SNT 2325-2009进出口食品中四唑嘧磺隆、甲基苯苏呋安、醚磺隆等45种农药残留量的检测方法高效液相色谱-质谱质谱法

中华人民共和国出入境检验检疫行业标准SN/T2325—2009进出口食品中四唑嘧磺隆、甲基苯苏呋安、醚磺隆等45种农药残留量的检测方法高效液相色谱-质谱/质谱法2009-07-07发布2010-01-16实施I本标准的附录A、附录B均为资料性附录。本标准起草单位：中华人民共和国河北出入境检验检疫局、中华人民共和国天津出入境检验检1进出口食品中四唑嘧磺隆、甲基苯苏呋安、醚磺隆等45种农药残留量的检测方法高效液相色谱-质谱/质谱法3.3环己烷。3.8无水硫酸钠：经650℃灼烧4h,置于干燥器内备用。大于等于98%。2称取试样5g(精确到0.01g)于150mL具塞锥形瓶中，加入0.5g硅藻土(3.16)和15mL去离子水，浸泡20min后加入50mL丙酮，在振荡器上振荡提取30mn,抽滤至浓缩瓶中。在40℃水浴中将漏斗中，然后加入15mL氯化钠溶液(3.9),振摇萃取2min,静置分层。将二氯甲烷层经5g无水硫酸6.3.1液相色谱条件时间/min流速/(μL/min)0.1%甲酸水溶液/%0.008.003表1(续)时间/min流速/(μL/min)0.1%甲酸水溶液/%6.3.2质谱条件6.3.3液相色谱-质谱/质谱测定士50x=AXkxYx=AXkxY4表345种农药不同基质、三个水平添加回收率范围分析物大米/%大麦/%糙米/%玉米/%578.6～92.177.7～83.778.1～91.180.6～91.665.2～87.376.5～86.680.2～90.980.0～93.785.3~93.970.9~92.178.5～93.483.2～95.484.0～99.587.0～96.778.8～90.3醚磺隆585.2～97.879.4～88.784.2～95.682.2～96.873.3～90.773.5～86.184.7～95.685.7～10385.1～97.370.1～96.485,5～99.387.5～10089.8～10686.7～10276.8～95.0咪草酸587.8～94.682.8～89.588.4～93.982.6～96.880.3～94.881.6～88.885.4～93.784.0～10384.9～98.383.1~98.190.6～98.083.8～98.492.3～11387.2~99.784.1~99.3583.3～92.482.7～87.783.8～91.386.4～95.468.7～91.466.0～83.286.7～94.081.8～97.684.9～98.770.6～93.483.5～94.084.4～97.788.8～10596.2～10573.4～95.8烟嘧磺降568.8～78.268.4～77.768.1～77.366.8～83.672.7～83.468.8～76.172.9～83.164.9～81.274.4～89.771.0～89.769.5～80.572.8～87.271.4～79.575.8～89.577.0～85.9灭草喹574.9～81.368.9～77.573.2～80.473.0-87.865.6～77.469.1～84.269.8～82.669.6～87.674.9～82.671.8～84.075.9～84.072.6～86.876.1～96.479.2～97.769.4～80.3萘草胺560.1～71.460.8～71.460.8～80.460.0～79.260.3～72.863.8～80.560.1～68.360.0～72.160.3～69.763.0～72.960.5～72.560.6～78.256.8～74.960.4～72.261.3～70.7582.5～96.380.5～89.082.7～95.282.6～93.872.0～86.169.5～83.382.8～95.980.5~10088.8～97.168.8～92.882.5～97.683.8～98.688.4～10591.9～10277.9～90.3581.8～99.078.9～88.684.8～96.783.6～93.671.1～91.973.3～86.287.3～97.383.7～10084.7～96.970.3～93.982.0～10086.8～10286.5～10788.2～10377.7～90.0丙苯磺隆578.8～99.567.7～82.479.7～98.485.4～10564.2～82.460.0～69.979.3～90.976.5～97.189.3～10670.3～10179.0～10072.7～95.484.2~10490.1～10372.2～96.1甲磺草胺583.0～99.979.0～90.787.9～98.867.4～78.471.7～91.876.2～89.685.1～10485.4～10270.4～89.973.9～94.683.0～10188.1～10392.0～11075.0～84.082.9～96.95表3(续)分析物大米/%小麦/%大麦/%糙米/%玉米/%579.3～91.373.8～82.780.4～90.377.2～95.463.5～89.469.6～79.382.1～89.676.5～94.884.6～10168.9～87.379.5～92.581.3～90.183.6～99.781.5～10176.2～87.0586