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GB 23200.7-2016 English PDF

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GB 23200.7-2016: Food safety national standard -- Determination of 497 pesticides and related chemical residues in honey, fruit juice and fruit wine -- Gas chromatography-mass spectrometry
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GB 23200.7-2016English1419 Add to Cart 7 days [Need to translate] Food safety national standard -- Determination of 497 pesticides and related chemical residues in honey, fruit juice and fruit wine -- Gas chromatography-mass spectrometry Valid GB 23200.7-2016

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Basic data

Standard ID GB 23200.7-2016 (GB23200.7-2016)
Description (Translated English) Food safety national standard -- Determination of 497 pesticides and related chemical residues in honey, fruit juice and fruit wine -- Gas chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 71,783
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) GB/T 19426-2006
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 23200.7-2016: Food safety national standard -- Determination of 497 pesticides and related chemical residues in honey, fruit juice and fruit wine -- Gas chromatography-mass spectrometry



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Food safety national standard - Determination of 497 pesticides and related chemical residues in honey, fruit juice and fruit wine - Gas chromatography-mass spectrometry GB ICS National Standards of People's Republic of China Replace GB/T 19426-2006 National standards for food safety Honey, fruit juice and wine in 497 kinds of pesticides and related Determination of chemical residues Gas chromatography - mass spectrometry National food safety standards- Determination of 497 pesticides and related chemicals Residues in honey, fruit juice and wine 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 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) 497 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, quantitative ion, qualitative ion and determination of 497 pesticides and related chemicals and internal standard compounds The ratio of the amount of ions to qualitative ions Appendix C (informative) A, B, C, D, E Group 5 Group of pesticide and related chemicals Selective ion monitoring group Table 32 Appendix D (informative) Reference material Selective ion monitoring in honey matrix GC-MS Figure 36 Appendix E (informative) Relative standard deviation in laboratory Appendix F (informative) Relative standard deviation between laboratories 42 Appendix G (informative) Experimental data on the concentration and recovery of samples

Foreword

This standard replaces GB/T 19426-2006 "Determination of 497 pesticides and related chemical residues in honey, fruit juice and fruit wine. Spectrum - mass spectrometry ". This standard compared with GB/T 19426-2006, 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 19426-2006. National standards for food safety Determination of 497 pesticides and related chemical residues in honey, fruit juice and fruit wine Gas chromatography - mass spectrometry

1 Scope

This standard specifies the residues of 497 pesticides and related chemicals in honey, fruit juice and fruit wine (see Appendix A). Gas Chromatography-Mass Spectrometry Method. This standard applies to the determination of 497 pesticides and related chemical residues in honey, fruit juice and fruit wine. Other foods can be used for reference.

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 dichloromethane, in series with Envi-Carb1) and Sep-Pak-NH2 2) column, eluting with acetonitrile-toluene solution (3 1) Pesticides and related chemicals, with gas chromatography - mass spectrometry.

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 Acetone (CH3COCH3, 67-64-1). Chromatographic Purification. 4.1.3 dichloromethane (CH2Cl2, 75-09-2). chromatographic purity. 4.1.4 anhydrous sodium sulfate (Na2SO4,7757-82-6). analytical grade. Before burning at 650 ℃ for 4h, stored in a dryer, cooling and standby. 4.1.5 Toluene (C7H8, 108-88-3). Excellent grade pure. 4.1.6 n-hexane (C6H14,110-54-3). pure chromatography. 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 Were weighed 5mg ~ 10mg (accurate to 0.1mg) pesticides and related chemicals in the standard 50mL beaker, according to the standard Dissolved in toluene, toluene - acetone mixture, dichloromethane and other solvents dissolved, transferred to 10mL volumetric flask, respectively, with the corresponding (See Appendix A for solvent selection). The standard solution is stored at 4 ° C for 4 months. The shelf life is one month. 4.3.2 Mixing standard solutions (mixed standard solutions A, B, C, D and E) 497 pesticides and related chemicals are divided into five groups A, B, C, D and E according to the retention time of pesticides and related chemicals, and Depending on the response sensitivity of each pesticide and associated chemical on the instrument, determine its mass concentration in the mixed standard solution. This is the standard The grouping of 497 pesticides and related chemicals and their mixed standard solution mass concentrations are given in Appendix A. Depending on the group number of each pesticide and associated chemical, the mass concentration of the mixed standard solution and the mass concentration of the standard stock solution A certain amount of standard pesticide and related chemicals standard stock solution in 100mL volumetric flask, with toluene volume to the scale. Mix the standard solution Dark 4 ℃ preservation, shelf life of one month. 4.3.3 internal standard solution Accurately weighed 3.5mg epoxy heptachlor in 50mL beaker, dissolved in toluene and then transferred into a 100mL volumetric flask, with toluene volume to Scale. 4.3.4 matrix mixed standard working solution 40 μl of the internal standard solution (4.3.3) and a volume of the mixed standard solution were added to 1.0 mL of the sample blank matrix extract, Mix, mix into matrix mixed standard working solutions A, B, C, D and E. Matrix mixed standard working solution should be used with the current distribution. 4.4 Materials 4.4.1 Envi-Carb Column. 6 mL, 0.5 g or equivalent. 4.4.2 Sep-Pak-NH2 column. 3 mL, 0.5 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. 0.01 g and 0.0001 g. 5.3 chicken heart bottle..200 mL. 5.4 Pipettes. 1 mL. 5.5 stoppered conical flask. 250 mL. 5.6 separatory funnel. 250 mL. 5.7 cylindrical funnel.

