voltage and collision energy are shown in Table B.1. Table B.1 Mass Spectrometric Parameters of Cyclohexenone Pesticide Reference Material The name of the compound Reference Reserved time Min Qualitative ion pair / (M/z) Quantitative ion pair / (M/z) Acquisition time / S Collision gas Volume/eV Cone hole voltage/V Pyrrione 1.85 0.05 30 32 342/250 0.05 19 32 Herbs off 2.58 0.05 30 30 324/234 0.05 21 30 Thiadenone 3.18 0.05 29 30 326/280 0.05 18 30 Oxalate 3.38 0.05 29 32 360/268 0.05 18 32 Olefinic acid 3.59 0.05 29 30 328/220 0.05 22 30 Bromethrin 3.78 0.05 28 30 330/284 0.05 18 30 Note. * 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. Non-commercial declaration. The reference mass spectrometry conditions listed in B.1 are performed on a Waters Quattro Premier LC/MS, where the test instrument Model only for reference, does not involve commercial purposes, to encourage standard users to try different manufacturers or models of equipment.

Appendix C

(Informative) Cyclohexanone Pesticide Standard Quality Spectrum Figure C.1 Standard spectrum of cyclohexanone pesticides Enherofen

Appendix D

(Informative) Table D.1 Recovery of Cyclohexenone Drugs in Different Substrates Compounds name Add level Μg/kg Rice Recovery rate range corn Recovery rate range Soybeans Recovery rate range Cabbage Recovery rate range garlic Recovery rate range potato Recovery rate range orange Recovery rate range grape Recovery rate range Pyranone 5 83.8 to 104 84.8 to 94.8 82.6 to 96.4 84.1 to 103 72.9 to 82.7 77.3 to 93.8 88.3 to 103 81.7 to 98.7 10 80.0 to 89.9 86.0 to 97.7 75.8 to 89.7 84.6 to 101 71.5 to 77.7 79.2 to 94.9 85.2 to 94.8 80.1 to 101 50 78.5 to 87.0 77.5 to 89.0 82.0 to 91.0 95.3 to 113 70.0 to 77.4 79.5 to 86.2 80.9 to 87.4 84.4 to 99.9 1000 92.6 to 106 81.1 to 90.2 80.4 to 84.4 89.3 to 92.2 92.9 to 97.4 83.2 to 89.4 80.5 to 86.2 80.4 to 84.4 10000 99.3 ~ 112 80.6 ~ 90.7 85.8 ~ 86.2 90.0 ~ 96.1 86.3 ~ 88.4 98.1 ~ 112 80.4 ~ 88.1 85.8 ~ 87.3 Grass off 5 86.6 to 107 87.8 to 97.6 87.8 to 99.8 70.0 to 84.0 75.5 to 82.9 92.4 to 110 84.0 to 90.1 80.9 to 92.3 10 84.9 to 93.8 83.2 to 93.4 84.7 to 93.8 81.2 to 95.6 68.4 to 73.8 105 to 116 80.4 to 87.5 82.0 to 97.5 50 79.5 to 89.0 75.0 to 84.0 83.0 to 94.2 89.0 to 95.0 70.3 to 78.6 87.2 to 97.2 74.3 to 80.6 88.3 to 106 1000 101 to 120 90.7 to 97.4 81.7 to 86.0 89.8 to 90.0 87.1 to 91.5 87.0 to 109 80.4 to 88.0 81.7 to 86.0 10000 87.8 to 114 88.6 to 90.2 78.5 to 86.2 80.2 to 82.3 83.1 to 96.5 99.6 to 106 86.6 to 88.8 