安捷伦LC、LC∕MSD安全食品分析——总体解决方案PPT课件.ppt

LC,LC/MSD,安全食品分析 总体解决方案,Agilent,Technologies,安捷伦科技,化学,分析事业部,第一部分,安全食品分析,2,第一章,安全食品分析概述,3,农药的分类,目前在世界上正在使用的农药有超过750余种；,在环境和食品中的农残对人类健康造成巨大威胁,农残分析日益受到重视,4,农药残留物的分析概述,农残分析的三个过程,定性,定量,确认,常用农残分析方法,气相色谱法-,FID,ECD,FPD and NPD,薄层层析法,液相色谱法-,UV and FLD,红外光谱法,气质联用技术,是目前最有效的方法,而且灵敏度很高。,色质联用是,最有效的,农残确认方法,液质联用技术,5,样品/分析的类型,样品的制备方法,样品的净化和浓缩,分析仪器的选型,数据分析,质量控制(,quality control),结果报告,农残分析流程,05 一月 2026,6,样品和农残的类型,样品的类型,高含水量的样品,低含水量的样品,含糖量高的样品,含脂肪高的样品,环境样品,特殊样品,分析农残物的类型,含卤素的样品,有机磷化合物,氨基甲酸盐类,有机氮化合物,有机硫化合物,除虫菊酯及拟除虫菊酯,05 一月 2026,7,样品的制备方法,样品的粉碎及均质,溶剂萃取,样品量:10,g,20g,50g,or 100g,混合及,Omni-mixer,溶剂,丙酮-,US FAD,Acetonitrile,-CDFA,Ethyl acetate-Sweden,05 一月 2026,8,提取方法,可根据待测农药的性质，样本种类和实验室条件选择适当的提取方法。常用方法有以下几种,：,浸渍，漂洗法,：对附着在样本表面的农药有很好的提取效果。,振荡法,：样本+提取剂，振荡数小时，普遍采用。,匀浆，捣碎法,：样本放在匀浆杯（捣碎杯）中，加提取剂，快速匀浆几分钟。简便，快速，效果好，普遍采用。,索氏提取法,：经典提取法，也叫完全提取法，效果好，但时间过长，干扰物质较多。,消化法,：样本先消化，再用提取液提取，用于不易匀浆，不易捣碎的动物组织样本。,其他方法,：超声波提取法，吹扫蒸馏法，,SFE,等。,为提取充分，往往要经三次或多次提取。提取含水量高的样本中时,有时需加无水硫酸钠；提取含糖量高的样本中农药时，或干燥土壤中农药时，需加适量水，能提高提取效果。,9,样本的净化,将样本中待测农药与干扰杂质分离的处理步骤,液-液分配法,：通常采用极性溶剂与非极性溶剂配成溶剂对进行多次分配，使干扰杂质和待测农药分离，达到净化目的。常用的溶剂对有：乙晴-正己烷（石油醚），二甲基甲酰胺（,DMF）-,正己烷（石油醚），二甲基亚砜（,DMSO）-,正己烷（石油醚），丙酮-正己烷，丙酮-二氯甲烷（石油醚），丙酮层需加10倍的2%或4%硫酸钠或氯化钠水溶液。,吸附柱层析法,：常用的吸附剂有：弗罗里硅土，三氧化二铝（酸性，中性，碱性），硅胶，活性碳，硅燥土。,通常吸附剂在用前需经高温烘烤3小时以上活化。,70年代后期，微型柱被应用于农药残留检测工作，提高了净化效果。,10,样本的净化（续）,凝结沉淀法,：,待净化溶液中加入一定的凝结剂（如氯化铵+磷酸），能使溶液中的蛋白质，脂肪，腊质等干扰物沉淀析出，再经离心，可达到净化目的。,冷冻法,：,低温处理样本提取液，使溶液中的蛋白质，脂肪，腊质等干扰物沉淀析出，过滤除掉杂质。,其它方法,：,吹扫蒸馏法，薄层层析法，磺化法，凝胶渗透层析法，离子交换层析法，高压液谱柱净化法。,11,样品的制备方法(续),样品净化,水相分离,加,NaCl,加无水硫酸钠,冷冻或吸附,溶剂分配,所有以上的组合,净化-前或后-水相分离,反相,SPE-C18,或活性炭,05 一月 2026,12,样品的制备方法(续),样品净化,凝胶过滤色谱(,gel permeation Chromatography),SPE,pH adjustment of solvent extracts,Phosphate Buffer(2M,limit volume added),05 一月 2026,13,样品的制备方法(续),样品的浓缩,K-D,样品浓缩器,氮气蒸发器,开口烧杯(水浴),真空旋转蒸发仪,05 一月 2026,14,分析仪器的选择,GC/FPD,(6890 GC),-,适合有机磷和有机硫农残化合物,GC/ECD,(6890 GC),-,适合有机氯农残化合物,GC/NPD,(6890 GC),-,适合有机氮和有机磷化合物,GC/MSD,(5973N GC/MSD),通用的分析方法,结合,NIST98,标准谱库和农药谱库可以进行农残化合物的鉴定,高灵敏度,高选择性,HPLC-,柱后衍生用荧光检测,(1100,HPLC Series),适合氨基甲酸盐类化合物的分析,LC/MS,-,高灵敏度,高选择性的检测方法,05 一月 