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GB 23200.10-2016 English PDF

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GB 23200.10-2016: Food safety national standard -- Determination of 488 pesticides and related chemicals residues in mulberry, honeysuckle, medlar and lotus leaf by gas chromatography-mass spectrometry
Status: Valid
Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
GB 23200.10-20161119 Add to Cart 6 days Food safety national standard -- Determination of 488 pesticides and related chemicals residues in mulberry, honeysuckle, medlar and lotus leaf by gas chromatography-mass spectrometry Valid

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Basic data

Standard ID: GB 23200.10-2016 (GB23200.10-2016)
Description (Translated English): Food safety national standard -- Determination of 488 pesticides and related chemicals residues in mulberry, honeysuckle, medlar and lotus leaf by gas chromatography-mass spectrometry
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Word Count Estimation: 56,536
Date of Issue: 2016-12-18
Date of Implementation: 2017-06-18
Older Standard (superseded by this standard): GB/T 23200-2008
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 23200.10-2016: Food safety national standard -- Determination of 488 pesticides and related chemicals residues in mulberry, honeysuckle, medlar and lotus leaf 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 - Determination of 488 pesticides and related chemicals residues in mulberry, honeysuckle, medlar and lotus leaf by gas chromatography-mass spectrometry ICS National Standards of People's Republic of China Replacing GB/T 23200-2008 National standards for food safety Mulberry, honeysuckle, medlar and lotus leaf in 488 kinds of agriculture Determination of residues of drugs and related chemicals Gas chromatography - mass spectrometry National food safety standards- Determination of 488 pesticides and related chemicals residues in mulberry twig, Honeysuckle, barbary wolfberry fruit and lotus leaf 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 GB Directory Preface II 1 Scope 1 2 normative reference document 1 Principle 1 4 reagents and materials 1 5 instruments and equipment 2 6 Preparation and storage of sample 2 7 Analysis Step 2 Calculation and presentation of results 3 9 precision 3 10% limit and recovery rate 3 Appendix A (informative) 488 pesticides and related chemicals Chinese and English names, methods Quantitative limits, grouping, solvent selection And mixed standard solution concentrations Appendix B (Informative Annex) Retention Time, Quantitative Ion, Qualitative Ions and Definitions of 488 Pesticides and Related Chemicals and Internal Labels The abundance ratio of the amount of ions to qualitative ions Appendix C (Informative Appendix) Group A, B, C, D, E and F Group 6 Pesticide and Related Chemicals Selection Ion Monitoring Group Table 30 Appendix D (informative) Reference substance Selective ion monitoring GC-MS in medlar substrate Figure 35 Appendix E (informative) Relative standard deviation in laboratory 4 1 Appendix F (informative) Relative standard deviation between laboratories Appendix G (informative) Experimental data on the concentration and recovery of samples

Foreword

This standard replaces GB/T 23200-2008 "residues of 488 pesticides and related chemicals in mulberry, honeysuckle, medlar and lotus leaf Determination of gas chromatography - mass spectrometry ". This standard compared with GB/T 23200-2008, 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. -GB/T 23200-2008. National standards for food safety 818 kinds of pesticides and related chemical residues in mulberry, honeysuckle, medlar and lotus leaf Determination of gas chromatography - mass spectrometry

