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Delivery: <= 6 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.11-2016: Food safety national standard -- Determination of 413 Pesticides and Related Chemicals Residues in Mangzhi, Honeysuckle, Medlar and Lotus Leaves by Liquid Chromatography-Mass Spectrometry Status: Valid
Basic dataStandard ID: GB 23200.11-2016 (GB23200.11-2016)Description (Translated English): Food safety national standard -- Determination of 413 Pesticides and Related Chemicals Residues in Mangzhi, Honeysuckle, Medlar and Lotus Leaves by Liquid Chromatography-Mass Spectrometry Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 59,595 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): GB/T 23201-2008 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.11-2016: Food safety national standard -- Determination of 413 Pesticides and Related Chemicals Residues in Mangzhi, Honeysuckle, Medlar and Lotus Leaves by Liquid 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 413 Pesticides and Related Chemicals Residues in Mangzhi, Honeysuckle, Medlar and Lotus Leaves by Liquid Chromatography-Mass Spectrometry Replacing GB/T 23201-2008 ICS National standards for food safety Mulberry, honeysuckle, medlar and lotus leaf 413 kinds of farmers Determination of residues of drugs and related chemicals Liquid chromatography - mass spectrometry National food safety standards- Determination of 413 pesticides and related chemicals residues in mulberry twig, Honeysuckle, barbary wolfberry fruitand lotus leaf Liqulid chromatography-mass spectrometry 2016-12-18 Release.2017-06-18 Implementation National Standards of People's Republic of China 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 4 9 precision 4 10% limit and recovery rate 4 Appendix A (informative) 413 kinds of pesticides and related chemicals in English name, method of quantitative limit, grouping, solvent selection and mixing Standard solution concentration Table 5 Appendix B (informative) 413 pesticides and related chemicals Monitoring of ion impact energy, source fragmentation voltage and retention Between 1 5 Appendix C (informative) 413 Pesticide and Related Chemicals Multiple Reaction Monitoring (MRM) Chromatogram 24 Appendix D (informative) Relative standard deviation in laboratory 4 2 Appendix E (informative) Relative standard deviation between laboratories Appendix F (informative) Experimental data on the concentration and recovery of samples ForewordThis standard replaces GB/T 23201-2008 "413 kinds of pesticide and related chemical residues in mulberry, honeysuckle, medlar and lotus leaf Determination of liquid chromatography - tandem mass spectrometry ". This standard compared with GB/T 23201-2008, 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 23201-2008. National standards for food safety 813 pesticides and related chemical residues in mulberry, honeysuckle, medlar and lotus leaf Determination of liquid chromatography - mass spectrometry1 ScopeThis standard specifies the residues of 413 pesticides and related chemicals (see Appendix A and Appendix E) residues in mulberry, honeysuckle, medlar and lotus leaf Determination of liquid chromatography - mass spectrometry. This standard applies to the determination of 413 pesticides and related chemicals residues in mulberry, honeysuckle, medlar and lotus leaf, and other foods may be Refer to execution.2 normative reference documentsThe 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 methods3 principleThe samples were extracted with acetonitrile homogenate, salted out by centrifugation and solid phase extraction column. The pesticide and related chemicals were eluted with acetonitrile-toluene solution (3 1) Determination by liquid chromatography - tandem mass spectrometry, external standard method.4 reagents and materialsUnless 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 Methanol (CH3OH, 67-56-1/170082-17-4). Chromatographic Purification. 