2026,15,食品中的有机物分析总结,挥发性,极性,亲水性的,疏水性的,挥发的,非挥发性,液相,气相,液相,气相,挥发性有机酸,醛类/酮类,乙二醇,PG,OG,DG,酚类化合物,抗氧化剂,脂肪酸,脂溶性维生素,三甘油三酯,芳香酯,多氯联苯,多环芳烃,C2/C6,烃类化合物,糖类物质的三硅氧烷衍生物,脂肪酸甲酯,食用油,聚合物,单体,醇类化合物,芳香胺,有机农药,磺胺药物,亚硝胺,磷酯类化合物,天然食品色素,黄曲霉素,黄酮类化合物,氨基酸,无机离子,糖类化合物,草甘磷,抗生素,合成食品色素,酶,环氧化合物,表面活性剂,胶,淀粉,合成代谢物,糖醇化合物,16,HP,化学工作站(局域网,LAN),单用户,多用户,分析实验室一体化,GC,和,GC/MS,分析,LC,和,LC/MS,分析,样品登录,数据处理,QA/QC,结果报告,第二章,安捷伦公司LC,LC/MSD,仪器特点,18,1100,HPLC,系列,见,HPLC,19,安捷伦公司新一代液相色谱/大气压电喷雾质谱,简单、耐用的离子源设计,直角喷雾设计减少系统污染。,优化的设计不需要调节喷雾器位置。,高温干燥气与直角喷雾器的设计可以产生更小的液滴。,ES,源与APCI源切换及清洗非常方便。,清洗被不挥发性缓冲液污染的离子源,0.5,mm毛细传输管设计：,调谐更稳定,CID质谱图重复性好,不容易阻塞及污染,500000,1000000,1500000,2000000,2.295,4.176,5.721,7.222,10.088,10.603,11.476,11.902,12.05912.462,Initial run,min,2.5,5,7.5,10,12.5,15,500000,1000000,1500000,2000000,2.342,4.278,5.888,7.359,10.301,10.812,11.710,12.066,12.268,12.624,14,hours later!,20,在离子透镜区,准分子离子与氮气发生碰撞,提高结构定性信息,产生碎片离子,适合定量分析,调节锥孔区电压,实现,CID,过程,碰撞诱导解离内源,CID,毛细管输入管,碰撞诱导,解离区,锥孔区,八极杆,透镜,四极杆质量滤过口,M,n,M,+,1,M,2,+,DETAIL,21,Turner-,kruger,透镜降低四级杆边缘效应,自动调谐液输送系统，不需要在APCI或ES调谐时手动更换调谐瓶。,加热气直接加热喷雾液滴，并不加热毛细传输管,冷,毛细传输管避免热不稳定化合物的分解,四级杆提供,SCAN,和SIM方式扫描,HED,组件提高灵敏度，且更换方便,22,和二为一的工作站界面友好，方便,质谱库检索,检索用户自己创建的质谱库,使用,NIST,程序,谱库可以包括分子结构,自动或手动检索,结合,DAD/MSD,两个谱库检索报告,23,第三章,LC，LC/MSD,在安全食品中应用的,24,LC,在安全食品中的应用,25,LC/MSD,在安全食品中的应用,26,LC/MS,联用技术的相对适用范围,分子量,分析物的极性,电喷雾(,ESI),GC/MS,大气压化学电离源(,APCI),1000,100,000,10,000,非极性,极性,农药及兽残化和物,27,用于食品/环境分析的液相检测器,检测器,灵敏度,选择性,定性能力,化合物,UV/VWD,+,-,-,类酯,UV/DAD,+,-,+,维生素,抗生素,氨基酸,农药,多环芳烃,Fluorescence,+,+,-,霉菌毒素,氨基甲酸酯,氨基酸,维生素,Electrochemical,+,+,-,维生素,离子,碳水化合物,Conductivity,+,+,-,离子,Refractive,index,-,-,-,碳水化合物类酯,LC-MS,+/-,+,+,全部,28,分析应用,食品添加剂,残留,“天然”化合物,酸类化合物,抗生素,氨基酸,抗氧化剂,霉菌毒素,酯类化合物,防腐剂,无机离子,糖,人工甜味剂,农药,维生素,香料化合物,无机离子,色素,29,检测蔬菜,水果及肉类食品中的农残,药残的一般检测方法,Created by Takino and edited by Li Ping,利用,LC/MS,技术检测食品中药残，兽残的必要性,在许多国家,食品中的农残及药残的种类和数量快速增加,此外,近来法规要求的农残的性质趋向高极性和热不稳定,要求方法可以同时检测多种残留,以用于快速检测,固定方法可以建立用于谱库检索的数椐库,Created by Takino and edited by Li Ping,建议分析条件,1.,柱子,:,Zorbax Eclips,XDB C18(150mm,2.1mm,5m),2.,流动相,:,A:ACN B:10-30mMCH,3,COONH,4,0.1-0.2%CH,3,COOH,HCOOH,5mM,二,丁基胺醋酸盐,3.,柱温,:40,4.,离子源,:,电喷雾,(,ESI),5.,碎片碰撞电压,:100,or 200V,6.,毛细管电压,:4000,V,7.,干燥气（,Drying gas,）,:10l/min 350,8.,雾化气（,Nebulizer,gas,）,:50psi,Created by Takino and edited by Li