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GB 23200.14-2016 English PDF

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GB 23200.14-2016: Food safety national standard -- Determination of 512 pesticides and related chemical residues in fruit and vegetable juices and fruit wine by liquid chromatography-mass spectrometry
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GB 23200.14-2016English1479 Add to Cart 8 days [Need to translate] Food safety national standard -- Determination of 512 pesticides and related chemical residues in fruit and vegetable juices and fruit wine by liquid chromatography-mass spectrometry Valid GB 23200.14-2016

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Basic data

Standard ID GB 23200.14-2016 (GB23200.14-2016)
Description (Translated English) Food safety national standard -- Determination of 512 pesticides and related chemical residues in fruit and vegetable juices and fruit wine by liquid chromatography-mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 74,786
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) GB/T 23206-2008
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 23200.14-2016: Food safety national standard -- Determination of 512 pesticides and related chemical residues in fruit and vegetable juices and fruit wine by liquid chromatography-mass spectrometry



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Food safety national standard - Determination of 512 pesticides and related chemical residues in fruit and vegetable juices and fruit wine by liquid chromatography-mass spectrometry SecbumetonICS National Standards of People's Republic of China Replacing GB/T 23206-2008 National standards for food safety Fruit and vegetable juice and fruit wine in 512 kinds of pesticides and related Determination of chemical residues Liquid chromatography - mass spectrometry National Food Safety Standards- Determination of 512 pesticides residues in fruit juice, vegetable juice and fruit Wine Liquid 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 4 9 precision 4 10% limit and recovery rate 4 Appendix A (informative) 512 kinds of pesticides and related chemicals, English name, method of quantitative limit, grouping, solvent selection and mixing Standard solution solution Appendix B (informative) 512 kinds of pesticides and related chemicals Monitoring of ion pairs, impact gas energy, source fragmentation voltage and retention Between 17 Appendix C (Informative Appendix) 512 Pesticides and Related Chemicals Multiple Reaction Monitoring (MRM) Chromatogram 28 Appendix D (informative) Relative standard deviation in laboratory Appendix E (informative) Relative standard deviation between laboratories Appendix F (informative) Experimental data on the concentration and recovery of samples

Foreword

The standard instead of GB/T 23206-2008 "fruit and vegetable juice, fruit wine in the determination of 512 kinds of pesticides and related chemical residues liquid chromatography - Tandem mass spectrometry ". This standard compared with GB/T 23206-2008, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the standard range to increase the "other fruit and vegetable juice, wine can refer to the implementation." This standard replaced the previous version of the standard release. -GB/T 23206-2008. National standards for food safety Determination of 512 pesticides and related chemical residues in fruit and vegetable juices and Liquid chromatography - mass spectrometry