4.1.4 Cyclohexane (C6H12,110-82-7). Chromatographic purity. 4.1.5 Isooctane (C8H18,540-84-1). Chromatographic pure. 4.1.6 Sodium chloride (NaCl, 7647-14-5). 4.1.7 anhydrous sodium sulfate (Na2SO4,7757-82-6). 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) pesticides and related chemical standards in 10mL volumetric flask, according to the standard solubility of the election Methanol, toluene, cyclohexane or isooctane and other solvents dissolved and constant volume to the scale (solvent options see Appendix A). The standard stock solution is protected from light by 0 ° C ~ 4 ℃ preservation, preservation period of one year. 4.3.2 Mixing standard solutions (mixed standard solutions A, B, C, D, E, F and G) 413 pesticides and related chemicals are classified into A, B, C, D, E, F according to the nature and retention time of pesticides and related chemicals And G seven groups, and according to the sensitivity of each pesticide and related chemicals on the instrument to determine its concentration in the mixed standard solution. This standard classifies 413 pesticide and related chemicals and their mixed standard solution concentrations (see Appendix A). Depending on the concentration 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 a fixed volume of methanol to the mark. Mixed standard solution light 0 ℃ ~ 4 ℃ Save, save for one month. 4.3.3 matrix mixed standard working solution Pesticide and related chemicals Substrate mixed standard working solution is prepared by mixing the sample with different concentrations of the substrate mixed with standard working solution Liquid A, B, C, D, E, F and G are used for standard working curves. Matrix mixed standard working solution should be used with the current distribution. 4.4 Materials 4.4.1 Cleanert TPH 1 column. 10mL 2.0g, or equivalent. 4.4.2 Microporous membrane (nylon). 13mm × 0.2μm.5 instruments and equipment5.1 Liquid Chromatography - Tandem Mass Spectrometer. Equipped with electrospray ion source (ESI). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Homogenizer. The maximum speed is 24000 r/min. 5.4 Centrifuge. The maximum speed is 4200 r/min. 5.5 Rotary evaporator. 5.6 chicken heart bottle. 150 mL. 5.7 Pipettes. 1 mL. 5.8 Centrifugal tube. 50 mL. 5.9 Vials. 2 mL, with Teflon capping. 5.10 nitrogen dryers.6 sample preparationWill mulberry, honeysuckle and lotus leaf three kinds of Chinese herbal medicine grinding into fine powder, the sample all over 425μm standard mesh sieve, mix well, prepared Samples are divided into two, into the cleaning container, sealed, marked mark. Wolfberry can be used directly.7 Analysis steps7.1 Extraction Weigh the honeysuckle, medlar, lotus leaf and mulberry sample 2g (accurate to 0.01g) in 50mL centrifuge tube, add 15mL acetonitrile And then add 2g of sodium chloride, and then homogenate extraction 1min, 4200 r/min Centrifuge 5min, take all the supernatant in 150 mL chicken heart bottle, in the centrifuge tube and then add 15mL acetonitrile, repeat homogenate extraction 1min, 4200 r/min centrifugal 5min, take all the supernatant and the previous extract combined in 40 ℃ water bath rotation to 1 mL ~ 2mL, to be purified. 