Ping,建立用于谱库检索的数椐库,1.,采用多种残留检测的通用方法,2.,碎片碰撞电压为,100,和,200,V,3.,浓度是,10,ppm,(,浓度的高低不会影响质谱图,),Created by Takino and edited by Li Ping,目标化和物,(,农药,),Created by Takino and edited by Li Ping,目标化和物,(,兽药残留,),Created by Takino and edited by Li Ping,色谱,液相,:,HP-1100,柱子,:,Zorbax,Eclips,XDB C18(150mm,2.1mm,5um),流动相,:,A:,MeCN,B:10mMCH,3,COONH,4,20%A/B-(30min)-100%A,柱温,:40,C,进样体积,:10,ul,流速,:0.2,ml/min,质谱,质谱,:,HP1100MSD SL,离子源,:,ESI(Positive),扫描范围,:,m/z 100-500,干燥气,:10,l/min at 350C,雾化气,:50,psi,碎片碰撞电压,:100,V,EM,gai,n :3,氨基甲酸盐类化和物的分析条件,Created by Takino and edited by Li Ping,36,1.,Oxamyl,2.,Methiocarbsulfoxide,3.,Methiocarbsulfone,4.,Aldicarb,5.,Bendiocarb,6.,Pirimicarb,7.,Carbaryl,8.,Ethiofencarb,9.,Fenobcarb,10.,Methiocarb,min,5,10,15,20,25,0,50000,100000,150000,200000,250000,300000,350000,1,2,3,4,5,6,7,8,9,10,氨基甲酸盐标样的总离子流图,(1,ppm,),1.,杀线威,2.,甲硫威亚砜,3.,甲硫威砜,4.,涕灭威,5苯恶威,6.,抗蚜威,7.,甲奈威,8.,乙硫甲威,9.,仲丁威,10.,甲硫威,Created by Takino and edited by Li Ping,37,氨基甲酸盐标样的质谱图,(1,ppm,),100000,100,150,200,250,0,50000,237(,M+H),+,100,150,200,250,0,50000,242(,M+H),+,m/z,100,150,200,250,0,10000,20000,275(,M+NH,4,),+,1.,Oxamyl,2.,Methiocarbsulfoxide,3.,Methiocarbsulfone,100,150,200,250,0,25000,50000,116,100,150,200,250,0,100000,224(,M+H),+,167,m/z,100,150,200,250,0,100000,200000,239(,M+H),+,213(,M+Na),+,4.,Aldicarb,5.,Bendiocarb,6.,Pirimicarb,杀线威,甲硫威亚砜,甲硫威砜,涕灭威,苯恶威,抗蚜威,Created by Takino and edited by Li Ping,38,氨基甲酸盐标样的质谱图,(1,ppm,),100,150,200,250,0,25000,50000,202(,M+H),+,145,219(,M+NH,4,),+,100,150,200,250,0,50000,100000,226(,M+H),+,107,164,m/z,100,150,200,250,0,50000,100000,10:226(,M+H),+,9:208(,M+H),+,169,243(,M+NH,4,),+,7.,Carbaryl,8.,Ethiofencarb,9.,Fenobcarb,10.,Methiocarb,甲奈威,乙硫甲威,9.,仲丁威,10.,甲硫威,Created by Takino and edited by Li Ping,39,对,1,ppm,的添加样品的药残分析的谱库检索结果,=,Injection Date :2001/01/24 11:59:17 AM,Sample Name :100,ppm fia,Location:Vial 1,Acq,.Instrument:Instrument 1,Inj,Volume:5,l,Acq,.Method :C:HPCHEM1METHODSCARBA.M,Analysis Method:C:HPCHEM1METHODSANY1_POS.M,=,NIST MS library search mode:Automatic library search,NIST MS library file name:,foodpest,RetTime Sig,MW Library Match Formula Name,min#Id,-|-|-|-|-|-|-|-,3.289 1 219 1 1 915 C7H13N3O3S,Oxyamyl,(pos,100V),5.302 