.7～99.076.5～86.188.2～98.081.0～97.876.1～91.674.6～89.490.3～10784.5～99.583.7～10176.7～98.288.0～10082.5～10491.5～101855～99.479.8～95.0玉嘧磺隆586.0～10673.6～87.788.2～10570.2～84.078.8～91.560.7～81.9857~10483.8～10172.7～90.371.0~96.388.5～10879.4～11090.7～10282.7～93.578.8～92.4苯磺隆565.9～98.959.7～78.570.9～87.966.4～87.466.1～93.071.0～10282.9～90.567.4～88.076.1～90.671.8～95.871.0～10075.4～95.072.6～92.570.1～92.266.0～98.6581.6～10078.8～91.584.0～99.374.4～99.064.1～87.4687～97.587.3～98.280.0～99.380.1~98,969.8~98.481.5～10286.7～10386.0～10582.9～98.177.4～93.5585.8～98.380.0～89.983.3～97.375.2～93.066.3～89.166.6～88.087.2～99.381.3～10277.7～96.374.7～10686.0～99.289.6～10485.6～99.882.5～96.180.9～101苄嘧磺隆580.2～10376.3～93.079.4～10680.6～97.077.2～93.672.0～89.084.1～97.381.8～10580.7～10475.9～97.583.4～10686.5～10290.0～10985.1～10678.2～96.8嘧啶磺隆584.4～10278.5～89.186.2～10181.2～92.866.2～92.067.3～88.590.5~99.581:9~99.980.5～98.972.3～95.684.5～10389.2～10592.1～10385.7～10382.0～92.9乙磺隆5823～97.080.2～89.585.4～96.081.8～95.071.5～87.569.1～82.589.9~99.881.1～97.682.5~98.671.2~94.982.5～98.488.8～10389.4～98.686.3～96.977.3～90.1氯嘧磺隆咪唑磺隆5824～98.976.9～86.985.6～97.876.6～93.865.9～90.673.7～89.284.2～95.184.8--10379.6~~97.073.9-~97.182.5～99.782.6～99.986.9～10080.8～10377.1～92.45754～98.681.5～94.884.2～95.878.4～96.873.7～90.867.3~82.081.6-~92.784,4～99.181.7～10064.8～90.6577.0～10085.7～10189.4～10282.7～10273.9～90.482.1～96.872.4～95.874.5～97.570.4～83.068.4～87.164.7～90.071.4~94.479.3～90.675.7～85.868.1～10682.0～99.177.9～93.380.1～10078.4～88.279.3～97.06表3(续)分析物添加水平/大米/%小麦/%大麦/%糙米/%玉米/%587.0～10176.2～89.986.1～99.468.8～98.076.5～93.870.5～89.187.0～97.681.8～10579.7～96.070.1～94.087.0～10287.6～10290.0～10272.6～99.776.4～93.5570.9～10360.4～84.882.6～10278.6～93.868.4～93.869.1～88.975.4～94.280.2～10479.2～97.169.8～96.473.7～10579.6～10288.2～10587.5～97.975.6～94.8吡嘧磺隆582.0～10274.2～87.682.2～98.066.4～90.577.3～86.886.3～98.477.0～96.084.0～10173.8～96.7-85-2～103-83.1～10391.1～10486.7～94.780.2～91.9恶草酸571.8～92.064.0～73.375.4～90.974.6～88.667.4～86.767.57.873.8～95.582.6～91.863.7～92.7~93.261.1～81.780.7～94.178.7～93.575.4～88.1580.4～119-74.2～90.285:6～10476.4～87.268.3～94.076.0～90.376.6～99.7~95.182.0～97.677.0～95.376.9～99.680.0～97.4~95.186.3～95.481.9～99.2醚苯磺隆598.5～10978.6～93.386.6～95.276.2～93.672.1～91.68295.475.8～93.282.2～10177.3～93.877.6～90.394.1~10784.7～99.2872～10180.5～94.381.8～95.9甲磺隆562.5~94.575.1～96.482.