使用GCMSMS技术结合农药残留专用色谱柱分析检测水果和蔬

VarianVF-5Pesticides色谱柱应用本文所选数据为典型数据结果，更详细的应用，请联系当地Varian使用GC/MS/MS技术结合农药残留专用色谱柱分析检测水果和蔬菜中的多种痕量农药残留美国瓦里安公司背景介绍传统的食品中农药多残留分析检测方法一般使用气相色谱仪（GC）结合选择性检测器或者是质谱检测器来进行分析。但传统方法中所分析的农药由于法规的约束，现在已经被禁用，取而代之的是高活性、环境效应较小的现代农药。为了符合法规最大残留限量水平的要求，现代农药超低的使用量和残留量水平（ppb级），使用常规气相色谱技术已经无法满足检测要求。越来越多的化合物必须使用专门的方法来检测，因此需要过长的分析时间，从而造成人力和物力的浪费。我们利用三级四极杆串联质谱技术（GC/MS/MS或LC/MS/MS）的选择性结合最近开发出来的QuEChERS(quick-easy-cheapeffectiverobustandsafe)萃取技术，对满足UK/EU最大残留限量或低于此残留限量水平的多种农药进行分析，研究出满足现代农药残留分析要求的农药多残留分析检测方法。实验仪器和实验条件三级四极杆质谱仪：Varian1200GC/MS/MS离子化方式：正EI模式碰撞气：氩气压力为1.5mTorr碰撞能量：针对每种化合物进行优化气相色谱：VarianCP-3800进样口：Varian1079进样口80--280°C程序升温色谱柱：熔融石英毛细管色谱柱FactorFourVF-5Pesticides*30mx0.32mmx0.25μm,订货号：CP9075柱温：75°C保持2分钟；20°C/min升至150°C；3°C/min升至225°C；15°C/min升至300°C载气：氦气，流量1mL/minVarianVF-5Pesticides色谱柱应用本文所选数据为典型数据结果，更详细的应用，请联系当地Varian图1使用GC/MS/MS结合农药专用分析柱同时分析170多种农药的色谱图表一，170多种农药名称、保留时间以及定量离子序号保留时间化合物中文名称定量离子16.343Methamidophos甲胺磷94.026.444Dichlorvos敌敌畏93.038.222Biphenyl联苯128.048.568Mevinphos速灭磷/美文松127.058.706Acephate乙酰甲胺磷94.069.093Etridazole嘧硫磷211.0710.3612-phenylphenol邻苯基苯酚141.0811.208Heptenophos庚硫磷124.0911.688Omethoate氧化乐果110.01011.762Tecnazene四氯硝基苯203.01111.781Methomyl/thiodicarb灭多威88.01212.021Cymoxanil霜脲氰44.01312.011Propoxur残杀威110.01412.341Demeton-s-methyl甲基内吸磷88.01512.523Diphenylamine二苯胺167.01612.624Ethoprophos灭克磷114.01713.152Chlorpropham氯苯胺磷127.01813.47Bendiocarb恶虫威166.01913.697Monocrotophos久效磷127.02013.825Cadusafos硫线磷158.02113.985Phorate甲拌磷75.02214.269HCH-alphaα-六六六45.02314.408Hexachlorobenzene六氯苯142.02414.572Thiometon甲基乙拌磷88.02514.852Dimethoate乐果87.02614.892Dicloran氯硝胺176.0VarianVF-5Pesticides色谱柱应用本文所选数据为典型数据结果，更详细的应用，请联系当地Varian序号保留时间化合物中文名称定量离子2715.003Ethoxyquin乙氧基喹啉174.02815.143Carbofuran克百威149.02915.35AtrazineD5莠去津205.03015.562HCH-betabeta-六六六181.03115.54HCH-betabeta-六六六145.03215.596Quintozene五氯硝基苯237.03315.829Aminocarb灭害威151.03415.903Lindane(HCH-gamma)林丹181.03515.886Lindane(HCH-gamma)林丹145.03616.03Disulfoton乙拌磷97.03716.032Terbufos特丁硫磷175.03816.031Dioxathion敌杀磷97.03916.044Propetamiphos胺丙畏194.04016.411Diazinon二嗪农179.04116.666Pyrimethanil嘧霉胺198.04216.706Chlorothalonil百菌清231.04317.032Isazophos氯唑磷119.04417.269Etrimfos乙嘧硫磷181.14517.734Pirimicarb抗蚜威166.04618.439Phosphamidon磷胺27.04718.867Chlorpyrifosmethyl甲基毒死蜱93.04819.121Vinclozolin乙烯菌核利212.0,4919.168SpiroxamineI葚孢菌素I100.05019.244Parathionmethyl甲基马拉松109.05119.266Tolclofosmethyl甲基立枯磷265.05219.575Heptachlorcis顺式-七氯237.05319.585Carbaryl西维因115.05419.665Acibenzolar-s-methyl甲基苯丙噻二唑107.05519.707Metalaxyl甲霜灵132.05620.335Demeton-