6 sample preparation

For non-crystalline honey samples, stir them evenly. For crystalline samples, in a sealed case, place a water bath at a temperature not exceeding 60 ° C In the warm, shaking, until the sample all melt and stir well, quickly cooled to room temperature. 0.5 kg as a sample, placed in a vial, sealed, And mark the mark. Juice, wine samples, all the original samples will be made into a clean enamel mixed barrels, stir and mix thoroughly, and then mix the same The goods are packed in two copies (500 mL each), sealed as a sample, marked with a mark.

7 Analysis steps

7.1 Extraction Weigh 15 g of sample (accurate to 0.01 g) in a 250 mL stoppered flask, add 30 mL of water, shake on a 40 ° C shaking bath Dissolved for 15min. 10 mL of acetone was added, and the contents of the flask were transferred to a 250 mL separatory funnel and washed with 40 mL of dichloromethane And the lotion was poured into a separatory funnel, shaken eight times, carefully vented, left to stand, and the lower organic phase was passed through an anhydrous sulfur The sodium carbonate funnel was collected in a.200 mL heart. Followed by the addition of 5 mL of acetone and 40 mL of dichloromethane in a separatory funnel Shake 1min, standing, stratified collection. The extraction was repeated twice, the extract was combined and the extract was evaporated to about 1 mL in a water bath at 40 ° C, To be purified. 7.2 Purification To the Envi-Carb column was added about 2 cm high anhydrous sodium sulfate, the column was connected to the top of the Sep-Pak-NH2 column and the column was placed The next set of chicken bottles on the fixed frame. The column was pre-washed with 4 mL of acetonitrile-toluene solution before loading, and when the liquid level reached the top of the sodium sulfate, The sample extract was transferred to a purification column and the sample vial was washed with 3 x 2 mL of acetonitrile-toluene solution and the washings were transferred to the column. In the series column Add 50mL of the reservoir, with 25mL acetonitrile - toluene solution of pesticides and related chemicals, collected The Envi-Carb column is the product name of the SUPELCO product, and this information is intended for the convenience of this standard and is not intended to be a recognition of the product. If other equivalent production Products have the same effect, you can use these equivalent products. The Sep-Pak-NH2 column is the product name of Waters' products, and this information is provided for the convenience of this standard and is not intended to be a recognition of the product. If other equivalent production Products have the same effect, you can use these equivalent products. All effluent was placed in a chicken heart and concentrated in a water bath at 40 ° C to about 0.5 mL. The solvent was exchanged twice with 2 x 5 mL of n-hexane, Finally, the sample volume is about 1mL, add 40μL internal standard solution, mix, for gas chromatography - mass spectrometry. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. DB-1701 (30m × 0.25mm × 0.25μm) quartz capillary column or equivalent; B) Column temperature. 40 ℃ for 1min, then 30 ℃/min program temperature to 130 ℃, then 5 ℃/min temperature to 250 ℃, and then The temperature was raised to 300 ℃ at 10 ℃/min for 5 min. C) Carrier gas. helium, purity ≥99.999%, flow rate. 1.2mL/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) Select ion monitoring. 497 kinds of pesticides and related chemicals according to the retention time is divided into A, B, C, D, E five groups, each compound were Choose a quantitative ion, 2 ~ 3 qualitative ions. Each group of all the need to detect the ions in accordance with the peak sequence, respectively, sub-time detection. each The retention time of the compound, the ratio of the quantitative ion, the qualitative ion and the abundance of the quantitative ion to the qualitative ion, see Appendix B. Each group is detected See Appendix C for the start time and dwell time of the ions. 7.3.2 Qualitative determination The samples were extracted according to the conditions of gas chromatography - mass spectrometry, and the samples were determined by group A, B, C, D and E respectively. When the sample is measured, if the test The retention time of the chromatographic peaks is consistent with the standard sample, and the selected ions appear in the sample spectra after subtracting the background, And the selected ion abundance ratio is consistent with the ion abundance ratio of the standard sample (relative abundance > 50%, allow ± 10% deviation; 20% to 50%, ± 15% deviation allowed; relative abundance > 10% to 20%, ± 20% tolerance allowed; relative abundance ≤10%, allowed ± 50% deviation), you can determine the presence of such pesticides or related chemicals in the sample. If you can not confirm, should re-injection to scan (yes Sufficient sensitivity) or by adding other confirmed ions or with other higher sensitivity analytical instruments to confirm. 7.3.3 Quantitative determination The method uses the internal standard method of single ion quantitative determination, the internal standard for the epoxy heptachlor. Quantitative standards should be used in the matrix mixed standard working solution. The mass concentration of the standard solution should be close to the mass concentration of the test compound. The method of A, B, C, D, E five groups of standard substances in honey Select the ion monitoring GC-MS in the 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