1 Scope

This standard provides orange juice, apple juice, grape juice, cabbage juice, carrot juice, dried wine, semi-dry wine, semi-liqueur, liqueur 512 Pesticide and related chemicals (see Appendix A) Residue Liquid Chromatography - Mass Spectrometry. This standard applies to orange juice, apple juice, grape juice, cabbage juice, carrot juice, dried wine, semi-dry wine, semi-liqueur, Pesticide and related chemical residues in the qualitative identification, but also for 490 kinds of pesticides and related chemical residues in the quantitative determination of other fruits and vegetables Juice, wine 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 sample was extracted with 1% acetonitrile solution, purified by Sep-Pak Vac column, eluted with acetonitrile-toluene solution (3 1) and related The samples were analyzed by liquid chromatography - tandem mass spectrometry and quantified by external 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 Acetone (CH3COCH3, 67-64-1). Chromatographic Purification. 4.1.3 Isooctane (C8H18,540-84-1). Chromatographic pure. 4.1.4 Methanol (CH3OH, 67-56-1/170082-17-4). Chromatographic Purification. 4.1.5 Toluene (C7H8, 108-88-3). Chromatographic pure. 4.1.6 acetic acid (CH3COOH, 64-19-7). excellent grade pure. 4.1.7 Formic acid (HCOOH, 64-18-6). Excellent grade pure. 4.1.8 ammonium acetate (CH3COONH4,631-61-8). excellent grade pure. 4.1.9 anhydrous sodium acetate (CH3COONa, 127-09-3). analytical grade. 4.1.10 anhydrous sodium sulfate (Na2SO4,7757-82-6), anhydrous magnesium sulfate (MgSO4, 7487-88-9). analytical grade. Before use at 650 ℃ burning Burning 4 h, stored in a dryer, cooling and standby. 4.2 solution preparation 4.2.1 0.1% formic acid solution. take 1000 mL of water, add 1 mL of formic acid, shake back standby. 4.2.2 5mmol/L ammonium acetate solution. Weigh 0.385g ammonium acetate, diluted with water to 1000mL. 4.2.3 acetonitrile - toluene solution (3 1). take 300 mL of acetonitrile, add 100 mL of toluene, shake back. 4.2.4 1% acetic acid acetonitrile solution. take 1000 mL of acetonitrile, add 1 mL of acetic acid, shake back. 4.2.5 acetonitrile - water solution (3 2). take 300 mL of acetonitrile, add.200 mL of water, 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 Respectively, weighing 5 mg ~ 10 mg (accurate to 0.1 mg) pesticides and related chemicals in the standard material in 10 mL volumetric flask, root According to the solubility of the reference substance, methanol, toluene, acetone, acetonitrile or isooctane are dissolved and fixed to the scale (see Appendix A for solvent selection) Standard solution dark 0 ℃ ~ 4 ℃ preservation, shelf life of one year. 4.4.2 Mixing standard solutions (mixed standard solutions A, B, C, D, E, F and G) According to the retention time of pesticides and related chemicals, 512 kinds of pesticides and related chemicals are divided into A, B, C, D, E, F and G And the concentration of each pesticide and associated chemical in the instrument to determine the concentration in the mixed standard solution. This standard For the classification of 512 pesticide and related chemicals and their mixed standard solution concentrations, see Appendix A. Depending on the grouping of each pesticide and associated chemical, the concentration of the standard solution and the concentration of the standard stock solution, the amount of individual Pesticide and related chemicals Standard stock solution in 100mL volumetric flask, with a fixed volume of methanol to the scale. Mixed standard solution light 0 ℃ ~ 4 ℃ Save, save for one month. 4.4.3 Substrate mixed standard working solution Pesticide and related chemical matrix mixed standard working solution is a blank sample matrix solution dubbed different concentrations of matrix mixed standard work As the solution A, B, C, D, E, F and G, for the standard working curve. Matrix mixed standard working solution should be used with the current distribution. 4.5 Materials 4.5.1 Microporous membrane (nylon). 13 mm × 0.2 μm. 4.5.2 Waters Sep-Pak Vac Ammonia Solid Phase Extraction Column. 6 mL, 1 g, or equivalent.

5 instruments and equipment

5.1 Liquid Chromatography - Tandem Mass Spectrometer. Equipped with electrospray ion source. 5.2 Analysis of balance. 0.1 mg and 0.01 g. 5.3 chicken heart bottle..200 mL. 5.4 Pipettes. 1 mL. 5.5 Vials. 2 mL, with Teflon Capping. 5.6 with a plug centrifuge tube. 50 mL. 5.7 Scroll Mixer. 5.8 Nitrogen Drying Machine. 5.9 Low speed centrifuge. 4200 r/min. 5.10 Rotary Evaporator.

6 sample preparation

Concentrate fruit and vegetable juice samples, all the original samples will be made into a clean enamel mixed barrels, stir well and mix well, then mix The goods are packed in two copies (500 mL each), sealed and marked. The samples were cryopreserved at -18 ° C.

