DB34T 4335-2022 芽菜類蔬菜中喹諾酮類藥物殘留量的測(cè)定 液相色譜-質(zhì)譜 質(zhì)譜法　　

34DB34/T4335—2022芽菜類蔬菜中喹諾酮類藥物殘留量的測(cè)定液相色譜-質(zhì)譜/質(zhì)譜法DeterminationofquinolonesresiduesinsproutvegetablesbyHPLC-MS/MSmethod2022-10-26發(fā)布2022-11-26實(shí)施安徽省市場(chǎng)監(jiān)督管理局發(fā)布I2GB2763食品安全國(guó)家標(biāo)準(zhǔn)食品中農(nóng)藥樣品均質(zhì)后經(jīng)0.3％甲酸-乙腈溶液提取，提取液經(jīng)固相萃取柱凈化后，液相色譜-質(zhì)）：）：35.2.10.3%甲酸-乙腈溶液(V/V:吸取3mL甲酸(5.1.2),加乙腈(5.1.1)至1000mL,混勻。5.2.20.1%甲酸水溶液(V/V):吸取1mL甲酸(5.1.2),加水稀釋至1000mL,混勻。4精確量取1.0mL流出液，45℃水浴氮吹至干，再加入1.0mL初始流動(dòng)相復(fù)溶，過(guò)0.22μm微b)流動(dòng)相：A相為0.1％甲酸水溶液（/%/%05555f)離子源類型：電噴霧離子源（ESI）；5中待測(cè)物的質(zhì)量色譜峰保留時(shí)間的偏差在±2.5％范圍內(nèi)；所有定性離子的信噪比相對(duì)離子豐度/%>50允許相對(duì)偏差/%將基質(zhì)匹配混合標(biāo)準(zhǔn)工作溶液和試樣溶液依次注入液相色譜-質(zhì)譜/質(zhì)譜儀中，保留時(shí)間和定性離9分析結(jié)果的表述ωωi——試樣中待測(cè)物殘留量的數(shù)值，單位為微克每千克(μg/kg）；ci——由標(biāo)準(zhǔn)曲線求得試樣溶液中待測(cè)物質(zhì)量濃度的數(shù)值，單位為微克每升(μg/LV——提取液體積的數(shù)值，單位為毫升（mL）；f——稀釋倍數(shù)；6726種化合物的名稱、英文通用名、CAS號(hào)和方法12345Norfloxacin6789NalidixicacidHydroxymetronidazo8n)鞘氣流速：11L/min；其他質(zhì)譜參數(shù)見(jiàn)表B.1。122；1723456720；178920；1520；139I/10I/10I/10I/10443210I/10I/10I/10I/104432100.80.40.02.52.00.50.0 304.1/217.1 304.1/286.12.42.73.03.33.63.9I/10I/10543210t/minI/10I/105432105.諾氟沙星 320.3/302.0320.3/233.13.63.94.24.54.85.1t/minI/10I/104I/10I/1042.麻保沙星363.1/319.9363.1/344.93.03.33.63.94.24.54.8765432107654321042 6.氧氟沙星 362.1/318.1362.1/261.13.33.63.94.24.54.85.1t/minI/10I/103.依諾沙星321.1/303.1321.1/232.03.33.63.94.24.54.8543204.氟羅沙星 370.1/326.1 370.1/269.1 3.33.63.94.24.54.8t/min6543210t/min6543210 332.2/314.0332.2/230.93.64.04.44.85.2I/10I/107.培氟沙星334.2/316.2334.2/290.23.63.94.24.54.85.1t/mint/min654320 9.洛美沙星I/102.52.01.51.00.50.0 376.2/332.2376.2/261.1 5.15.45.76.06.36.6t/minII/10I/10432010.達(dá)氟沙星386.0/342.0386.0/299.05.45.76.06.36.6t/min55432105432011.恩諾沙星 4642064204.50.0400.2/382.1400.2/356.15.45.76.06.36.66.9t/min12.奧比沙星12.奧比沙星88 393.1/292.1II/104I/1040.50.0402.3/384.5402.3/357.9t/min18.吉米沙星6420391.1/360.0391.1/314.0I/I/10432020.妥蘇沙星405.0/387.0405.0/344.05.76.06.36.6t/min665432103210321021.西諾沙星 22.噁喹酸 5I/1030.50.0210t/minI/1030.50.021025.甲硝唑172.1/82.0