s-methyl-sulfone砜吸磷169.05720.519Pirimiphosmethyl甲基嘧啶磷276.05820.614SpiroxamineII孢菌素II100.05920.65Fenitrothion杀螟硫磷109.06020.962Dichlofluanid抑菌灵123.06121.204Malathion马拉松99.06221.501Chlorpyrifos毒死蜱258.06321.515Aldrin艾氏剂191.06421.889Fenpropimorph芬普福128.06521.972Parathionethyl乙基对硫磷109.06622.148Triadimefon三泰酚181.06722.376Dichlorobenzophenone4,4-二氯苯甲酮111.0VarianVF-5Pesticides色谱柱应用本文所选数据为典型数据结果，更详细的应用，请联系当地Varian序号保留时间化合物中文名称定量离子6822.83Pirimiphosethyl乙基嘧啶磷333.06923.459ChlorfenvinphosEisomer毒虫畏（Z体）异构体267.07023.512Cyprodinil嘧菌环胺224.07123.762Penconazole戊菌唑248.07223.896Tolyfluanid甲苯氟磺胺137.07324.045ChlorfenvinphosZisomer毒虫畏（E体）异构体267.07424.213Mecarbam灭牙磷131.07524.212Folpet灭菌丹76.07624.315Phenthoate稻丰散121.07724.3Meposfolan140.07824.349Quinalphos奎硫磷118.07924.467Furalaxyl呋霜灵95.08024.543Procymidone腐霉利96.08124.407Thiabendazole涕必灵174.08224.62Triadimenol三唑醇70.08324.832Captan克菌丹79.08425.119Bromophosethyl乙基溴硫磷303.08525.13Methidathion杀扑磷85.08625.223Chinomethionate灭螨孟206.08725.374DDE2.4-o，p'-DDE176.08825.59Vamidothion灭蚜硫磷87.08925.562Paclobutrazole多效唑125.09025.846Endosulfanalpha-α-硫丹143.09126.099Ditalimfos灭菌磷130.19226.236Picoxystrobin定氧菌酯115.09326.248Mepanipyrim灭派林222.09426.711Hexaconazole己唑醇214.09526.800Prothiophos丙硫磷239.09627.008Fludioxanil咯菌氰182.09727.117Profenofos丙溴磷267.09827.204Imazalil抑霉唑173.09927.306DDE4.4-p，p'-DDE246.010027.434Dieldrin狄氏剂241.010127.672DDD2.4-o，p'-DDD165.010227.659Myclobutanil腈菌唑179.010327.780Buprofezin噻嗪酮105.010427.782Flusilazole氟硅唑233.010527.901Bupirimate乙嘧酚磺氨酯273.010628.395Binapacryl乐杀螨55.010728.609CyproconazoleI烯唑醇I222.010828.591CyproconazoleII烯唑醇II222.0VarianVF-5Pesticides色谱柱应用本文所选数据为典型数据结果，更详细的应用，请联系当地Varian序号保留时间化合物中文名称定量离子10929.320Endosulfanbeta硫丹143.011029.404Fenthionsulfoxide倍硫磷亚砜125.011129.735Oxadixyl恶霜灵132.011229.776DDT4.4-p，p'-DDT165.011329.776DDD4.4-p，p'-DDD165.011429.776DDT2.4-o，p'-DDT165.011529.808Ethion乙硫磷129.011630.662Triazophos三唑磷162.011730.707Ofurace乙氧肤霜灵232.011830.911Benalaxyl苯霜灵91.011931.031Carbophenothion三硫磷199.012031.212Endosulphansulphate内硫烷硫酸盐272.012131.231PropiconazoleI丙环唑I173.012231.302Trifloxystrobin戊菌酯116.012331.395Fenhexamid环酰菌胺97.012431.448PropiconazoleII丙环唑II173.012532.016Propargite克螨特135.012632.132TetramethrinI胺菊酯I81.012732.129Resmethrin-cis顺式-卞呋菊酯143.012832.326Resmethrin-trans反式-卞呋菊酯143.012932.337Captafol敌菌丹79.013032.434Zoxamide草酰胺187.013132.897Iprodione异菌脲56.013232.856Phosmet亚胺硫磷77.013332.928EPN苯硫磷157.013432.965Bromopropylate溴满酯183.013532.966TetramethrinII胺菊酯II81.013633.079Fenoxycarb苯氧威88.013733.188Fenpropathrin甲氰菊酯181.013833.516Furathioc