～95.874.2～85.667.1～82.368.0~83.73.-87.466.8~87.479.4～90.469.9～83.581.4～95.871.7~87.478.4～91.973.4～85.8氯磺隆5U69～83.~97.276.4～92.472.4～86.568.7～79.964.~80.780.3～97.873.1～84.467.9～91.980.7～95.668/0～84.284.5～92.276.8～91.3586.3～11275.8～94.076.0～89.275.8～94.078.2～94.381.4～f⁰177.6～96.479.8～94.181.4～96.083.8～10781.7～10682.3～99.384.0～99.085.9～101593.3～11074.9～93.888.0～10286.4～98.468.0～88.285.5～99.971.1～86.584.9～10590.8～99.674.8～88.589.7～10680.0～98.590.1～10593.2～10078.6～93.1587.1～10872.6～98.584.2～97.871.8～87.868.6～86.688.6～10170.1～88.588.0～10678.2～92.976.9～91.090.7～10781.8～97.893.3～10275.9～95.375.5～91.4烯草酮砜575.6～11167.8～87.467.8～87.467.8～86.867.8～87.465.1～89.971.8～92.664.7～83.571.2～91.874.0～95.476.5～10373.1～91.968.6～83.574.9～88.978.4～92.27表3(续)分析物添加水平/大米/%小麦/%大麦/%糙米/%玉米/%594.3～10174.7～98.284.2～96.676.6～98.063.4～81.868.9～98.169.7～86.981.8～98.180.4～97.972.0～84.490.8～10179.6～10372.6～98.184.6～10375.1～86.0氟磺隆581.3～10963.9～78.278.0～10882.8～92.460.1～79.174.9～99.075.9～95.073.8～96.385.4～97.074.6～89.278.2～10779.2～94.581.0～96.187.5～99.972.5～89.3杀鼠灵88.5～11471.8～93.890.4|-98.686.2～95.067.8～90.7280.0～92,470.9～83.290.7～10168.6～91.14-85.2～115-81,6～91.584.3~97.391.1～10181.9～94.32-甲-4-氯丙酸561.6～74.063.5～74.565.4～80.260.8～74.060.4～74.160.5-~71.361.6~~75.360.3～73.968.5～83.767~86.465.4～75.462.3～78.970.5～83.1氟嘧磺隆580.7～10160-2*=72-460-280.061.8～72.061.0～76.066.4～84.161.4--68.665.04-77.260.7~77.760.1~73.777.6～99.860.9～75.5~88.661.5～75.762.0～80.2576.8～10460.0～75.560.0～73.664.4～87.062.0～79.660.0～69.165.6～73.068.2～91.161.1～70.160.7～78.367.2～76.178.6～95.960.4～76.6氟胺磺隆583.098.360.9～82.675.-98.083.0～97.864.0～86.887.9～10068.2～86.182.9～9791.9～99.171.6～89.05738～90.270.8～92.677.6～94.866.6～88.265.~80.674.4～98.067.0～84.376.6～10580.1～9(5.270,/8～87.278.3～97.975.2～100达诺杀594.4～11480.6～98.680.8～96.861.5～88.779.2~92.(73.7～90.278.7～95.685.2～96.970.9～89.989.3～10281.1～98.083.5～97.085.9～10277.1～93.6特乐酚594.5～11470.7～90.184.8～99.077.0～93.873.6～89.171.2～87.271.3～89.575.0～89.381.6～98.075.0～86.391.2～10278.4～96.975.0～91.984.5～99.478.8～93.88j)其他质谱参数见表A.1和A.2。