1 Scope

This standard specifies the residues of 488 pesticides and related chemicals (see Appendix A and Appendix F) residues of mulberry, honeysuckle, medlar and lotus leaf Quantitative Gas Chromatography - Mass Spectrometry. This standard applies to the qualitative identification of 488 pesticides and related chemicals in mulberry, honeysuckle, medlar and lotus leaf, 431 pesticides and phase Quantitative determination of chemicals, 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 homogenate, salted out by centrifugation, solid phase extraction column, eluted with n-hexane-acetone and related chemicals. Chromatography - mass spectrometry, internal 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 Acetonitrile (CH3CN, 75-05-8). Chromatographic Purification. 4.1.2 sodium chloride (NaCl, 7647-14-5). excellent grade pure. 4.1.3 dichloromethane (CH2Cl2, 75-09-2). chromatographic purity. 4.1.4 Acetone (CH3COCH3, 67-64-1). Chromatographic pure. 4.1.5 n-Hexane (C6H14,110-54-3). Chromatography pure, re-distillation. 4.1.6 Toluene C7H8, 108-88-3). Chromatographic Purification. 4.1.7 anhydrous sodium sulfate (Na2SO4,7757-82-6). analytical grade. 650 ℃ burning 4h, stored in a dryer, cooling and standby. 4.2 standards Pesticide and Related Chemical Reference Material. Purity ≥95%, see Appendix A. 4.3 standard solution preparation 4.3.1 Standard stock solution Respectively, to take appropriate (accurate to 0.1mg) a variety of pesticides and related chemical standards were 10mL volumetric flask, according to the standard Solvents Toluene, toluene-acetone mixture, dichloromethane and other solvents (solvents are used chromatographic pure) dissolved and fixed to the scale (solvent Select the reference to Appendix A), the standard solution from light 0 ℃ ~ 4 ℃ preservation, shelf life of one year. 4.3.2 Mixing standard solutions (mixed standard solutions A, B, C, D, E and F) According to the nature and retention time of pesticides and related chemicals, 488 kinds of pesticides and related chemicals are divided into A, B, C, D, E, F Six groups and determine their concentration in the mixed standard solution based on the response sensitivity of each pesticide and associated chemical on the instrument. This standard Refer to Appendix A for the grouping of 488 pesticides and related chemicals and their mixed standard solution concentrations. Depending on the group number of each pesticide and associated chemical, the concentration of the standard solution and the concentration of the standard stock solution, Pesticide and related chemicals standard stock solution in a 100mL volumetric flask, with toluene volume to the scale. Mixed standard solution light 0 ℃ ~ 4 ℃ Save, save for one month. 4.3.3 internal standard solution Accurately weigh 3.5 mg Epoxy Heptachlor in a 100 mL volumetric flask and settle with a volume of toluene. 4.3.4 matrix mixed standard working solution A, B, C, D, E, F group of pesticides and related chemical matrix mixed standard working solution is 40 μL internal standard solution and a certain volume The mixed standard solutions of A, B, C, D, E and F were added to 1.0 mL of the sample blank matrix extract respectively, Standard working solutions A, B, C, D, E and F. Matrix mixed standard working solution should be used with the current distribution. 4.4 Materials 4.4.1 Solid phase extraction column. CleanertTPH1) 10 mL, 2.0 g, or equivalent. 4.4.2 Microporous membrane (nylon). 13mm × 0.2μm.

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. Equipped with an electron impact source (EI). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Rotary Evaporator. 5.4 Homogenizer. The maximum speed is 24 000 r/min. 5.5 Centrifuge. Maximum speed is 4.200 r/min. 5.6 chicken heart bottle. 150 mL. 5.7 Pipettes. 1 mL.

6 Preparation and storage of samples

6.1 Preparation of the sample Will be mulberry, honeysuckle, medlar and lotus leaf four kinds of Chinese herbal medicine grinding into fine powder, the sample all over 425μm standard mesh sieve, mix, The prepared samples are divided into two parts, packed in a clean container, sealed and marked.

