SNT 3541-2013 出口食品中多种醚类除草剂残留量检测方法 气相色谱-负化学离子源-质谱法

出口食品中多种醚类除草剂残留量检测方法气相色谱-负化学离子源-质谱法I本标准按照GB/T1.1—2009给出的规则起草。1试样经正己烷饱和过的乙腈(含1%冰醋酸)提取，分散固相萃取净化，气相色谱-负化学离子源质3.7提取溶剂(含1%冰醋酸的经正己烷饱和过的乙腈溶液):加10mL冰醋酸到990mL的(事先用(Pyraflufen-ethyl,CAS号：12963glycofen-ethyl,CAS号：77501-903.11混合标准工作液：根据需要用丙酮稀释成适当浓度的标准工作溶液，4℃下保存(有效期为1个月)。234定性离子(m/z)乙氧氟草醚除草醚吡草醚喹氧灵甲氧除草醚甲羧除草醚7.86～结束乙羧氟草醚注：标“”者为定量离子。允许的相对偏差士20%士30%5本方法各种基质的11种二苯醚类农药的测定低限均为0.01mg/kg。不同基质中添加浓度水平下的回收率范围参见表大葱79J3～92.2猪肉蜂蜜6(资料性附录)醚类除草剂标准溶液GC-MSD/NCI选择离子流色谱图图A.1醚类除草剂混合标准溶液GC-MS/NCI总离子流图7(资料性附录)待测农药的分子结构式信息B.2Lactofen乳氟禾草灵B.3aclonifen苯草醚8B.5Bifenox甲羧除草醚B.6Fluoroglycofenethyl乙羧氟草醚B.7Nitrofen除草醚B.8Ethoxyfenethyl氟乳醚9Thisstandardspecifiespreparationoftestsample,determinatiinrice,soybean,spinach,acetatefollowingbyasimplecleanuostepknownbydispersivesolid-phasewater.3.8Standards:Fluorodifen(CAS.15457-05-3),Oxyfluorfen(CAS:42874-03-3),Nitrofen(CAS:1836-75-5),Aclonifen(CAS:74070-46-5),Pyraflufen-ethyl(CA124495-18-7),Ethoxyfen-ethyl(CAS:131086-42-5),Chlometho(CAS:42576-02-3),Lactofen(CAS:77501-63-4)andFlpurities≥98.0%.3.11Mixturestandardworkingsolution:ThendiluteAbout500grepresentativesamplesshouldAbout500grepresentativesamplesshouldbetsamplehasmelted,thenprecautionsmustbetakentoavoidevaporationofwaterfromthesample.Thendividethepulpinto4℃.Thetestsamplesofspinach,welsh,capsicum,strawberry,sweetpea,redswampcrayficondensor.Evaporatetheextracttodrybyaphasefiber,andwaitforGC-MSdeterminatio6.4.1.1Column:DB-17m6.4.1.3Inlettemper6.4.1.4Interfacetemper6.4.1.5Carriergas:Hel6.4.1.10lonizationsourcetemperature:150℃;6.4.1.12Reage6.4.1.13Acquisitionmode:Selectedlo7standardworkingsolutionwithsimshouldbewithinthcordingtoqualitativeion(lonwithsymbodiphenyletherstandardsolutioomissionofsampleadditVx—thefinalvolumeofthesolution,mL;Table3(continued)%TotalionchromatogramofGC-MS/NClfor4—AclonifenFiureA.1-T