表A.1正离子模式组27种被测物的英文名称、CAS号、参考保留时间、监测离子对和碰撞能量药物名称英文名称CAS号保留时间/min监测离子对碰撞能量/ev氟唑嘧磺草胺Flumetsulam98967-40-96.52325.9/129.0325.9/109.0醚磺隆Cinosulfuron94593-91-69.52414.2/183.0¹414.2/157.0咪草酸Imazamethabenz-methyl81405-85-89.54289.1/143.9*289.1/220.0甲基噻吩磺隆Thifensulfuron-methy79277-27-3388.2/167.0*388.2/205.0烟嘧磺隆Nicosulfuron111991-09-4411.1/182.04411.1/213.0灭草喹Imazaquin81335-37-7312.1/267.0*312.1/180.9萘草胺Naptalam292.2/144.1*292.2/149.0甲氧磺草胺Metonsulam139528-85-1418.0/175.0*418.0/140.0氯酯磺草胺Cloransulam-methyl147150-35-4430.1/397.9a430.1/370.09药物名称英文名称CAS号保留时间/min监测离子对碰撞能量/ev丙苯磺隆Propoxycarbazone-sodium181274-15-7416.1/399.1⁸8416.1/199.0甲磺草胺Sulfentrazone122836-35-5404.0/387.0*404.0/307.0甲酰胺磺隆Foramsulfuron173159-57-4452.9/182.0*452.9/255.0甲基胺苯磺隆Ethametsulfuron-methyl97780-06-8411.2/196.1*411.2/168.0玉嘧磺隆Rimusulfuron122931-48-0432.0/182.0432.0/325.0苯磺隆Tribenuron-methyl101200-48-0396.2/155.1*396.2/181.0三氟啶磺隆Trifloxysulfuron-sodium199119-58-9438.0/182.0*438.0/139.0四唑嘧磺隆Azimsulfuron120162-55-2425.1/182.0*425.1/156.0苄嘧磺隆Bensulfuron-methyl83055-99-6411.1/149.0411.1/182.0嘧啶磺隆Flazasulfuron104040-78-0408.2/182.0*408.2/139.1乙磺隆Sulfosulfuron141776-32-1471.1/211.1*471.1/218.0氯嘧磺隆Chlorimuron-ethyl90982-32-4415.1/186.0*415.1/184.7咪唑磺隆Imazosulfuron122548-33-8413.1/153.0*413.1/156.0苯并双环酮Benzobicyclon156963-66-5446.9/257.0*446.9/229.0乙氧嘧磺隆Ethoxysulfron126801-58-9399.1/261.0°399.1/218.0环丙嘧磺隆Cyclsulfamuron136849-15-5422.1/260.9422.1/218.0吡嘧磺隆Pyrazosulfuron-ethyl93697-74-6415.2/182.1*415.2/139.1表A.1(续)药物名称英文名称CAS号保留时间/min监测离子对碰撞能量/ev恶草酸Propaquizafop444.1/100.0*444.1/371.0a为定量离子对，对于不同质谱仪器，仪器参数可能存在差异，测定前应将质谱参数优化到最佳药物名称离子对碰撞能量/ev双氟磺草胺Florasulam醚苯磺隆Triasulfuron9.82400.1/139.2°甲磺降Metsulfuron-methyl氯磺隆Chlorsulfuron五氟磺草胺Penoxsulam双氯磺草胺Diclosulam145701-21-9甲基碘磺隆烯草酮砜Clethodim-sulfone/甲磺胺磺隆Mesosulfuron-methyl氟磺隆Prosulfuron杀鼠灵Warfarin2-甲-4-氯丙酸Mecoprop氟嘧磺隆Primisulfuron-methyl氟磺胺草醚Fomesafen药物名称英文名称CAS号保留时间/min离子对碰撞能量/ev氟胺磺隆Triflusulfuron-methyl126535-15-7491.2/236.1*-17491.2/196.1-39氯吡嘧磺隆Halosulfuron-methyl100784201432.9/252.1*432.9/154.2-18-32达诺杀Dinoseb88-85-7239.1/194.1*-22239.1/193.1-26特乐酚Dinoterb1420-07-1239.1/207.1°-27239.1/177.2-34a为定量离子对，对于不同质谱仪器，仪器参数可能存在差异，测定前应将质谱参数优化到最佳。氯酯磺草胺416.1/399.1RT:10.81404.0/387.0RT:10.80404.0/307.00玉嘧磺隆苯磺降396.2/155.50396.0三氟啶磺隆50438.0/139.0/min325.9/129.0414.2/183.050-432.0/182.0289.1/143.9418.0/175.0甲基噻吩磺隆388.2/167.0咪草酸414.2/157.0312.1/267.0蒸草胺325.9/109.00RT:9.45(/min00RT:11.1050-080氮嘧磺隆氨嘧磺隆415.1/184.7咪唑磺降咪唑磺隆413.1/156.0苯并双环酮446.9/257.0446.9/229.0399.1/261.0200烯草酮砜506.1/139.2烯草酮砜506.1/139.2482.0/179.00双氯磺草胺358.0/167.1358.0/167.1502