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) X = Cs × Ci Asi × (1) As Csi Ai m 1000 Where. 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); The chromatographic peak area of the analyte in the sample solution; As Matrix chromatographic peak area of the test solution in the 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); Asi Matrix chromatographic peak area of standard working solution; Ai The chromatographic peak area of the internal standard in the sample solution; The final volume of the sample solution in milliliters (mL); 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 (percentage) of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean shall be in accordance with the Appendix E requirements. 9.2 The ratio of the absolute difference between the two independent measurements obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with the Appendix 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, 2 × LOQ, 5 × LOQ, the recovery rate is given in Appendix G.

Appendix A

(Informative) 497 kinds of pesticides and related chemicals, English name, method of quantitative limit, grouping, solvent selection and mixed standard solution concentration table A.1 497 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 Chinese name English name The limit of quantitation Solvent Mix the standard solution Mass concentration mg/L mg/kg Epichlorohydrin Heptachlor-epoxide Toluene Group A 1 Dipropenenamine Allidochlor 0.066 Toluene 5 2 allyl amide Dichlormid 0.034 Toluene 2.5 3 soil fungus Etridiazol 0.100 Toluene 7.5 4 Chloromethylthiophosphate Chlormephos 0.066 Toluene 5 5 Aniline Ling Propham 0.034 Toluene 2.5 6 ring grass enemy Cycloate 0.034 toluene 2.5 7 biphenyl diamine Diphenylamine 0.034 Toluene 2.5 8 Chlordimeform 0.034 n-Hexane 2.5 Ethanolluralin 0.132 Toluene 10 10 Phorado Phorate 0.034 Toluene 2.5 11 Methylphenanthroline Thiometon 0.034 Toluene 2.5 12 Pentachlorobenzene Quintozene 0.066 Toluene 5 13 deacetylated atrazine-desethyl 0.034 toluene acetone (8 2) 2.5 14 Clamazone 0.034 Toluene 2.5 15 Diazinon 0.034 Toluene 2.5 16 Pesticide Pon Pum Foxofos 0.034 Toluene 2.5 17 spiramide Etrimfos 0.034 Toluene 2.5 18 Simazine Simazine 0.160 Methanol 2.5 19 Amphetamine Propetamphos 0.034 Toluene 2.5 20 sec-butyl pass Secbumeton 0.034 Toluene 2.5 21 Removal of phosphorus Dichlofenthion 0.034 Toluene 2.5 22 Acetyl Acetate Pronamide 0.034 Toluene Acetone (9 1) 2.5 23 Zeke Mexacarbate 0.100 Toluene 7.5 24 dimethoate 0.102 Toluene 10 25 Aldrin Aldrin 0.066 Toluene 5 26 Ammonol Dinitramine 0.132 Toluene 10 27 Flies Phosphorus Ronnel 0.066 Toluene 