DB37T 3474-2018土壤中12種有機磷農(nóng)藥及代謝物殘留量的測定液相色譜-質(zhì)譜質(zhì)譜法

DB37DB37/T3474—2018土壤中12種有機磷農(nóng)藥及代謝物殘留量的測定液相色譜-質(zhì)譜/質(zhì)譜法Determinationof12organophosphorouspesticidesandmetabolitesresiduesinsoilLiquidchromatography-massspectrometry2018-12-29發(fā)布2019-01-29實施山東省市場監(jiān)督管理局發(fā)布I1土壤中12種有機磷農(nóng)藥及代謝物殘留量的測定液相色譜-質(zhì)譜/質(zhì)譜法0.02%甲酸水溶液（含5mmol/L乙酸銨）：準(zhǔn)確移取0.2mL甲酸和稱取0.385g乙酸銨于1000mL2分別準(zhǔn)確稱取適量（精確至0.1mg）12種有機磷農(nóng)藥及代謝物標(biāo)準(zhǔn)品于10mL容量瓶中，準(zhǔn)確吸取適量中間標(biāo)準(zhǔn)溶液（4.4.2用甲醇稀釋配制成所需濃度的混合標(biāo)準(zhǔn)工作溶液，現(xiàn)配現(xiàn)4.5.2分散固相萃取凈化管（DispersiveSPE15mL，Rruitsand取土壤樣品約500g，除去土壤中的碎石、雜草和植物根莖等雜物后，3），移取約7mL上層提取液至分散固相萃取凈化管（4.5.2）中，在旋中以4500r/min離心3min。準(zhǔn)確移取4.055范圍以內(nèi)。對混合基質(zhì)標(biāo)準(zhǔn)溶液和樣液等體積參插進(jìn)樣測定。12種有機磷農(nóng)藥及代謝物多反應(yīng)監(jiān)測4S——標(biāo)準(zhǔn)溶液質(zhì)量濃度，單位為毫克每升（mg/L）；）；）；）；V4——待測液進(jìn)樣體積，單位為微升(μL）；V5——標(biāo)準(zhǔn)溶液進(jìn)樣體積，單位為微升(μL）；）；9.1在重復(fù)性條件下，兩次獨立測定結(jié)果的絕對差不大于重復(fù)性限（r重復(fù)性限（r）的9.2在再現(xiàn)性條件下，兩次獨立測定結(jié)果的絕對差不大于再現(xiàn)性限（R再現(xiàn)性限（R）的56123456789794125.10.00125.0094125.10.00125.00.00Inten.1001009080706050403020090100110120m/zInten.10010090807060504030200120130140m/zInten.10010090807060504030200150160170180m/z89080706050403020009080706050403020000100.0125.015908070605040302010960807060504030201059.153.107129.10100.153.107129.101009080706050403020100119Inten..15100.0125.0150.0175.0m/zInten.10010090807060504030200150160170m/zInten.1001009080706050403020075.0100.0125.0m/z75.80345.0010090807075.80345.001009080706050403020100100.0125.0150.0175.0m/z96.95.90..90807060504030200Inten..1009080706050403020100300.0