.2/267.100双氟磺草胺双氟磺草胺358.0/152.0甲基碘磺隆甲基碘磺隆000醚苯磺隆烯草酮氧0甲磺隆380.2/139.1380.2/107.2380.2/107.2404.0/153甲磷胺磺隆506.1/308.0min0t/min0886min0t/min0886氟嗜磺隆436.9/195.0432.9/154.2239.1/194.1氟嘧磺隆467.0/226.0212.9/141.12-甲-4-氯丙酸212.9/83.2氟胺磺隆氟磺隆417.9/252.0239.1/177.2417.9/139.2307.0/250.1307.0/161.1氧磺胺草醚//min0-00RT:15.64特乐酚0t/mAnnexA,AnnexBofthisstandardareaninformativeoneficationandAccreditatioChina.ChengchengandLinAnqing.firsttime.azimsulfron,bensulfron-methyl,cinosulfronetalinfoodsforimportandexport—HPLC-MS/MSmethodliquidchromatography-tandemmasssImazamethabenz-methyl,Thifensulfuron-methy,Nicosulfuron,Imazaquin,Naptalam,Metonsulam,Clo-rnsulam-methyl,Propoxycarbazone-sodium,Sulfentrazone,Foramsulfuron,Ethametsulfuron-methyl,Rimusulfuron,Tribenuron-methyl,Trifloxysulfuron-sodium,Azimsulfron,Bensulfron-methyl,Flazasul-furon,Sulfosulfuron,Chlorimuron-ethyl,Imazosulfuron,Benzobicyclon,Ethoxysulfron,Cyclsulfamu-ron,Pyrazosulfron-ethyl,Propaquizafop,Florasulam,Triasulfuron,Metsulfuron-methyl,Chlorsulfuron,Penoxsulam,Diclosulam,lodosulfuron-methyl,Clethodim-sulfone,Mesosulfuron-methyl,Prosulfuron,Warfarin,Mecoprop,Primisulfuron-methyl,Fomesafen,Triflusulfuron-methyl,Halosufuron-methyl,Di-noseb,andDinoterbinrice,brownrice,wtheat,barleytionedwithdichloromethane,andcleane3.1Methanol,HPLCgrade.3.6Dichloromethane.cool.3.915%sodiumchloridesolution:Accuratelyweigh1503.10Ethylacetate-cycloheane.3.11Methanol-warter(50+50,V/V):MixthesamevolumeMethan3.12Standardsof45pesticide(theallcoum3.14Mixedstandardsolution:Accuratehomogeneity.3.15Standardworking3.16Diatomite.cellite545.4.3MechanicalShaker.4.4Rotaryvacuumevaporator.grindertoletallpassthroughbestored0℃~4℃andkeptawayfromlight.Inthecourseofsamplepreparation,pretionsmustbetakentoavoidcontaminationoranyfactorsthatmaycausethechangeofresi-duecontent.Weigh5gofthetestsampleinto150mLconicalflask,add0.5g.cellite545(3.16)and15mLwater,andstandfor20min.Add50mLacetoneandshakefor30minwithashaker.Filtertheextractinto200mLevaporatedflaskunderreducedpressure.Concentfatethefiltratesolutionat40℃untilapprox.20mL.Transferthesolutionintoasepafatorfunnel,Washtheflaskthriceusing30mLdichloromethaneandtransfernthewashingsolutiontbthesameseparatorfunnel.Add15mLsodiumchloridesolution(3.9),thenshakeviolentlyfor2minandletstandtosepatateclearly.Filterthedichloromethanelayerthroughananhydroussodiumdulfatelayerintoaevaporatedflask.thenuse20mLdichloromethanetoliquid-lig.uidextractagainandmixthedichloromethaneintotheflask.Evaporatethedehydratedichlromethanetodrynesswithrotaryevaporatoninawater-bathbelow45E.Dissovletheresidueswith10mLcyclohex-ane-ethylacetate(3.10).ThesolutionisreadycleanupbyiGPC.a)Column:PackedwithS-X3Bio-Breads,300mm×25mm(i.d),orequivalentb)Mobilephase:Cyclohexane-ethylacetate(3.10),flowrate:5.0mL/mind)Clean-upprocedure:Thefirstfractionof0min~19minwasdiscarded;thesecondfractionof19min～30minwascollected.todrynessunderanitrogenftextohomogeneity.Afterbeingfiltratedwith0.22μa)Column:Ca150mm×2.1mm(i.d.),5μmparticlesize,orequivalent;Time/minFlowrate/(μL/min)0.1%formicacidsolution/%Methanol/%0.008.0020.020.123.0c)otherreferencemassoperatingconditionsarelistedinTableA.1andA.2ofAnnexA.Accordingtotheapproximateconcentrationofanalyteinthetestsamplesolution,selectthestand.ardworkingsolutionwith)similarresponsestothatofsamplesolution.TheresponsesoftheanalyteinjuectionsofthesamplesolutimatogramofthestandardcanbefoudinannexB.士25士30theomissionofsampleaddition.…where:X;—theresiduecontentofanalyteintestsample,μg/kg;c;—theconcentrationofanalyteinthestandardV—thefinalvolumeofthesamplesolution,mThelimitofquantificationforwarfarinis1pg/kg;theshowdinTable3.CompoundLevels/Rice/%Wheat/%Barley/%Brownrice/%Maize/%Flumetsulam578.6～92.177.7～83.778.1～91.180.6～91.665.2～87.376.5～86.680.2～90.980.0～93.785.3～93.970.9～92.178.5～93.483.2～95.484.0～99.587.0～96.778.8～90.3Cinosulfuron585.2～97.879.4～88.784.2～95.682.2～96.873.3～90.773:5~86-1-84:-7≈95:6~85:7~10385.1～97.370.1～96.485.5～99.387.5～10089.8～10686.7～10276.8～95.0Imazamethabenz-methyl587.8～94.682.8～89.588.4～93.982.6～96.880.3～94.881.6～88.884.0～10384.9～98.383.1～98.190.6～98.0,83.8～98.492.3～11387.2～99.784.1～99.3Thifensulfuron-methy583.3~92.482.7～87.783.8～91.386.4～95.468.7～91.466.0～83.286.7～94.084.9～98.770.6～93.483.5～94.084.4～97.796.2～10573.4～95.8Nicosulfuron568.8～78.268.4～77.766.8～83.672.7～83.468.8～76.172.9～83.164,9～81.274.4～89.771.0～89.775.8～89.577.0～85.9574.9～8373.0～87.865.6～77.469.1～84.269.8～82.674.9～82.671.8～84.06.4G479.2～97.769.4～80.3Naptalam560.8～80.460.0～79.260.3～72.860.3～69.763.0～72.960.5～72.560.4～72.261.3～70.7Metonsulam582.5～96.380,5～89.082.6～93.872.0～86.169.5～83.382.8～95.980.5～10088.8～97.168