SNT 3541-2013 出口食品中多種醚類(lèi)除草劑殘留量檢測(cè)方法 氣相色譜-負(fù)化學(xué)離子源-質(zhì)譜法

出口食品中多種醚類(lèi)除草劑殘留量檢測(cè)方法氣相色譜-負(fù)化學(xué)離子源-質(zhì)譜法I本標(biāo)準(zhǔn)按照GB/T1.1—2009給出的規(guī)則起草。1試樣經(jīng)正己烷飽和過(guò)的乙腈(含1%冰醋酸)提取，分散固相萃取凈化，氣相色譜-負(fù)化學(xué)離子源質(zhì)3.7提取溶劑(含1%冰醋酸的經(jīng)正己烷飽和過(guò)的乙腈溶液):加10mL冰醋酸到990mL的(事先用(Pyraflufen-ethyl,CAS號(hào)：12963glycofen-ethyl,CAS號(hào)：77501-903.11混合標(biāo)準(zhǔn)工作液：根據(jù)需要用丙酮稀釋成適當(dāng)濃度的標(biāo)準(zhǔn)工作溶液，4℃下保存(有效期為1個(gè)月)。234定性離子(m/z)乙氧氟草醚除草醚吡草醚喹氧靈甲氧除草醚甲羧除草醚7.86～結(jié)束乙羧氟草醚注：標(biāo)“”者為定量離子。允許的相對(duì)偏差士20%士30%5本方法各種基質(zhì)的11種二苯醚類(lèi)農(nóng)藥的測(cè)定低限均為0.01mg/kg。不同基質(zhì)中添加濃度水平下的回收率范圍參見(jiàn)表大蔥79J3～92.2豬肉蜂蜜6(資料性附錄)醚類(lèi)除草劑標(biāo)準(zhǔn)溶液GC-MSD/NCI選擇離子流色譜圖圖A.1醚類(lèi)除草劑混合標(biāo)準(zhǔn)溶液GC-MS/NCI總離子流圖7(資料性附錄)待測(cè)農(nóng)藥的分子結(jié)構(gòu)式信息B.2Lactofen乳氟禾草靈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