7 Analysis steps

7.1 Extraction Respectively, to take honeysuckle, medlar sample 5 g or lotus leaf, mulberry sample 2.5 g (accurate to 0.01g) in 50mL centrifuge tube, plus Into 15 mL of acetonitrile, (wolfberry fruit samples need to add 5 mL of water), 15000 r/min homogenate extraction 1min, add 2 g sodium chloride, and then homogenate Extract 1min, 4200 r/min centrifugal 5 min, take all the supernatant in 150mL chicken heart bottle, and then in the centrifuge tube by adding 15 mL of acetonitrile, Repeat the homogenate for 1 min, centrifuge at 4200 r/min for 5 min, take all the supernatant and the previous extract combined, the extract in 40 ℃ water Bath rotation to 1mL ~ 2 mL, to be purified. 7.2 Purification Add about 2 cm high anhydrous sodium sulphate to the CleanertTPH solid phase extraction column and place it on a holder. Before loading, add 10mL Alkyl-acetone solution, the sample concentrate (7.1) is rapidly moved into the column when the pre-wash liquid level reaches the top of the anhydrous sodium sulfate, And receive the leaching solution with a chicken heart bottle. Wash the heart with 2 mL n-hexane-acetone solution, repeat three times, the same washing liquid into the column, The column was connected to a 25 mL reservoir and the pesticide and related chemicals were eluted with 25 mL of n-hexane-acetone solution. The eluent was rotated at 40 ° C Concentrated to near dry, add 1 mL of n-hexane dissolved residue, add 40 μL internal standard solution, mix, 0.2 μm filter, gas chromatography - Mass spectrometry. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. DB-1701 quartz capillary column [14% cyanopropyl-phenyl-methylpolysiloxane; 30 m x 0.25 mm (inner diameter), 0.25 Μm] or equivalent. B) Column temperature. 40 ℃ for 1 min, then 30 ℃/min program temperature to 130 ℃, then 5 ℃/min temperature to 250 ℃, And then to 10 ℃/min temperature to 300 ℃, keep 5 min; C) Carrier gas. helium, purity ≥99.999%, flow rate. 1.2 mL/min; D) Inlet temperature. 290 ° C; E) Injection volume. 1 μL; F) Injection method. no split injection, 1.5 min after the opening valve; G) electron bombardment source. 70 eV; H) ion source temperature. 230 ° C; I) GC-MS interface temperature. 280 ° C; J) solvent delay. 8.3 min in group A, 7.8 min in group B, 7.3 min in group C, 5.5 min in group D, 6.1 min in group E, 6.1 min in group E, Group was 5.5 min; Cleanert TPH is a trade name of Agela's products, and this information is intended for the convenience of users of this standard and is not intended to endorse the product. If other equivalent Products have the same effect, you can use these equivalent products. K) Select the ion monitoring. each compound selected a quantitative ion, 2 ~ 3 qualitative ions. Each group needs to be tested Ions in accordance with the peak sequence, respectively, sub-time detection. The retention time of each compound, the quantitative ion, the qualitative ion and the quantitative ion For the abundance ratio of qualitative ions, see Appendix B. Refer to Appendix C for the start time and residence time of each group to detect ions. 7.3.2 Qualitative determination When the sample is measured, if the retention time of the detected peaks is consistent with the standard sample, and after the background mass In the figure, the selected ions are present, and the selected ion abundance ratio is consistent with the ion abundance ratio of the standard sample (relative abundance > 50% Allow ± 10% deviation; relative abundance > 20% to 50% allow ± 15% deviation; relative abundance > 10% to 20% allow ± 20% deviation; Relative abundance ≤ 10%, allowing ± 50% deviation), you can determine the presence of this pesticide or related chemicals in the sample. If it can not be confirmed, should be heavy New injection, in scanning mode (with sufficient sensitivity) or by adding other confirmed ions or with other higher sensitivity analytical instruments To confirm. 7.3.3 Quantitative determination This standard uses the internal standard method of single ion quantitative determination. The internal standard is epoxy heptachlor. To reduce the impact of the matrix, quantitative standards should be used Quality sample solution mixed with standard working solution. The concentration of the standard solution should be close to the concentration of the compound to be tested. The method of A, B, C, D, E, F group of reference substances in the wolfberry matrix selection of ion monitoring GC-MS Figure see Appendix D. 7.4 parallel test Perform the parallel test of the same sample according to the above steps. 7.5 blank test Unless the sample is not weighed, according to the above steps.