7.2 Purification Add about 2 cm of anhydrous sodium sulfate to the Cleanert TPH column and place it on a holder. Add 10 mL of acetonitrile-toluene solution before loading Pre-wash the column, when the pre-wash liquid level to reach the top of anhydrous sodium sulfate, the rapid concentration of the sample into the column, and with the heart of the bottle to receive leaching Out of liquid. Respectively, with 2mL acetonitrile - toluene solution washed heart bottle twice, the washing liquid is also transferred into the column, the column connected 25mL reservoir, With 25mL acetonitrile - toluene solution of pesticides and related chemicals, the eluent in the 40 ℃ water bath spin concentrated to 1 mL ~ 2 mL, will be concentrated The solution was dried on a nitrogen dry drier, 1 mL of acetonitrile-water was added, mixed with a 0.2 μm filter, and analyzed by liquid chromatography-tandem mass spectrometry. 7.3 Determination 7.3.1 Liquid Chromatography - Tandem Mass Spectrometry Conditions 7.3.1.1 A, B, C, D, E, F LC-MS-MS measurement conditions (ESI positive ion source) A) Column. ZORBOX SB-C18, 3.5 μm, 100 mm x 2.1 mm (inner diameter) or equivalent; 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 With the same effect, you can use these equivalent products. B) mobile phase and gradient elution conditions in Table 1; Table 1 Mobile phase and gradient elution conditions table Total flow/min Flow rate/(μL/min) Mobile phase A (0.1% formic acid) /% Mobile phase B (acetonitrile) /% 0 0.00 400 99.0 1.0 1 3.00 400 70.0 30.0 2 6.00 400 60.0 40.0 3 9.00 400 60.0 40.0 4 15.00 400 40.0 60.0 5 19.00 400 1.0 99.0 6 23.00 400 1.0 99.0 7 23.01 400 99.0 1.0 C) Column temperature. 40 ° C; D) Injection volume. 10 μL; E) ion source. ESI; F) Scanning mode. positive ion scanning; G) Detection method. multiple reaction monitoring; H) ion spray voltage. 4000V; I) atomization gas pressure. 0.28 MPa; J) Dry gas temperature. 350 ° C; K) Dry gas flow rate. 10 L/min; L) Monitor ion pair, collision energy and source fragmentation voltage See Appendix B. 7.3.1.2 Group G LC-MS-MS Assay Conditions (ESI Negative Ion Source) A) Column. ZORBOX SB-C18, 3.5 μm, 100 mm x 2.1 mm (inner diameter) or equivalent; B) mobile phase and gradient elution conditions in Table 2; Table 2 Mobile phase and gradient elution conditions table Total flow time/min Flow rate/(μL/min) Mobile phase A (5 mmol/L ammonium acetate water) /% Mobile phase B (acetonitrile) /% 0 0.00 400 99.0 1.0 1 3.00 400 70.0 30.0 2 6.00 400 60.0 40.0 3 9.00 400 60.0 40.0 4 15.00 400 40.0 60.0 5 19.00 400 1.0 99.0 6 23.00 400 1.0 99.0 7 23.01 400 99.0 1.0 C) Column temperature. 40 ° C; D) Injection volume. 10 μL; E) ion source. ESI; F) scanning method. negative ion scanning; G) Detection method. multiple reaction monitoring; H) ion spray voltage. 4000V; I) atomization gas pressure. 0.28 MPa; J) Dry gas temperature. 350 ° C; K) Dry gas flow rate. 10 L/min; L) Monitor ion pair, collision energy and source fragmentation voltage See Appendix B. 7.3.2 Qualitative determination When the sample is measured under the same experimental conditions, if the retention time of the detected chromatographic peaks is consistent with the standard sample, After the background of the sample mass spectrum, the selected ions are present, and the selected ion abundance ratio is proportional to the ion abundance ratio of the standard sample (Relative abundance > 50%, allow ± 20% deviation; relative abundance > 20% to 50%, allow ± 25% deviation; relative abundance > 10% to 20%, allow ± 30% deviation; relative abundance ≤ 10%, allow ± 50% deviation), you can determine the presence of this sample pesticide or related chemistry Goods. 