1 241 1 3 901 C11H15NO3S,Methiocarbsulfoxide,(pos,100v),11.464 1 257 1 5 922 C11H15NO4S,Methiocarbsulfon,(pos,100),14.140 1 190 1 7 903 C7H14N2O2S,Aldicarb,(pos,100v),23.715 1 223 1 9 961 C11H13NO4,Bendiocarb,(pos,100v),26.156 1 238 1 11 970 C11H18N4O2,Pirimicarb,(pos,100v),27.508 1 201 1 13 832 C12H11NO2,Carbaryl,(pos,100v),29.617 1 225 1 101 929 C11H15NO2S,Ethiofencarb,(pos,100v),43.461 1 225 1 17 934 C11H15NO2S,Methiocarb,(pos,100v),43.687 1 207 1 19 757 C12H17NO2,Fenobucarb,(pos,100v),=,Created by Takino and edited by Li Ping,40,氨基甲酸盐标样,(1,ppb),的选择离子模式的谱图,5,10,15,20,25,0,200,400,600,800,5,10,15,20,25,0,200,400,600,800,1000,1200,min,5,10,15,20,25,0,100,200,300,400,500,600,1.,Oxamyl,2.,Methiocarbsulfoxide,3.,Methiocarbsulfone,m/z=237,m/z=242,m/z=275,5,10,15,20,25,0,500,1000,1500,2000,25000,5,10,15,20,25,0,500,1000,1500,2000,min,5,10,15,20,25,0,500,1500,2500,3500,4.,Aldicarb,5.,Bendiocarb,6.,Pirimicarb,m/z=239,m/z=224,m/z=116,杀线威,甲硫威亚砜,甲硫威砜,涕灭威,苯恶威,抗蚜威,Created by Takino and edited by Li Ping,41,氨基甲酸盐标样,(1,ppb),的选择离子模式的谱图,5,10,15,20,25,0,400,800,1200,5,10,15,20,25,0,500,1000,1500,2000,min,5,10,15,20,25,0,400,800,1200,7.,Carbaryl,8.,Ethiofencarb,9.,Fenobcarb,10.,Methiocarb,m/z=116,m/z=208,m/z=226,甲奈威,乙硫甲威,仲丁威,甲硫威,Created by Takino and edited by Li Ping,42,Chromatogram,HPLC :HP-1100 SL,Column :,Zorbax,Eclips,XDB C18(150mm,2.1mm,5um),Mobile,pahse,:A:,MeCN,B:15mMCH3COONH4+0.05%CH,3,COOH,30%A/B-(30min)-100%A/B,Flow rate :0.2ml/min,Columnn,temp :40C,Sample volume :10ul,MS,MS :HP1100MSD,Ionization :ESI(Positive),Pentoxazone,(Negative),Scan range :m/z 100-900,SIM ion :base peak,Drying gas :10,l/min at 350C,Nebulizer,gas :50psi,Fragmentor,:100v,EM gain :3,食品中7种必检的农药残留的分析条件,Created by Takino and edited by Li Ping,食品中7种必检的农药残留的总离子流图（,1,ppm,),1.,Azimsulfuron,2.,Flazasulfron,3.,Dimethomorph,4.,Cyclosulfamuron,5.,Quizalfop,-ethyl,6.,Pentoxazone,7.,Emamectin,5,10,15,20,25,0,50000,100000,150000,200000,min,5,10,15,20,25,60000,65000,70000,75000,80000,1,2,3,4,5,6,7,这些化合物必须用液质联用确认,C,13,H,16,N,10,O,5,S,C,13,H,12,F,3,N,5,O,5,S,C,21,H,22,ClNO,4,C,17,H,19,N,5,O,6,S,C,17,H,13,ClN,2,O,4,C,17,H,17,ClFNO,4,C,49,H,75,NO,13,+C,48,H,73,NO,13,杀虫剂,Created