5 Smoothing Prometryne 0.034 Toluene 2.5 29 Cycloprozine Cyprazine 0.034 Toluene Acetone (9 1) 2.5 30 Chlorothalonil 0.066 Toluene 5 31 Vinylloxacin Vinclozolin 0.034 Toluene 2.5 32 β-666 Beta-HCH 0.034 Toluene 2.5 33 Metalaxyl 0.100 Toluene 7.5 34 Chlorpyrifos Chlorochrifos (-ethyl) 0.034 Toluene 2.5 Table A.1 35 methyl parathion Methyl-Parathion 0.132 Toluene 10 36 anthraquinone Anthraquinone 0.034 dichloromethane 2.5 37 δ-666 Delta-HCH 0.066 Toluene 5 38 times thiophosphate Fenthion 0.034 Toluene 2.5 39 Malathion 0.182 Toluene 10 40 Fenitrothion 0.066 Toluene 5 Paraoxon-ethyl 0.066 Toluene 10 42 Triadimefon 0.034 Toluene 5 Parathion 0.066 Toluene 10 44 pendimethalin Pendimethalin 0.022 Toluene 10 45 Lee Valley Long Linuron 0.066 Toluene Acetone (9 1) 10 Table A.1 (continued) Chinese name English name quantitative limit solvent Mix the standard solution Concentration (mg/L) (Mg/kg) 46 Acetone Chlorbenside 0.034 Toluene 5 Ethyl bromothiophosphate Bromophos-ethyl 0.016 Toluene 2.5 48 Quetiapine Quinalphos 0.016 Toluene 2.5 49 trans-Chlordane 0.012 Toluene 2.5 50 Puffing Powder Phenthoate 0.034 Toluene 5 51 Pyrazolamine Metazachlor 0.020 Toluene 7.5 52 Benzylthio fenothiocarb 0.012 Acetone 0 53 Phoxim Prothiophos 0.016 Toluene 2.5 54 sterilization Dan Fol Fol 0.200 Toluene 30 55 Flavor alcohol Chlorflurenol 0.010 Toluene Acetone (9 1) 7.5 56 Dieldrin Dieldrin 0.034 Toluene 5 57 Procymidone 0.016 Toluene 2.5 Methidathion 0.022 Toluene 5 Cyanazine 0.026 Toluene Acetone (8 2) 7.5 60 Diquat Napropamide 0.020 Toluene 7.5 61 oxadoxine Oxadiazone 0.016 Toluene 2.5 62 Phenanthroline Fenamiphos 0.034 Toluene 7.5 63 acarbosulfuricides Tetrasul 0.008 toluene 2.5 64 mite special Aramite 0.008 dichloromethane 2.5 Ethyl pyrimethanone Bupirimate 0.012 Toluene 2.5 66 Carrotin Carassin 0.010 Toluene 7.5 67 fluoroamide Flutolanil 0.008 Toluene 2.5 68 p, p'-drop 4,4'-DDD 0.008 Toluene 2.5 69 Ethiophene Ethyl 0.016 Toluene 5 70 thiophosphate Sulprofos 0.014 Toluene 5 71 Acetrazole Etaconazole 0.024 Toluene 7.5 Myclobutanil 0.016 Toluene 2.5 73 Wo Ling Ling Diclofop-methyl 0.008 Toluene 2.5 74 Propiconazole 0.024 Toluene 7.5 Table A.1 Forsulfothion 0.022 Toluene 5 76 Bifenthrin Bifenthrin 0.012 n-hexane 2.5 77 Butylcyclopedia Carbosulfan 0.020 Toluene 7.5 78 Mirex 0.008 Toluene 2.5 79 wheat rust Ling Benodanil 0.016 Toluene 7.5 80 Fluorophenylpyrone Nuarimol 0.014 Toluene Acetone (9 1) 5 81 Methoxyzone 0.0 Methoxychlor 0.0 0.0 Toluene 2.5 82 Oxalic acid Oxadixyl 0.016 Toluene 2.5 83 Tetramethrin Tetramethirn 0.014 Toluene 5 84 tebuconazole 0.024 toluene 7.5 85 Fluorinated Norflurazon 