7.3.3 Quantitative determination In this standard, liquid chromatography-tandem mass spectrometry was quantitatively determined by external standard-calibration curve method. To reduce the impact of matrix on quantitative determination, quantitative use The standard solution should be prepared using a standard solution of the matrix mixed standard solution. And to ensure that the measured samples of pesticides and related chemicals response value Are within the linear range of the instrument. 413 Pesticide and Related Chemical Multiple Reaction Monitoring (MRM) chromatograms, see Appendix C. 7.4 parallel test Perform the parallel test of the same specimen according to the above procedure. 7.5 blank test Unless the sample is not weighed, according to the above steps.8 results are calculated and expressedThe results of liquid chromatography-tandem mass spectrometry were quantified by standard curve method. The quantitative results of standard curve method were calculated according to formula (1) Xi = ci × (1) M 1000 Where. Xi - Residue of test component in milligrams per kilogram (mg/kg); Ci - the concentration of the solution to be measured from the standard curve, in micrograms per milliliter (μg/mL); Volume of sample solution in milliliters (mL); V - M - The weight 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 precision9.1 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 D requirements. 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 quantitative limits of this method are given in Appendix A. 10.2 Recovery rate When adding levels of L0Q, 4 × LOQ, add the recovery rate see Appendix F.Appendix A(Informative) 413 kinds of pesticides and related chemicals in English name, method of quantitative limit, grouping, solvent selection and mixed standard solution concentration table A.1413 kinds of pesticides and related chemicals in English name, method of quantitative limit, grouping, solvent selection and mixed standard solution concentration table See Table A.1. Table A.1 413 kinds of pesticides and related chemicals in English name, method of quantitative limit, grouping, solvent selection and mixed standard solution concentration table Chinese name English name The limit of quantitation/ Solvent Mixed standard Quasi solution concentration / (Mg/L) (Μg/kg) Group A 1 aniline spirit propham 220.0000 toluene 11 2 isoprocarb isoprocarb 4.6000 methanol 0.23 3 3,4,5-acylated 3,4,5-trimethacarb 0.6800 methanol 0.03 4 cycloplock cycluron 0.4200 methanol 0.02 5 Carbaryl carbaryl 20.6400 Methanol 1.03 6 Toxicant propachlor 0.5400 Methanol 0.03 7 pimidazole raenzazole 2.6600 Methanol 0.13 8 West grass net a simetryn 0.2800 Methanol 0.01 9 Green Valley Long monolinuron 7.1200 Methanol 0.36 10 times out of phosphorus mevinphos 3.1400 Toluene 0.16 11 azepine aziprotryne 2.7600 methanol 0.14 12 Micronautics Secancownet 0.1400 Methanol 0.01 13 Azathione Sulfonamide cyprodinil 1.4800 Methanol 0.07 14 Sulong Long buturon 17.9200 Methanol 0.9 15 bisacyl chloride carbetamide 7.2800 methanol 0.36 16 pirimicin pirimicarb 0.3000 methanol 0.02 Clomazone dimethazone 0.8400 methanol 0.04 18 cyanocobalt cyanazine 0.3200 methanol 0.02 19 promised net prometryne 0.3200 methanol 0.02 20 methyl paraoxon methyl 1.5200 methanol 0.08 21 thiaclapine thiacloprid 0.7400 methanol 0.04 22 imidacloprid 44.0000 Methanol 2.2 23 sulfothiazide ethidimuron 3.0000 methanol 0.15 24 Butoxalone isomethiozin 2.1400 Methanol 0.11 25 oat enemy diallate 178.4000 methanol 8.92 26 Acetochlor acetochlor 94.8000 Methanol 4.74 27 nitrilpyram 34.2400 methanol 1.71 28 methoxypropine methoprotryne 0.4800 methanol 0.02 29 xylenol amide dimethenamid 8.6000 methanol 0.43 30 terracolone terbucarb 4.2000 methanol 