by Takino and edited by Li Ping,44,463(,M+K),+,100,150,200,250,300,350,400,450,0,447(,M+Na),+,425(,M+H),+,100,150,200,250,300,350,400,450,0,10000,408(,M+H),+,430(,M+Na),+,100,150,200,250,300,350,400,450,0,20000,388(,M+H),+,410(,M+Na),+,426(,M+K),+,m/z,100,150,200,250,300,350,400,450,0,20000,422(,M+H),+,444(,M+Na),+,460(,M+K),+,20000,1.,Azimsulfuron,2.,Flazasulfron,3.,Dimethomorph,4.,Cyclosulfamuron,食品中7种必检的农药残留的总离子流图（,1,ppm,),C,13,H,16,N,10,O,5,S,C,13,H,12,F,3,N,5,O,5,S,C,21,H,22,ClNO,4,C,17,H,19,N,5,O,6,S,Created by Takino and edited by Li Ping,45,100,200,300,400,500,600,700,800,900,20000,40000,60000,373(,M+H),+,395(,M+Na),+,411(,M+K),+,100,200,300,400,500,600,700,800,900,2000,4000,6000,301.2,352(,M-H),-,141m/z,100,200,300,400,500,600,700,800,900,25000,50000,886(,M+H),+,590.4,546.3,502.4,634.4,5.,Quizalfop,-ethyl,6.,Pentoxazone,7.,Emamectin,食品中7种必检的农药残留的总离子流图（,1,ppm,),C,17,H,13,ClN,2,O,4,C,17,H,17,ClFNO,4,C,49,H,75,NO,13,+C,48,H,73,NO,13,Created by Takino and edited by Li Ping,46,5,10,15,20,25,0,100,300,500,5,10,15,20,25,0,100,300,500,5,10,15,20,25,0,400,800,min,5,10,15,20,25,0,200,600,1000,1.,Azimsulfuron,2.,Flazasulfron,3.,Dimethomorph,4.,Cyclosulfamuron,m/z=425,m/z=408,m/z=388,m/z=422,食品中7种必检的农药残留的选择离子流图（0.,1,ppb),Created by Takino and edited by Li Ping,47,5,10,15,20,25,0,50,150,250,350,5,10,15,20,25,0,1000,3000,5000,min,5,10,15,20,25,600,1000,1400,5.,Emamectin,6.,Quizalfop,-ethyl(1ppb),7.,Pentoxazone,(20ppb),m/z=886,m/z=373,m/z=354,食品中7种必检的农药残留的选择离子流图（0.,1,ppb),Created by Takino and edited by Li Ping,48,Chromatogram,HPLC :HP-1100 SL,Column :,Zorbax,Eclips,XDB C18(150mm,2.1mm,5um),Mobile,pahse,:A:,MeCN,B:30mMCH3COONH4,20%A/B-(30min)-100%A/B,Flow rate :0.2ml/min,Columnn,temp :40C,Sample volume :7ul,MS,MS :HP1100MSD,Ionization :ESI(Positive,Negative),Scan range :m/z 100-600,SIM ion :base peak,Drying gas :10l/min at 350C,Nebulizer,gas :50psi,Fragmentor,:100v,EM gain :5,食品中7种农药残留的分析条件Created by Takino and edited by Li Ping,食品中7种农药残留的总离子流图（,1,ppm,),0,5,10,15,20,25,0,100000,200000,300000,400000,500000,600000,1,2,3,4,min,0,5,10,15,20,25,0,100000,200000,300000,400000,500000,600000,5,6,7,1.,Chrorimuron,-ethyl,2.,Mepanipyrim,metabolite,3.,Mepanipyrim,4.,Ethobenzanid,5.,hexaflumuron,6Fulfenoxuron,7.,Hexathizox,Created