.8～92.882.5～97.683.8～98.688.4～10591.9～10277.9～90.3Cloransulam-methyl581.8～99.078.9～88.684.8～96.783.6～93.671.1～91.973.3～86.287.3～97.383.7～10084.7～96.970.3～93.982.0～10086.8～10286.5～10788.2～10377.7～90.0Propoxycarbazone-578.8～99.567.7～82.479.7～98.485.4～10564.2～82.460.0～69.979.3～90.976.5～97.189.3～10672.7～95.484.2～10490.1～10372.2～96.1Sulfentrazone583.0～99.979.0～90.787.9～98.867.4～78.471.7～91.876.2～89.685.1～10485.4～10270.4～89.973.9～94.683.0～10188.1～10392.0～11075.0～84.082.9～96.9Table3(continued)Levels/Wheat/%Barley/%Maize/%Foramsulfuron5Ethametsulfuron-methyl5573.6～87.7Tribenuron-methyl582.9～90:575.4～95.0Trifloxysulfuron-5Azimsulfuron5H87.2～99.3Bensulfuron-methyl572.0<89.090.0~Flazasulfuron5L101582.3～97.0Chlorimuron-55Benzobicyclon5CompoundLevels/Rice/%Wheat/%Barley/%Brownrice/%Maize/%Ethoxysulfron587.0～10176.2～89.986.1～99.468.8～98.076.5～93.870.5～89.187.0～97.681.8～10579.7～96.070.1～94.087.0～10287.6～10290.0～10272.6～99.776.4～93.5Cyclsulfamuron570.9～10360,4～84.882.6～10278.6～93.868.4～93.869.1～88.975.4～94.280.2～10479.2～97.169.8～96.473.7～10579.6～10288.2～10587.5～97.975.6～94.8Pyrazosulfuron-582.0～10274.2～87.681.1～10082.2～98.066.4～90.577.3～86.886.3～98.477.0～96.084.0～10173.8～96.785.2～10383.1～10391.1～10486.7～94.780.2～91.9Propaquizafop571.8～92.064.0～73.375.4～90.974.6～88.667.4～86.775.2～10467.5～77.873.8～95.582.6～91.863.7～92.772.5～93.261.1～81.780.7～94.178.7～93.575.4～88.1Florasulam580.4～11974.2～90.285.6～10476.4～87.268.3～94.076.0～90.376.6～99.771.2～95.182.0～97.677.0～95.376.9～99.680.0～97.475.5～95.186.3～95.481.9～99.2Triasulfuron598.5～10978.6～93.386.6～95.276.2～93.672.1～91.682.8～95.475.8～93.282.2～10177.3～93.877.6～90.394.1～10784.7～99.287.2～10180.5～94.381.8～95.9Metsulfuron-methyl562.5～94.575.1～96.482.8～95.874.2～85.667.1～82.368.0～83.073.3～87.466.8～87.479.4～90.469.9～83.564.2～83.581.4～95.871.7～87.478.4～91.973.4～85.8Chlorsulfuron568.3～85.069.7～83.984.8～97.276.4～92.472.4～86.568.7～79.973.4～87.864.7～80.780.3～97.873.1～84.467.9～91.980.7～96.668.0～84.284.5～92.276.8～91.3Penoxsulam586.3～11275.8～94.075.8～94.076.0～89.275.8～94.078.2～94.381.4～10177.6～96.479.8～94.181.4～96.083.8～10781.7～10682.3～99.384.0～99.085.9～101Diclosulam593.3～11074.9～93.888.0～10286.4～98.468.0～88.285.5～99.971.1～86.584.9～10590.8～99.674.8～88.589.7～10680.0～98.590.1～10593.2～10078.6～93.1lodosulfuron-methy!587.1～10872.6～98.584.2～97.871.8～87.868