0.21 31 tebuconazole penconazole 4.0000 Methanol 0.2 32 myclobose myclobutanil 2.0000 methanol 0.1 33 Paclobutrazole paclobutrazol 1.1400 Methanol 0.06 34 times thiophosphor sulfoxide fenthion sulfoxide 0.6200 methanol 0.03 35 triadimenol triadimenol 21.1000 methanol 1.06 Chinese name English name The limit of quantitation/ Solvent Mixed standard Quasi solution concentration / (Mg/L) (Μg/kg) 36 Zhong Ding Ling butralin 3.8000 methanol 0.19 37 Spiroxamine 0.1% Methanol 0.01 38 Methyl Formaldehyde tolclofos methyl 133.1200 Methanol 6.66 39 beetamine desmedipham 8.0600 methanol 0.4 40 Methomethanate 21.3200 Methanol 1.07 41 Allyl alcohol allethrin 120.8000 Methanol 6.04 42 diazinon 1.4200 toluene 0.07 43 Phytophthora edifenphos 1.5000 Methanol 0.08 44 Flusilazole flusilazole 1.1600 Methanol 0.06 45 Propane Zinc iprovalicarb 4.6400 Methanol 0.23 46 wheat rust Ling benodanil 6.9600 methanol 0.35 47 fluoroamide flutolanil 2.3000 methanol 0.11 48 Sulfonamph famphur 7.2000 Methanol 0.36 49 Benzoprene Benalyxyl 2.4800 Methanol 0.12 50 benzyl chlorotriazole alcohol diclobutrazole 0.9400 methanol 0.05 51 Acetiazole etaconazole 3.5600 Methanol 0.18 52 Chlorophenoxyphenol fenarimol 1.2200 Methanol 0.06 53 Tetramethrin tetramethirn 3.6400 Methanol 0.18 54 Lactobacillus cloquintocet mexyl 3.7600 Methanol 0.19 55 Biphenyltriazole alcohol bitertanol 66.8000 Methanol 3.34 56 methyl chlorpyrifos chlorpifos methyl 32.0000 methanol 1.6 Amoxia Phosphorus azinphos ethyl 217.8600 Methanol 10.89 58 Acetyl oxalate clodinafop propargyl 4.8800 Methanol 0.24 59 Klebsuron triflumuron 7.8400 Methanol 0.39 60 isoxazolone isoxaflutole 7.8000 methanol 0.39 61 Quixi Ling quizalofop-ethyl 1.3600 Methanol 0.07 62 Fenflufenoxylate Haloxyfop-methyl 5.2800 Methanol 0.26 63 Fluorinated chlorpyrifos butyl 0.5200 Methanol 0.03 Ethyl bromothiophosphorus bromophos-ethyl 1135.3800 Methanol 56.77 65 Scavenging bensulide 68.4000 Methanol 3.42 66 bromophenylene phosphate bromfenvinfos 6.0400 methanol 0.3 67 azoxystrobin 0.9000 methanol 0.05 68 Pyridobacillus pyrazophos 3.2400 Methanol 0.16 69 Fluorfins flufenoxuron 6.3400 Methanol 0.32 70 indoxacarb 15.0800 methanol 0.75 Group B 71 ethylene thiourea ethylene tiourea 104.4000 methanol 5.22 72 Cotton Long dazomet 254.0000 Methanol 12.7 73 Nicotine nicotine 4.4000 Methanol 0.22 74 non-grass long fenuron 2.0600 methanol 0.1 75 rat death crimidine 3.1200 methanol 0.16 76 grasses molybd. 4.2000 methanol 0.21 Chinese name English name The limit of quantitation/ Solvent Mixed standard Quasi solution concentration / (Mg/L) (Μg/kg) 77-chloro-4-hydroxy-3-phenylpyridazine 6-chloro-4-hydroxy-3-phenyl-pyridazin 3.3000 methanol 0.17 78 Propoxur propoxur 48.8000 Methanol 2.44 Amoxazole isouron 0.8.200 Methanol 0.04 80 Chlorotoluron 1.2400 Methanol 0.06 81 long-potted thiofanox 314.0000 methanol 15.7 82 Chlorobenzene chlorbufam 366.0000 Methanol 18.3 83 Wicked Viola bendiocarb 6.3600 Methanol 0.32 84 Fighting prop propazine 0.6400 Methanol 0.03 85 tert-butyl terbuthylazine 0.9400 methanol 0.05 86 diuron diuron 3.1200 methanol 0.16 87 Chloromethylthiophosphate chlormephos 896.0000 Methanol 44.8 88 Moisturizer Pyorin 1.1200 Methanol 0.06 Amoxamine 6.3 90 Take the grass special pronamide 30.7600 Methanol 1.54 91 dimethachlor dimethachloro 3.8000 methanol 0.19 92 Bromoglyphine methobromuron 33.6800 Toluene 1.68 Potassium phorate 94 benzoate aclo......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 23200.11-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.11-2016_English as soon as possible, and keep you informed of the progress. 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