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GB 23200.15-2016 English PDF

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GB 23200.15-2016: Food safety national standard -- Determination of residues of 503 pesticides and related chemicals in edible fungi by gas chromatography-mass spectrometry
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GB 23200.15-2016English1159 Add to Cart 6 days [Need to translate] Food safety national standard -- Determination of residues of 503 pesticides and related chemicals in edible fungi by gas chromatography-mass spectrometry Valid GB 23200.15-2016

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Basic data

Standard ID GB 23200.15-2016 (GB23200.15-2016)
Description (Translated English) Food safety national standard -- Determination of residues of 503 pesticides and related chemicals in edible fungi by gas chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 58,595
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) GB/T 23216-2008
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 23200.15-2016: Food safety national standard -- Determination of residues of 503 pesticides and related chemicals in edible fungi by gas chromatography-mass spectrometry


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Food safety national standard - Determination of residues of 503 pesticides and related chemicals in edible fungi by gas chromatography - mass spectrometry ICS National Standards of People's Republic of China Replace GB/T 23216-2008 National standards for food safety 503 pesticides and related chemicals in edible fungi Determination of residual amount Gas chromatography - mass spectrometry National Food Safety Standards- Determination of 503 pesticides residues in mushrooms Gas chromatography-mass spectrometry 2016-12-18 Release.2017-06-18 Implementation 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 of sample 2 7 Analysis Step 2 Calculation and presentation of results 3 9 precision 4 10% limit and recovery rate 4 Appendix A (informative) 503 kinds of pesticides and related chemicals, English name, method of quantitative limit, grouping, solvent selection and mixing Standard solution concentration Table 5 Appendix B (informative) Retention time for 503 pesticides and related chemicals and internal standard compounds, quantitative ions, qualitative ions and Quantitative ion and qualitative ion abundance ratio Appendix C (informative) A, B, C, D, E, F Six groups of pesticide and related chemicals Selective ion monitoring group Table 27 Appendix D (informative) Reference material Select ion monitoring GC-MS in the medium of the mushroom. Figure 32 Appendix E (informative) Relative standard deviation in the laboratory 38 Appendix F (informative) Inter-laboratory relative standard deviation 39 Appendix G (informative) Experimental data on the concentration and recovery of samples

Foreword

This standard replaces GB/T 23216-2008 "Determination of 503 pesticides and related chemical residues in edible fungi by gas chromatography-mass spectrometry". This standard compared with GB/T 23216-2008, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - increase the "other edible fungi can refer to the implementation" in the standard range. This standard replaced the previous version of the standard release. -GB/T 23216-2008. National standards for food safety Determination of Residues of 503 Pesticides and Related Chemicals in Edible Gas chromatography - mass spectrometry