.6~86.688.6～10170.1～88.588.0～10678.2～92.976.9～91.090.7～10781.8～97.893.3～10275.9～95.375.5～91.4Clethodim-sulfone575.6～11167.8～87.467.8～87.467.8～86.867.8~87.465.1～89.971.8～92.664.7～83.571.2～91.874.0～95.476.5～10373.1～91.968.6～83.574.9～88.978.4～92.2CompoundLevels/Rice/%Wheat/%Barley/%Brownrice/%Maize/%Mesosulfuron-methyl594.3～10174.7～98.284.2～96.676.6～98.063.4～81.868.9～98.169.7~86.981.8～98.180.4～97.972.0～84.490.8～10179.6～10372.6～98.184.6～10375.1～86.0Prosulfuron581.3～10963.9～78.278.0～10882.8～92.460.1～79.174.9～99.075.9～95.073.8～96.385.4～97.074.6～89.278.2～10779.2～94.581.0～96.187.5～99.972.5～89.3Warfarin188.5～11471.8～93.890.4～98.686.2～95.067.8～90.7280.0～92.470.9～83.279.5～91.490.7～10168.6～91.1485.2～11581.6～91.584.3～97.391.1～10181.9～94.3Mecoprop561.6～74.063.5～74.565.4～80.260.8～74.060.4～74.162.9～71.560.5～71.361.6～75.360.3～73.968.5～83.760.3～72.167.7～86.465.4～75.462.3～78.970.5～83.1Primisulfuron-methyl580.7～10160.2～72.460.2～80.061.8～72.061.0～76.066.4～84.161.4～68.665.0～77.260.7～77.760.1～73.777.6～99.860.9～75.570.4～88.661.5～75.762.0～80.2Fomesafen576.8～10460.0～75.560.0～73.664.4～87.062.0～79.663.8~72.260.0~69.165.6～73.068.2～91.161.1～70.173.9～91.860.7～78.367.2～76.178.6～95.960.4～76.6Triflusulfuron-methyl583.0～98.360.9～82.675.0～98.083.0～97.864.0～86.874.0～10163.9~86.174.1～10087.9~10068.2～86.182.9～97.772.1～94.878.7～99.291.9～99.171.6～89.0Halosulfuron-methyl581.0～10873.8～90.280.4～10670.8～92.677.6～94.866.6～88.270.1～87.565.4～80.674.4～98.067.0～84.376.6～10580.1～96.270.8～87.278.3～97.975.2～100Dinoseb594.4～11474.1～93.480.6～98.680.8～96.861.5～88.779.2～92.073.7～90.278.7～95.685.2～96.970.9～89.989.3～10281.1～98.083.5～97.085.9～10277.1～93.6Dinoterb594.5～11470.7～90.184.8～99.077.0～93.873.6～89.171.2～87.271.3～89.575.0～89.381.6～98.075.0～86.391.2～10278.4～96.975.0～91.984.5～99.478.8～93.8AnnexA(Informative)a)Sheathgas:30unit;d)lonspayvoltageinESl-e)Capillarytempreture:320℃i)Colisiongaspressure:1.5nTorr,OtherA.2.TableA.—Themassbperatingconditfonsandcompoundmessageforthe27pesticidesunderESlfmodeCompoundCAS#Reientiontime/minlonpairs(m/z)Collisionenergy/Flumetsulam98967-40-96.52325.9/129.0325.9/109.0Cinosulfuron94593-91-69.52414.2/183.0⁸414.2/157.0Imazamethabenz-methyl81405-85-89.54289.1/143.9a289.1/220.01)Non-commercialstatement:thereferencemassparametersinAnnexAareaccomplishedbyThermoTSQQuantumUItraAMLC-MS/MS,th