8 results are calculated and expressed

The result of gas chromatography-mass spectrometry can be calculated automatically by computer according to internal standard method, and can be calculated according to formula (1) Xi = cs × Ci Asi (1) As csi Ai m 1000 Where. Xi - Residue of the test substance in milligrams per kilogram (mg/kg); Cs - the concentration of the test substance in the standard working solution in micrograms per milliliter (μg/mL); A - the chromatographic peak area of the analyte in the sample solution; As - the chromatographic peak area of the test substance in the matrix standard working solution; Ci - the concentration of the internal standard in the sample solution, in micrograms per milliliter (μg/mL); Csi - the concentration of the internal standard in the standard working solution of the matrix, in micrograms per milliliter (μg/mL); Asμ - the chromatographic peak area of the internal standard in the matrix standard working solution; Ai - the chromatographic peak area of the internal standard in the sample solution; V - the final volume of the sample solution in milliliters (mL); M - the mass of the sample represented by the sample solution, in grams (g). The result of the calculation should be deducted from the blank value. The result of the measurement is expressed by 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 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 quantitative limits of this method are given in Appendix A. 10.2 Recovery rate When adding levels of LOQ, 20 × LOQ, add the recovery rate see Appendix G.

Appendix A

(Informative) 488 kinds of pesticides and related chemicals Chinese and English name, method of quantitative limit, grouping, solvent selection and mixed standard solution concentration A.1 488 Pesticides and Related Chemicals Chinese and English Name, Method Quantification Limits, Grouping, Solvent Selection and Mixing Standard Solution Concentration See Table A.1 Table A.1 unit.% Serial number Chinese name English name The limit of quantitation/ Solvent Mixed standard Solution concentration / (Mg/L) (Mg/kg) Internal standard epoxy heptachlor-epox Group A 1 2-Propyl Acetate allidochlor 0.0500 Toluene 5 2 allyl chloride dichlormid 0.0500 toluene 5 3 soil fungus etridiazol 0.0750 toluene 7.5 4 Chloromethylthiophosphate chlormephos 0.0500 Toluene 5 5 aniline spirit propham 0.0250 toluene 2.5 6 ring grass enemy cycloate 0.0250 toluene 2.5 7 biphenyl diamine diphenylamine 0.0250 toluene 2.5 8 chlordimeform chrysanthemum 0.0250 n-hexane 2.5 9 Ethylene Bromine Ethalfluralin 0.1000 Toluene 10 10 phorate phorate 0.0250 toluene 2.5 11 methyl ethyl phthalide thiometon 0.0250 toluene 2.5 12 Pentachloronitrobenzene quintozene 0.0500 Toluene 5 13 deethyletrazine atrazine-desethyl 0.0250 Toluene Acetone (8 2) 2.5 14 isosubicin clomazone 0.0250 toluene 2.5 15 diazinon 0.0250 toluene 2.5 16 toxaphene fonofos 0.0250 toluene 2.5 17 spiramide etrimfos 0.0250 toluene 2.5 18 Amipropion propetamphos 0.0250 Toluene 2.5 19 sec. Sec. Secancourt 20 propargyl grass amine pronamide 0.0250 Toluene Acetone (9 1) 2.5 21 Removal of phosphorus dichlofenthion 0.0250 Toluene 2.5 22 zwick mexacarbate 0.0750 