by Takino and edited by Li Ping,50,食品中7种农药残留的质谱图（,1,ppm,),100,150,200,250,300,350,400,450,5000,10000,15000,415(,M+H),+,100,150,200,250,300,350,400,450,100000,200000,100,150,200,250,300,350,400,450,200000,400000,244(,M+H),+,224(,M+H),+,m/z,100,150,200,250,300,350,400,450,10000,20000,30000,40000,340(,M+H),+,m/z,100,150,200,250,300,350,400,450,40000,80000,120000,459(,M-H),-,439,1.,Chlorimuron,-ethyl,2.,Mepanipyrim,metabolite,3.,Mepanipyrim,4.,Ethobenzanid,5.,hexaflumuron,m/z,氯嘧磺隆乙酯,Created by Takino and edited by Li Ping,51,食品中7种农药残留的质谱图（,1,ppm,),100,150,200,250,300,350,400,450,20000,40000,60000,80000,487(,M-H),-,m/z,100,150,200,250,300,350,400,450,5000,10000,15000,353(,M+H),+,6.,Fl,u,fenoxuron,7.,Hexythiazox,C,17,H,21,ClN,2,O,2,S,噻螨酮,C,21,H,11,ClF,6,N,2,O,3,Created by Takino and edited by Li Ping,52,食品中7种农药残留的选择离子流图（,1,ppm,),0,5,10,15,20,25,500,1000,1500,2000,min,0,5,10,15,20,25,5000,10000,15000,20000,0,5,10,15,20,25,2000,4000,6000,8000,10000,12000,min,0,5,10,15,20,25,500,1500,2500,3500,4500,1.,Chrorimuron,-ethyl(0.2ppb),2.,Mepanipyrim,metabolite(0.2ppb),3.,Mepanipyrim,(0.2ppb),4.,Ethobenzanid,(1ppb),m/z=415,m/z=244,m/z=224,m/z=340,Created by Takino and edited by Li Ping,53,食品中7种农药残留的选择离子流图（,1,ppm,),0,5,10,15,20,25,1000,2000,3000,4000,min,0,5,10,15,20,25,500,1000,1500,2000,2500,min,0,5,10,15,20,25,2000,4000,6000,8000,10000,5.,hexaflumuron,(1ppb),6.,Fulfenoxuron,(1ppb),7.,Hexathizox,(5ppb),m/z=459,m/z=487,m/z=353,Created by Takino and edited by Li Ping,54,0,5,10,15,20,25,500,1500,2500,3500,min,0,5,10,15,20,25,20000,40000,60000,80000,100000,0,5,10,15,20,25,20000,40000,60000,80000,100000,min,0,5,10,15,20,25,2000,4000,6000,8000,花茎甘蓝萃取物中添加农残物(,10,ppb),的选择离子流图,1.,Chrorimuron,-ethyl,2.,Mepanipyrim,metabolite,3.,Mepanipyrim,4.,Ethobenzanid,m/z415,m/z=244,m/z=224,m/z=340,Created by Takino and edited by Li Ping,55,0,5,10,15,20,25,5000,10000,15000,20000,min,0,5,10,15,20,25,2000,4000,6000,8000,min,0,5,10,15,20,25,100000,200000,300000,400000,500000,600000,700000,5.,hexaflumuron,6.,Fulfenoxuron,7.,Hexathizox,m459,m/z=487,m/z=353,花茎甘蓝萃取物中添加农残物10,ppb),的选择离子流图,Created