7 Analysis steps

7.1 Extraction Weigh 15 g of sample (accurate to 0.01 g) (15 mL of wine) in a 50 mL stoppered centrifuge tube, add 15 mL of 1% acetonitrile solution, Swirl on a vortex mixer for 2 min. Add 1.5 g of anhydrous sodium acetate to the plug centrifuge tube and shake for 1 min, then add to the centrifuge tube 6g anhydrous magnesium sulfate, shaking 2min, 4200r/min centrifugal 5min, take 7.5mL supernatant to another clean tube, to be purified. Sep-Pak Vac column is the product name of Waters' products, and this information is intended to facilitate the user of this standard and does not indicate the acceptance of the product. If other equivalent products have The same effect, you can use these equivalent products. 7.2 Purification Add about 2 cm of anhydrous sodium sulfate to the Sep-Pak Vac column and place the column on the holder of the flask. Use before loading 5 mL of acetonitrile-toluene solution, the sample was quickly transferred to the purification column and the replacement was made when the liquid level reached the top of the sodium sulfate New chicken heart bottle to receive. In the solid phase extraction column with 50mL reservoir, with 25mL acetonitrile - toluene solution of pesticides and related chemicals, Was added to the heart of a chicken heart and concentrated in a water bath at 40 ° C to about 0.5 mL, dried at 35 ° C under nitrogen, and dissolved in 1 mL of acetonitrile-water Solution residue, 0.2μm microporous membrane filter for liquid chromatography - tandem mass spectrometry. 7.3 Determination 7.3.1 Liquid Chromatography - Tandem Mass Spectrometry Reference Conditions 7.3.1.1 Determination of LC-MS-MS for pesticides and related chemicals in Groups A, B, C, D, E and F A) Column. ZORBAX SB-C18, 3.5 μm, 100 mm × 2.1 mm (inner diameter) or equivalent; B) mobile phase and gradient elution conditions in Table 1; Table 1 Mobile phase and gradient elution conditions 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) ionization source mode. electrospray ionization; F) ionization source polarity. positive mode; G) atomization gas. nitrogen; H) atomization gas pressure. 0.28 MPa; I) ion spray voltage. 4000V; J) Dry gas temperature. 350 ° C; K) Dry gas flow rate. 10 L/min; L) Monitor the ion pair, the collision gas energy and the source fragmentation voltage, see Appendix B. 7.3.1.2 Determination of conditions for LC-MS-MS for pesticides and related chemicals in Group G A) Column. ZORBAX SB-C18, 3.5 μm, 100 mm × 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 Total 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) ionization source mode. electrospray ionization; F) ionization source polarity. negative mode; G) atomization gas. nitrogen; H) atomization gas pressure. 0.28 MPa; I) ion spray voltage. 4000 V; J) Dry gas temperature. 350 ° C; K) Dry gas flow rate. 10 L/min; L) Monitor the ion pair, the collision gas energy and the 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%, allowing ± 30% deviation; relative abundance ≤ 10%, allowing ± 50% deviation), you can determine the presence of this pesticide or related chemical 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. See Appendix C for the Pesticide and Related Chemicals Multi-Reaction Monitoring (MRM) chromatograms. 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 expressed

The 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); V - volume of sample solution in milliliters (mL); M - The weight of the sample represented by the sample solution, in grams (g) (the wine is mL). 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 D. 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 LOQ, 4 × LOQ, add the recovery rate see Appendix F.