toluene 7.5 23 dimethoate 0.1000 toluene 10 24 Amificin dinitramine 0.1000 Toluene 10 25 aldrin aldrin 0.0500 toluene 5 26 dolphin phosphorus ronnel 0.0500 toluene 5 27 promised net prometryne 0.0250 toluene 2.5 28 cycloprozine cyprazine 0.0250 Toluene Acetone (9 1) 2.5 29 Vermoderma vellozolin 0.0250 Toluene 2.5 30? -hexachlorazine-HCH 0.0250 Toluene 2.5 31 metalaxyl metalaxyl 0.0750 toluene 7.5 32 methyl parathion methyl-parathion 0.1000 Toluene 10 Serial number Chinese name English name The limit of quantitation/ Solvent Mixed standard Solution concentration / (Mg/L) (Mg/kg) 33 chlorpyrifos (-ethyl) 0.0250 toluene 2.5 34 δ-six six six delta-HCH 0.0500 Toluene 5 35 times thiophosphate fenthion 0.0250 toluene 2.5 36 malathion malathion 0.1000 Toluene 10 37 paraoxon-ethyl 0.8000 toluene 80 38 fenitrothion 39 triazolone triadimefon 0.0500 toluene 5 40 Lee Valley Long linuron 0.1000 Toluene Acetone (9 1) 41 pendimethalin pendimethalin 0.1000 toluene 10 42 acylidene chloride 43 Ethyl bromothiophosphate bromophos-ethyl 0.0250 Toluene 2.5 44 quetiapine quinalphos 0.0250 toluene 2.5 45 trans-chlordane 0.0250 toluene 2.5 Potato powder scattered phenthoate 47 pyrazolamine metazachlor 0.0750 toluene 7.5 48 propithiol prothiophos 0.0250 toluene 2.5 49 shaped plastic chlorfurenol 0.0750 Toluene Acetone (9 1) 7.5 50 Pythium Bermidipine 0.0250 Toluene 2.5 Dieldrin dieldrin 0.0500 Toluene 5 52 Methamidone A methidathion 0.0500 Toluene 5 53 Dihydroxylamine napropamide 0.0750 Toluene 7.5 54 cyanocobalt cyanazine 0.0750 Toluene Acetone (8 2) 7.5 55 maloxine oxadiazone 0.0250 toluene 2.5 56 benzene line phosphorus fenamiphos 0.0750 toluene 7.5 57 acaricides sulfur sulfide tetrasul 0.0250 toluene 2.5 58 Ethyl pyrimethanol sulfonate bupirimate 0.0250 Toluene 2.5 59 fluoroamide a flutolanil 0.0250 toluene 2.5 60 Moisturizer a carboxin 0.6000 Toluene 60 61 p, p'-drop p, p'-DDD 0.0250 toluene 2.5 62 Ethiophenazine Ethion 0.0500 Toluene 5 63 Acetazole-1 etaconazole-1 0.0750 Toluene 7.5 64 thiophosphate sulprofos 0.0500 toluene 5 65 etetonazole-2 etaconazole-2 0.0750 toluene 7.5 66 myclobutamycin myclobutanil 0.0250 toluene 2.5 67 Forskophil Pineulfothion 0.0500 Toluene 5 68 禾 grass spirit diclofop-methyl 0.0250 toluene 2.5 69 propiconazole-1 propiconazole-1 0.0750 toluene 7.5 70 propiconazole-2 propiconazole-2 0.0750 Toluene 7.5 71 bifenthrin bifenthrin 0.0250 n-hexane 2.5 72 Mirex mirex 0.0250 Toluene 2.5 73 Butylcyclopedia carbosulfan 0.0750 Toluene 7.5 Serial number Chinese name English name The limit of quantitation/ Solvent Mixed standard Solution concentration / (Mg/L) (Mg/kg) 74 Fluorophenylpyrimidine nuarimol 0.0500 Toluene Acetone (9 1) 75 wheat rust Ling benodanil 0.0750 Toluene 7.5 76 Oxygen DDT methoxychlor 0.2000 Toluene 20 77 Oxalic acid oxadixyl 0.0250 Toluene 2.5 78 tebuconazole 0.0750 toluene 7.5 79 Tetramethrin tetramethirn 0.0500 Toluene 5 80 Fluorfenin norflurazon 0.0250 Toluene Acetone (9 1) 2.5 81 pyridazine sulfur phosphorus pyridaphenthion 0.0250 toluene 2.5 82 Dicofloxacin tetradifon 0.0250 Toluene 2.5 83 cis-permethrin cis-permethrin 0.0250 toluene 2.5 84 Pyridobacill......
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