0.016 Toluene Acetone (9 1) 2.5 86 pyridazine phosphoric acid Pyridaphenthion 0.016 Toluene 2.5 87 Amimidophos Phosmet 0.016 Toluene 5 88 Diclofenac Tetradifon 0.012 Toluene 2.5 89 Oxidized Oxalic Acid Oxycarboxin 0.024 Toluene Acetone (9 1) 15 90 cis-permethrin cis-Permethrin 0.016 Toluene 2.5 91 trans-permethrin trans-Permethrin 0.016 Toluene 2.5 Pyralophosphate Pyrazophos 0.014 Toluene 5 Cypermethrin 0.050 toluene 7.5 94 Fenvalerate 0.034 Toluene 10 Deltamethrin 0.100 Toluene 15 Group B 96 Green grass enemy EPTC 0.024 Toluene 7.5 97 Butylate 0.024 Toluene 7.5 98 Diclovir Dichlobenil 0.002 Toluene 0.5 99 grams of grass enemy Pebulate 0.024 toluene 7.5 100 Trichloromethylpyridine Nitrapyrin 0.050 Toluene 7.5 101 V-Phenol Mevinphos 0.034 Toluene 5 102 Chloroanisole Chloroneb 0.016 Toluene 2.5 103 Tetrachloronitrobenzene Tecnazene 0.034 Toluene 5 104 heptenol phosphate Heptanophos 0.050 toluene 7.5 105 Hexachlorobenzene 0.016 Toluene 2.5 106 off line phosphorus Ethoprophos 0.050 toluene 7.5 Chlorpyrifos Propoxlor 0.024 Toluene 7.5 108 oat black cis and trans-diallate 0.034 toluene 5 109 Trifluralin 0.034 Toluene 5 110 Chlorohydrin Ling Chlorpropham 0.034 Toluene 5 111 Chopsticks Sulfotep 0.016 Toluene 2.5 112 Chicken Grass Sulfallate 0.034 Toluene 5 113 α-hexahydra Alpha-HCH 0.034 Toluene 2.5 114 Tb - Sulfur Terbufos 0.034 Toluene 5 115 Tinting Terbumeton 0.024 Toluene 7.5 116 Ciprofloxacin Profluralin 0.066 Toluene 10 117 Oxygen Phosphorus Dioxathion 0.136 Toluene 10 Table A.1 118 Propoxazine Propox 0.016 Toluene 2.5 119 Chloroacetyl Chlorbufam 0.066 Toluene 5 120 nitronamide Dicloran 0.066 toluene acetone (9 1) 5 121 Terbuthylazine 0.016 Toluene 2.5 122 Green Valley Long Monolinuron 0.066 Toluene 10 123 Fipronil Fluffenoxuron 0.100 Toluene Acetone (8 2) 7.5 124 Cacao Cyanophos 0.066 Toluene 5 125 Chlorpyrifos-methyl 0.016 Toluene 2.5 126 Diclofen Desmetryn 0.016 Toluene 2.5 127 Dimethachlor 0.020 Toluene 7.5 128 Alachlor 0.050 Toluene 7.5 129 Methylpyrimidine Pirimiphos-methyl 0.016 Toluene 2.5 130 Tertin Pure Terbutryn 0.034 Toluene 5 131 Shabu Dan Thiobencarb 0.034 Toluene 5 132 Propionate Aspon 0.034 Toluene 5 133 Dicofol 0.034 Toluene 5 134 Metolachlor 0.016 Toluene 2.5 Alkyl Chloride Oxy-chlordane 0.034 Toluene 2.5 Potassium pyrimidine Pirimiphos-ethyl 0.034 Toluene 5 Insectylate Methoprene 0.066 Toluene 10 138 bromothiophosphate Bromofos 0.034 Toluene 5 Phenanthroline Dichlofluanid 0.100 Toluene 15 140 Ethoxy Diclofenac Ethofumesate 0.034 Toluene 5 Isopropalin 0.034 Toluene 142 Endosulfan I 0.100 Toluen...

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