1 Scope

This standard specifies the amount of 503 pesticides and related chemicals (see Appendix A) Residual gas from mushroom, mushroom, black fungus, mushrooms Determination of Chromatography - Mass Spectrometry. This standard applies to the qualitative identification of 503 kinds of pesticides and related chemicals in the mushroom, mushroom, black fungus, mushrooms, 478 kinds of pesticides and Quantitative determination of related chemicals, other edible fungi 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. 2763 Food Safety National Standard Food Pesticide Maximum Residue Limits 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 acetonitrile toluene (3 1, volume ratio) Off the chemical, with gas chromatography - mass spectrometry, internal 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, 75-05-8). Chromatographic Purification. 4.1.2 Toluene (C7H8, 108-88-3). Chromatographic pure. 4.1.3 n-hexane (C6H14,110-54-3). pure chromatography. 4.1.4 Acetone (CH3COCH3, 67-64-1). Chromatographic pure. 4.1.5 Cyclohexane (C6H12,110-82-7). Chromatographic Purification. 4.1.6 Isooctane (C8H18,540-84-1). Chromatographic pure. 4.1.7 Ethyl acetate (CH3COOCH2CH3,141-78-6). Chromatographic purity. 4.1.8 sodium chloride (NaCl, 7647-14-5). excellent grade pure. 4.1.9 anhydrous sodium sulfate (Na2SO4,7757-82-6). analytical grade. 650 ℃ burning 4 h, stored in a dryer, cooling and standby. 4.2 solution preparation Acetonitrile-toluene solution (3 1). take 300 mL of acetonitrile, add 100 mL of toluene, shake back. 4.3 standards Pesticide and Related Chemical Reference Material. Purity ≥95%, see Appendix A. 4.4 standard solution preparation 4.4.1 Standard stock solution Accurately weigh 5 mg to 10 mg (accurate to 0.1 mg) Pesticides and related chemicals are placed in 10 mL volumetric flask, root According to the solubility of the standard and the need for determination of toluene, toluene acetone mixture, dichloromethane and other solvents dissolved and constant volume to the scale (solvent Choose see Appendix A). The standard stock solution is stored at 4 ° C for 1 year. 4.4.2 internal standard solution Accurately weighed 3.5 mg epoxy heptachlor in 100 mL volumetric flask, with toluene volume to the scale. 4.4.3 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, 503 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 503 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 100 mL volumetric flask, with toluene volume to the scale. Mix the standard solution in the dark at 4 ℃ Save, save for a month. 4.4.4 Substrate 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. 4.5 Materials Sep-Pak CarbonNH2 1) solid phase extraction column. 6 mL, 1 g or equivalent.

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. Equipped with an electron impact source (EI). 5.2 Analysis of balance. 0.1 mg and 0.01 g. 5.3 Centrifuge tube. 80 mL. 5.4 high-speed organization crusher. the minimum speed of not less than 12 000 r/min. 5.5 Centrifuge. the minimum speed of not less than 4.200 r/min. 5.6 chicken heart bottle. 100 mL 5.7 Pipettes. 1 mL and 10 mL. 5.8 Rotary evaporator. 5.9 Vials. 2 mL, with Teflon capping.

6 sample preparation

Edible fungus sample sampling site according to GB 2763 Appendix A, the sample chopped and homogenized homogenized homogenized, the prepared samples were Divided into two, packed into a clean sample container, sealed and marked. The samples were cryopreserved at -18 ° C.

7 Analysis steps

7.1 Extraction Weigh 20 g of sample (accurate to 0.01 g) in 80 mL centrifuge tube, add 40 mL of acetonitrile, 1 5000 r/min homogenate extraction 1 min, Add 5 g sodium chloride, and then homogenate extraction 1 min, at 4.200 r/min under the conditions of centrifugation 5 min, take the supernatant 20 mL (equivalent to 10 g Sample volume), 40 ℃ water bath rotation concentrated to about 1 mL, to be purified. 7.2 Purification Add about 2 cm high anhydrous sodium sulfate to the Sep-Pak CarbonNH2 solid phase extraction column and place the solid phase extraction unit on. The column was pre-washed with 4 mL of acetonitrile-toluene solution before loading, and the sample concentrate was rapidly transferred when the liquid level reached the top of anhydrous sodium sulfate To the purification column, and replace the heart of the bottle to receive. The residual sample was transferred to the extraction column with 2 mL of acetonitrile-toluene solution Times. A 50 mL reservoir was connected to the top of the SPE column and the pesticide and related chemicals were eluted with 25 mL of acetonitrile-toluene solution. 100mL chicken heart bottle, 40 ℃ water bath spin concentrated to about 0.5 mL. Add 5 mL of n-hexane for solvent exchange and repeat twice. set Volume of about 1 mL, add 40 μL internal standard solution, mix, for gas chromatography - mass spectrometry. Sep-Pak CarbonNH2 solid phase extraction column is the product name of Waters' products. This information is provided for the convenience of users of this standard and does not indicate the recognition of the product. If it is His equivalent product has the same effect, you can use these equivalent. At the same time take no pesticide and related chemicals, edible fungus samples, according to the above steps to prepare sample blank extract for the preparation of matrix mixing Standard working solution. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. DB-1701 (14% cyanopropyl-phenyl) -methylpolysiloxane, 30 m x 0.25 mm x 0.25 μm, quartz capillary column Or quite; 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 opening the valve; G) electron bombardment source. 70 eV; H) ion source temperature. 230 ° C; I) GC-MS interface temperature. 280 ° C; J) solvent delay. 8.30min in group A, 7.80min in group B, 7.30min in group C, 5.50min in group D, 6.10min in group E, 5.50min in group F, 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 dwell 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 standard A, B, C, D, E, F Six groups of reference substances Select the ion monitoring GC-MS diagram in the mushroom matrix 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