by Takino and edited by Li Ping,56,Chromatogram,HPLC :HP-1100,Column :,Zorbax Eclips,XDB C18(150mm,2.1mm,5m),Mobile,pahse,:A:,MeCN,B:10%CH,3,COONH,4,20%A/B-(30min)-100%A/B/7min,Flow rate :0.2ml/min,Columnn,temp :40C,Sample volume :10ul,MS,MS :HP1100MSD SL,Ionization :ESI(Positive/Negative),Scan range :m/z 100-600,SIM ion :base peak,Drying gas :10l/min at 350C,Nebulizer,gas :50psi,Fragmentor,:100V/200V,EM gain :5,9种农药残留的分析条件,Created by Takino and edited by Li Ping,9种农药残留的总离子流图（,1,ppm,),5,10,15,20,25,30,0,200000,400000,600000,800000,min,5,10,15,20,25,30,0,100000,200000,300000,400000,500000,1.,Quinclorac,2.,Sethoxydim,3.,Iprodione,4.,Tebufenozide,5.,Ethoxyquin,6.,Pencycuron,7.,Fenproxymate,8.,Etofenprox,9.,Silafluofen,1,2,3,4,5,6,7,8,9,2,3,4,6,9,Created by Takino and edited by Li Ping,9种农药残留的质谱图（,1,ppm,正离子模式,),100,200,300,400,0,20000,40000,242(,M+H),+,m/z,100,200,300,400,0,100000,200000,328(,M+H),+,100,200,300,400,0,2000,4000,6000,8000,352(,M+Na),+,330(,M+H),+,m/z,100,200,300,400,0,100000,200000,300000,400000,500000,297(,M+H),+,353,1.,Quinclorac,2.,Sethoxydim,3.,Iprodione,4.,Tebufenozide,二氯喹啉酸,异菌脲,稀禾定,一种新杀虫剂,Created by Takino and edited by Li Ping,9种农药残留的质谱图（1,ppm,正离子模式,),100,150,200,250,300,350,400,0,100000,200000,300000,218(,M+H),+,m/z,100,150,200,250,300,350,400,0,100000,200000,300000,400000,329(,M+H),+,100,150,200,250,300,350,400,450,0,200000,400000,600000,422(,M+H),+,m/z,100,150,200,250,300,350,400,450,0,100000,200000,394(,M+H),+,5.,Ethoxyquin,6.,Pencycuron,7.,Fenproxymate,8.,Etofenprox,乙氧三甲喹啉,杀螨酯,禾穗宁,唑螨酯,Created by Takino and edited by Li Ping,9种农药残留的质谱图（,1,ppm,正离子模式,),m/z,100,150,200,250,300,350,400,450,500,0,1000,2000,3000,4000,287(,M+H),+,9.,Silafluofen,Created by Takino and edited by Li Ping,9种农药残留的质谱图（,1,ppm,负离子模式,),100,150,200,250,300350,0,20000,40000,60000,80000,326(,M-H),-,119,163,m/z,100,150,200,250,300,350,0,5000,10000,243,150,200,250,300,350,0,100000,200000,300000,351(,M-H),-,m/z,150,200,250,300,350,0,50000,100000,150000,327(,M-H),-,2.,Sethoxydim,3.,Iprodione,6.,Pencycuron,4.,Tebufenozide,Created by Takino and edited by Li