Appendix A

(Informative) 512 kinds of pesticides and related chemicals, English name, method of quantitative limit, grouping, solvent and mixed standard solution concentration A.1 The names of the pesticides and related chemicals in English and Chinese, the method of quantification, grouping, solvent and mixed standard solution concentrations See Table A.1 Table A.1 The names and methods of quantification, grouping, solvent and mixed standard solution concentrations in 512 pesticides and related chemicals. Serial number Chinese name English name The limit of quantitation/ (Μg/kg) Solvent Mix the standard solution Concentration/(mg/L) Group A 1 Aniline Ling propham 36.66 Toluene 11.00 2 isoprocarb isoprocarb 0.76 methanol 0.23 3, 3, 4, 4, 3, 3, 3, 4, 5, trimethacarb 0.12 Methanol 0.03 4 ring curmitine cycluron 0.06 methanol 0.02 5 Carbaryl carbaryl 3.44 Methanol 1.03 6 Toxicant propachlor 0.10 Methanol 0.03 7 pimidazole oxenzazole 0.44 methanol 0.13 8 West grass net simetryn 0.04 methanol 0.01 9 Green Valley Long monolinuron 1.18 Methanol 0.36 10 times out of phosphorus mevinphos 0.52 toluene 0.16 11 azepine aziprotryne 0.46 methanol 0.14 12 sec. Sec. Secancourt 13 Azathione Sulfonamide cyprodinil 0.24 Methanol 0.07 14 sulton buturon 2.98 methanol 0.90 15 bisacyl chloride carbetamide 1.22 methanol 0.36 16 pirimicarum pirimicarb 0.06 methanol 0.02 17 Isosubicin clomazone 0.14 Methanol 0.04 18 cyanocobalt cyanazine 0.06 methanol 0.02 19 promised net prometryne 0.06 methanol 0.02 20% paraoxon methyl 0.26 methanol 0.08 21 4,4-dichlorobenzophenone a 4,4-dichlorobenzophenone 4.54 Methanol 1.36 22 thiacloprid thiacloprid 0.12 methanol 0.04 23 imidacloprid 7.34 Methanol 2.20 24 sulfothiazide ethidimuron 0.50 methanol 0.15 25 Butoxalone isomethiozin 0.36 Methanol 0.11 26 oat enemy diallate 29.74 methanol 8.92 27 Acetochlor acetochlor 15.80 Methanol 4.74 28 nitrilpyram 5.70 methanol 1.71 29 caustic sorbitan methoprotryne 0.08 methanol 0.02 30 xylenolide dimethenamid 1.44 methanol 0.43 31 Terracuria terrbucarb 0.70 Methanol 0.21 32 tebuconazole penconazole 0.66 methanol 0.20 33 myclobose myclobutanil 0.34 methanol 0.10 34 Paclobutrazole paclobutrazol 0.20 Methanol 0.06 35 times thiophosphor sulfoxide fenthion sulfoxide 0.10 methanol 0.03 36 triazole alcohol triadimenol 3.52 methanol 1.06 37 Zhong Ding Ling butralin 0.64 Methanol 0.19 38 Spiroxamine 0.02 Methanol 0.01 39 Methylphenol tolclofos methyl 22.18 Methanol 6.66 40 beetin desmedipham 1.34 methanol 0.40 41 Pomperide methidathion 3.56 Methanol 1.07 42 Allyl alcohol allethrin 20.14 Methanol 6.04 43 Diazinon 0.24 Toluene 0.07 44 insecticides edifenphos 0.26 methanol 0.08 45 Propoxamine pretilachlor 0.12 Methanol 0.03 Table A.1 (continued) Serial number Chinese name English name The limit of quantitation/ (Μg/kg) Solvent Mix the standard solution Concentration/(mg/L) 46 Fluorosiliconazole flusilazole 0.20 Methanol 0.06 47 Propane Zinc iprovalicarb 0.78 Methanol 0.23 48 wheat rust Ling benodanil 1.16 methanol 0.35 49 fluoroamide flutolanil 0.38 methanol 0.11 50 Frozen Phosphorus famphur 1.20 Methanol 0.36 51 Benzoprene benalaxyl 0.42 Methanol 0.12 52 benzyl chlorotriazole alcohol diclobutrazole 0.16 methanol 0.05 53 Acetazole etaconazole 0.60 Methanol 0.18 54 Chlorophenylpyrimidinol fenarimol 0.20 Methanol 0.06 55 phthalic acid phthalic acid, dicyclobexyl ester 0.66 methanol 0.20 56 Tetramethrin tetramethirn 0.60 Methanol 0.18 57 antibacterial spirit dichlofluanid 0.86 toluene 0.26 58 solution grass cloquintocet mexyl 0.62 methanol 0.19 59 Biphenyltriazole alcohol bitertanol 11.14 Methanol 