Gas chromatography - mass spectrometry results can be automatically calculated by the internal standard method of the chromatographic workstation, can also 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 - concentration of internal standard in the standard working solution 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, 4 × LOQ, add the recovery rate see Appendix G.

Appendix A

(Informative) 503 kinds of pesticides and related chemicals, English name, method of quantitative limit, grouping, solvent selection and mixed standard solution concentration A.1 503 kinds of pesticides and related chemicals, English name, method of quantitative limit, grouping, solvent selection and mixed standard solution concentration See Table A.1 Table A.1 503 kinds of pesticides and related chemicals, English name, method of quantitative limit, grouping, solvent selection and mixed standard solution concentration Serial number Chinese name English name The limit of quantitation/ (Μg/kg) Solvent Mix the standard solution Concentration/(mg/L) Group A 1 diacetophenanthrene allidochlor 0.0250 toluene 5.00 2 soil bacteria el etantiazol 0.0376 toluene 7.50 3 Chloromethylthiophosphate chlormephos 0.0250 Toluene 5.00 4 Aniline Ling propham 0.0126 Toluene 2.50 5 ring grass enemy cycloate 0.0126 toluene 2.50 Benzene diamine a diphenylamine 0.0126 Toluene 2.50 7 chlordimeform chlordimeform 0.0126 n-hexane 2.50 8 Ethylene Bromine Ethalfluralin 0.0500 Toluene 10.00 9 phorate phorate 0.0126 toluene 2.50 10 Methyl ethyl phiophosphate thiometon 0.0126 Toluene 2.50 11 Pentachloronitrobenzene quintozene 0.0250 Toluene 5.00 12 Deethyl Etrazine a atrazine-desethyl 0.0126 Toluene Acetone (8 2) 2.50 13 Isosubin pine clomazone 0.0126 Toluene 2.50 14 diazinon 0.0126 toluene 2.50 15 Diposulfuron fonofos 0.0126 Toluene 2.50 16 pyrimethazine etrimfos 0.0126 toluene 2.50 17 Amipropion propetamphos 0.0126 Toluene 2.50 18 sec. Sec. Secancourton 0.0126 Toluene 2.50 19 Acetyl Acetate pronamide 0.0126 Toluene Acetone (9 1) 2.50 20 Removal of phosphorus dichlofenthion 0.0126 Toluene 2.50 21 zyke mexacarbate 0.0376 Toluene 7.50 22 dimethoate 0.0500 Toluene 10.00 23 Amificin dinitramine 0.0500 Toluene 10.00 24 aldrin aldrin 0.0250 toluene 5.00 25 Flies Phosphorus ronnel 0.0250 Toluene 5.00 26 promised net prometryne 0.0126 toluene 2.50 27 cycloprozine cyprazine 0.0126 toluene acetone (9 1) 2.50 Staphylococcus aureus vinclozolin 0.0126 Toluene 2.50 29 beta-hexabutabut-beta-HCH 0.0126 Toluene 2.50 30 metalaxyl metalaxyl 0.0376 toluene 7.50 31 methyl parathion methyl-parathion 0.0500 toluene 10.00 32 chlorpyrifos chlorpyrifos (-ethyl) 