81.5 to 86.2 Thiadenone 5 70.0 to 81.2 70.0 to 77.8 70.0 to 74.8 70.0 to 82.9 70.2 to 82.6 70.3 to 82.7 88.1 to 92.6 85.0 to 100 10 72.4 to 76.6 70.0 to 75.5 70.0 to 76.0 72.8 to 81.3 72.8 to 79.4 77.6 to 80.0 83.6 to 94.3 84.9 to 95.6 50 70.0 to 75.5 70.0 to 78.0 70.0 to 76.5 70.0 to 78.7 86.1 to 92.9 70.4 to 74.7 78.8 to 89.0 86.8 to 101 1000 80.7 to 88.8 82.4 to 89.9 80.0 to 82.3 80.3 to 86.6 82.2 to 87.4 84.7 to 89.3 87.1 to 87.4 80.0 to 82.3 10000 80.1 to 82.1 84.3 to 87.9 80.0 to 82.8 84.8 to 89.2 80.0 to 86.0 80.8 to 90.2 86.4 to 95.8 83.4 to 87.8 Oxadiazone 5 70.4 to 79.0 71.0 to 79.0 70.0 to 87.0 75.0 to 91.3 79.1 to 84.9 71.7 to 84.7 75.0 to 91.3 70.6 to 83.2 10 70.0 to 78.4 70.0 to 77.4 71.0 to 78.6 89.7 to 105 86.2 to 91.3 84.7 to 91.8 89.7 to 105 77.0 to 85.5 50 70.0 to 78.0 70.0 to 74.0 70.3 to 78.5 88.9 to 104 92.5 to 101 71.8 to 78.7 88.9 to 104 83.9 to 94.1 1000 80.5 to 88.1 81.8 to 85.9 80.9 to 84.3 88.0 to 91.1 86.5 to 99.4 88.6 to 90.3 92.2 to 108 78.5 to 82.8 10000 80.1 to 89.7 84.8 to 88.4 85.4 to 89.6 83.3 to 95.5 96.7 to 102 81.1 to 88.1 97.4 to 107 85.4 to 89.6 Phenacetone 5 85.4 to 110 85.2 to 94.6 91.8 to 107 75.9 to 90.8 83.8 to 96.4 79.0 to 83.3 89.2 to 92.3 68.3 to 84.8 10 78.4 to 94.8 74.8 to 79.7 80.9 to 93.6 86.0 to 103 88.4 to 95.4 90.2 to 98.5 88.9 to 97.1 82.5 to 96.5 50 87.0 to 104 84.5 to 87.5 83.0 to 94.0 92.0 to 106 88.7 to 93.5 81.5 to 87.9 87.6 to 91.7 83.7 to 101 1000 81.8 ~ 120 83.9 ~ 90.0 85.8 ~ 90.9 80.5 ~ 87.9 86.6 ~ 90.0 84.3 ~ 88.3 86.9 ~ 88.3 85.8 ~ 90.9 10000 99.3 to 112 80.9 to 82.0 81.0 to 89.0 80.8 to 81.0 80.1 to 83.0 81.8 to 90.4 87.1 to 89.4 83.1 to 89.0 Enanthrene 5 73.4 to 83.2 70.0 to 75.0 70.0 to 79.0 73.3 to 82.3 76.5 to 83.6 74.1 to 83.4 73.3 to 82.3 81.4 to 94.4 10 70.3 to 77.0 71.1 to 76.8 70.0 to 80.4 86.5 to 103 83.2 to 91.3 78.4 to 90.1 86.5 to 103 80.5 to 97.8 50 70.0 to 75.0 70.0 to 77.0 70.0 to 78.0 87.3 to 104 87.7 to 95.5 72.7 to 76.6 87.3 to 104 83.5 to 101 1000 82.6 to 106 80.6 to 85.2 92.6 to 97.8 83.9 to 84.6 80.1 to 81.8 80.9 to 88.2 94.4 to 111 82.8 to 97.8 10000 91.7 to 97.4 80.6 to 85.3 87.5 to 100 81.4 to 88.7 90.4 to 98.9 80.0 to 89.2 99.1 to 110 97.5 to 101

Appendix E

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

Appendix F

(Normative appendix) Inter-laboratory reproducibility requirements Table F.1 Inter-laboratory reproducibility requirements Measured component content Mg/kg Precision 0.001 54 > 0.01 > 1 19

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