3.34 60 methyl chlorpyrifos chlorprifos methyl 5.34 methanol 1.60 61 pyranosone tepraloxydim 4.06 methanol 1.22 62 methyl thiophanate methyl 13.34 methanol 2.00 Phosphorus Azinphos ethyl 36.30 Methanol 10.89 64 ethynyl oxalate clodinafop propargyl 1.62 methanol 0.24 65 Klebsuri triflumuron 1.30 Methanol 0.39 66 isoxazolone isoxaflutole 1.30 methanol 0.39 67 thiophanat ethyl 13.44 methanol 2.02 68 Quizalofop-ethyl 0.22 Methanol 0.07 69 Fiprofenamate Haloxyfop-methyl 0.88 Methanol 0.26 70 glazaprolone fluazifop butyl 0.08 methanol 0.03 71 Ethyl bromothiophosphorus bromophos-ethyl 189.24 Methanol 56.77 72 Scavenging bensulide 11.40 Methanol 3.42 73 ether benzenesulfuron triasulfuron 0.54 methanol 0.16 74 bromophenylene phosphate bromfenvinfos 1.00 methanol 0.30 75 azoxystrobin 0.16 Methanol 0.05 7 Pyridobacillus pyrazophos 0.54 Methanol 0.16 77 Fipronil flufenoxuron 1.06 Methanol 0.32 78 indoxacarb 2.52 methanol 0.75 Amino-avermectin benzene Formate Emamectin benzoate 0.10 Methanol 0.03 Group B 80 ethylene thiourea 17.40 methanol 5.22 81 Butyric acid hydrate daminozide 0.86 Methanol 0.26 82 cotton Long dazomet 42.34 methanol 12.70 83 nicotine 0.74 methanol 0.22 84 non-grass long fenuron 0.34 methanol 0.10 85 Methionine cyromazine 4.82 Methanol 0.72 86 rat death crimidine 0.52 methanol 0.16 87 Acephate Acephate 4.44 Methanol 1.33 88 grasses enemy molinate 0.70 methanol 0.21 89 carbendazim carbendazim 0.16 methanol 0.05 6-chloro-4-hydroxy-3-phenyl Pyridazine 6-chloro-4-hydroxy-3-phenyl-pyridazin 0.56 methanol 0.17 91 Propoxur 8.14 Methanol 2.44 92 isoxon isouron 0.14 methanol 0.04 93 Chlorotoluron 0.20 Methanol 0.06 94 long effect Granule thiofanox 52.34 methanol 15.70 Table A.1 (continued) Serial number Chinese name English name The limit of quantitation/ (Μg/kg) Solvent Mix the standard solution Concentration/(mg/L) 95 Chlorobenzene chlorbufam 61.00 Methanol 18.30 96 Worms bendiocarb 1.06 Methanol 0.32 97 Fighting Chin propazine 0.10 Methanol 0.03 98 tert-butyl terbuthylazine 0.16 methanol 0.05 99 diuron diuron 0.52 methanol 0.16 100 Chloromethylthiophosphate chlormephos 149.34 Methanol 44.80 101 Moisturizer Pyorin 0.18 Methanol 0.06 102 wild Yan dry difenzoquat-methyl sulfate 0.28 methanol 0.08 Benzothiazide 17.00 Methanol 6.30 104 Acetylbenzoacetate pronamide 5.12 Methanol 1.54 105 dimethamine dimethachlor 0.64 methanol 0.19 106 Bromoguron Metobromuron 5.62 Toluene 1.68 107 phorate phytate 104.66 methanol 31.40 108 benzoate aclonifen 8.06 methanol 2.42 109 dean phosphorus mephosfolan 0.78 methanol 0.23 110 Benzylimidazole imibenzonazole-des-benzyl 2.08 Methanol 0.62 111 grass less long neburon 2.36 methanol 0.71 112 Aroma cream mefenoxam 0.52 Methanol 0.15 113 thiophosphate prothoate 1.64 methanol 0.25 114 ethofume sate 124.00 methanol 37.20 115 different rice blast net iprobenfos 2.76 methanol 0.83 116 Tepu TEPP 6.94 Methanol 1.04 117 Ciproazoleazole cyproconazole 0.24 Methanol 0.07 118 thiamethoxam thiamethoxam 11.00 methanol 3.30 119 Feeding phosphorus crufomate 0.18 Methanol 0.05 120 spiramide etrimfos 12.50 methanol 1.88 121 Klebsilk coumatetralyl 0.46 Methanol 0.14 Spodophosphate cythioate 26.66 Methanol 8.00 123 phosphamine phosphamidon 1.30 methanol 0.39 124 beetin phenmedipham 1.50 methanol 0.45 125 Bentonate Bifenazate 7.60 Methanol 2.28 Carbamate fenhexamid 0.32 methanol 0.09 Albazole alcohol flutriafol 2.86 Methanol 0.86 128 antibacterial propyl alcohol furalaxyl 0.26 methanol 0.08 129 bio-allyrin bioallethrin 66.00 methanol 19.80 130 benzonitrile phospho...

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