0.0126 toluene 2.50 33 δ-six six six delta-HCH 0.0250 toluene 5.00 34 anthraquinone anthraquinone 0.0126 dichloromethane 2.50 35 times thiophosphate fenthion 0.0126 toluene 2.50 36 malathion a malathion 0.0500 toluene 10.00 37 paraoxon-ethyl 0.4000 toluene 80.00 38 fenitrothion fenitrothion 0.0250 toluene 5.00 39 triadimefon 0.0250 toluene 5.00 40 Lee Gu Long a linuron 0.0500 Toluene Acetone (9 1) 10.00 41 pendimethalin pendimethalin 0.0500 toluene 10.00 42 acaricides chlorbenside 0.0250 toluene 5.00 43 ethyl bromothiophosphorus bromophos-ethyl 0.0126 toluene 2.50 Table A.1 (continued) Serial number Chinese name English name The limit of quantitation/ (Μg/kg) Solvent Mix the standard solution Concentration/(mg/L) 44 quetiapine quinalphos 0.0126 toluene 2.50 45 trans-chlordane 0.0126 toluene 2.50 Potato powder phenthoate 0.0250 Toluene 5.00 47 pyrazolamine a metazachlor 0.0376 toluene 7.50 48 propithiol prothiophos 0.0126 Toluene 2.50 49 plasticizer chlorfurenol 0.0376 toluene acetone (9 1) 7.50 50 Pythium Bacteria procymidone 0.0126 Toluene 2.50 51 Dieldrin dieldrin 0.0250 Toluene 5.00 52 Mopapine a methidathion 0.0250 Toluene 5.00 53 Dihydroxylamine napropamide 0.0376 Toluene 7.50 54 Cyhalothiazide a cyanazine 0.0376 Toluene Acetone (8 2) 7.50 55 oxadoxazole oxadiazone 0.0126 Toluene 2.50 56 benzene line phosphorus a fenamiphos 0.0376 toluene 7.50 57 dexamethasone sulfur tetrasul 0.0126 toluene 2.50 58 Ethylpyrazole sulfonate bupirimate 0.0126 Toluene 2.50 59 fluoroamide flutolanil 0.0126 Toluene 2.50 60 Moisturizer 61 p, p'-drop p, p'-DDD 0.0126 Toluene 2.50 Ethoxine 0.0250 Toluene 5.00 63 acetalazole-1 etaconazole-1 0.0376 Toluene 7.50 64 thiophosphate sulprofos 0.0250 toluene 5.00 65 Ethylenediamine-etaconazole-2 0.0376 Toluene 7.50 66 myclobutamycin myclobutanil 0.0126 toluene 2.50 67 Forskophane fensulfothion 0.0250 Toluene 5.00 68 禾 grass spirit diclofop-methyl 0.0126 toluene 2.50 69 propiconazole-1 propiconazole-1 0.0376 Toluene 7.50 70 propiconazole-2 propiconazole-2 0.0376 Toluene 7.50 71 bifenthrin bifenthrin 0.0126 n-hexane 2.50 72 mirex mirex 0.0126 toluene 2.50 73 Fluorophenoxyphenol nuarimol 0.0250 Toluene Acetone (9 1) 5.00 74 wheat rust Ling benodanil 0.0376 toluene 7.50 75 Methanol Drops 76 Oxalic acid oxadixyl 0.0126 Toluene 2.50 77 tebuconazole 0.076 toluene 7.50 78 Tetramethrin tetramethirn 0.0250 Toluene 5.00 79 Fluorfen norflurazon 0.0126 Toluene Acetone (9 1) 2.50 80 pyridazine phosphoric acid pyridapapenthion 0.0126 Toluene 2.50 81 imine thiophosphate phosmet 0.0250 toluene 5.00 82 Diclofenac tetradifon 0.0126 Toluene 2.50 83 cis-permethrin cis-permethrin 0.0126 toluene 2.50 84 Pythium phosphate pyrazophos 0.0250 Toluene 5.00 85 trans-permethrin 0.0126 toluene 2.50 86 cypermethrin cypermethrin 0.0376 toluene 7.50 87 fenvalerate-1 fenvalerate-1 0.0500 toluene 10.00 88 fenvalerate-2 fenvalerate-2 0.0500 toluene 10.00 89 deltamethrin deltamethrin 0.0750 toluene 15.00 Group B 90 turfgrass EPTC 0.0376 Toluene 7.50 Aobutan a butylate 0.0376 Toluene 7.50 92 Diclovir dichlobenil 0.0026 Toluene 0.50 Table A.1 (continued) Serial number Chinese name English name The limit of quantitation/ (Μg/kg) Solvent Mix the standard solution Concentration/(mg/L) 93 grams of grass enemy pebulate 0.0376 toluene 7.50 94 Trichloromethylpyridine nitrapyrin 0.0376 Toluene 7.50 95 times the speed of phosphorus mevinphos 0.0250 toluene 5.00 Chlorobenzene Chloroneb 0.0126 Toluene 2.50 97 Tetrachloronitrobenzene tecnazene 0.0250 Toluene 5.00 98 heptenol heptanophos 0.0376 toluene 7.50 99 off line phosphorus ethoprophos 0.0376 toluene 7.50 100 hexachlorobenzene 0.0126 toluene 2.50 Glutanamine propachlor 0.0376 Toluene 7.50 102 cis - oat enemy cis-diallate 0.0250 toluene 5.00 103 trifluralin 0.0250 toluene 5.00 104 trans - oat enemy trans - diallate 0.0250 toluene 5.00 105 Chloroaniline Ling chlorpropham 0.0250 Toluene 5.00 106 governance borer phosphorus sulfotep 0.0126 toluene 2.50 107 cabbage crabsulfallate 0.0250 toluene 5.00 108 α-hexaflumer alpha-HCH 0.0126 Toluene 2.50 109 Tbn Sulfur Phosphor terbufos 0.0250 Toluene 5.00 110 Tintin a terbumeton 0.0376 Toluene 7.50 111 Ciprofloxacin profluralin 0.0500 Toluene 10.00 112 oxadiazine dioxathion 0.0500 Toluene 10.00 113 Fighting Chin propazine 0.0126 Toluene 2.50 114 Chlorohydrin chlorbufam 0.0250 Toluene 5.00 115 Chloronitamine dicloran 0.0250 Toluene 5.00 116 Tertin butyl terbuthylazine 0.0126 Toluene 2.50 117 Green Valley Long monolinuron 0.0500 Toluene 10.00 118 flufenafil flufenoxuron 0.0376 Toluene 7.50 119 methyl chlorpyrifos-methyl 0.0126 toluene 2.50 120 deer net desmetryn 0.0126 toluene 2.50 121 dimethachlor dimethachlor 0.0376 Toluene 7.50 122 alachlor alachlor 0.0376 toluene 7.50 123 Methylpyrimidine Phosphorus pirimiphos-methyl 0.0126 Toluene 2.50 124 terbutined net terbutryn 0.0250 toluene 5.00 125 Propionate aspon 0.0250 Toluene 5.00 126 Shatan Dan thiobencarb 0.0250 Toluene 5.00 Polychloride dicofol 0.0250 Toluene 5.00 128 metolachlor metolachlor 0.0126 toluene 2.50 129 Pyrimidine Pirimiphos-ethyl 0.0250 Toluene 5.00 130 benzofluorosulfonamide dichlofluanid 0.6000 Toluene Acetone (9 1) 120.00 Potoxapine 10.00 132 bromothiophosphate bromofos 0.0250 tol...

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