SNT 3649-2013 飼料中氟喹諾酮類藥物含量的檢測(cè)方法 液相色譜-質(zhì)譜質(zhì)譜法

飼料中氟喹諾酮類藥物含量的檢測(cè)方法液相色譜-質(zhì)譜/質(zhì)譜法11飼料中氟喹諾酮類藥物含量的檢測(cè)方法5.525%氨水。25.11定容液：乙腈+甲醇+5mmol/L甲酸溶液(2+20+78)。量取2mL乙腈(5.1)、20mL甲醇37.3測(cè)定時(shí)間乙腈%甲醇%%123456允許的最大偏差4根據(jù)試樣中被測(cè)物的含量情況，選取響應(yīng)值相近的標(biāo)準(zhǔn)工作液一起進(jìn)行色譜分析。標(biāo)準(zhǔn)工作液和待測(cè)液中13種氟喹諾酮類藥物的響應(yīng)值應(yīng)在儀器線性響應(yīng)范圍內(nèi)。對(duì)標(biāo)準(zhǔn)工作液和樣液等體積參插進(jìn)行測(cè)定。在上述色譜條件下13種氟喹諾酮類藥物的參考保留時(shí)間見(jiàn)附錄B.13種氟喹諾酮類藥物的標(biāo)準(zhǔn)溶液的多反應(yīng)監(jiān)測(cè)(MRM)色譜圖參見(jiàn)圖D.1。7.3.4空白試驗(yàn)稱取陰性樣品1g(精確至0.01g),按7.1和7.2操作。8結(jié)果計(jì)算X?——試樣中13種氟喹諾酮類藥物含量，單位為毫克每千克(mg/kg);c——從標(biāo)準(zhǔn)工作曲線得到的13種氟喹諾酮類藥物溶液濃度，單位為微克每升(pg/L);v—樣品溶液最終定容體積，單位內(nèi)毫升(mL);9.1測(cè)定低限本方法的測(cè)定低限為0.5mg/kg.9.2回收率飼料中13種氟喹諾酮類藥物的添加濃度及其同收率的實(shí)驗(yàn)數(shù)據(jù)見(jiàn)表3。表313種氟喹諾酮類藥物的添加濃度及其回收率5表3(續(xù))回收率/%司帕沙星奧比沙星6相關(guān)信息中文名稱CAS號(hào)12345甲磺酸單諾沙星C.H?FN,O.S678司帕沙星9DifloxacinHydrochlo7保留時(shí)間VV12345678司帕沙星9奧比沙星8(資料性附錄)表C.1參考質(zhì)譜參數(shù)輔助加熱氣溫度/℃9Intensity/cpsACDIntensity/cpsACD0B1KM0sa0說(shuō)明：B——環(huán)丙沙星；E———單諾沙星；H——司帕沙星；K——氟羅沙星；ThisstandardspecifiesthemethodofdetermNorfloxacin,Ofloxacin,Danofloxacin,Marbofloxacin,Sarafloxacin,Sparfloxacin,Difloxcin,Fleroxacin,LomefloxacinandEnoxacininfeefloxacin,Marbofloxacin,Sarafloxacin,Sparfloxacin,Diftle.CertainmeasuresshallbetakentopreventcontaminationofthesamplesordecompositionoftheUnlessspecified,allreagen5.525%Ammonium5.70.1mol/LHydrochloric5.9Ammoniamethanol(1+5.11Thecapacityofliquid:AcetonitrHlemothanol55.13Standardstocksolution:1000mg/LAccuratelyweighthesuitableamountoffluorofloxacinfirstdissolvesinsomewateran5.14Standardstocksolution:50mg/L.Pipettethesuitableam0℃~4℃,andkeptawayfromlightingbrownglassvolumetricflaskandmixwell.ThesolutionshallbestoredatthetemperatureO℃~(5.11)(theformulafeedandtheconcentratb)Columntemperatu%%%123456c)Monitormode:Mtimizetheflowrateofeachgastoreac7.3.3.1QualitativedThequalitativeionsforeachanalystincludshallcorrespondtothatofthecalibrationsolutionatathedetectedionsofeachanalyte,shallcorrespondtAccordingtotheapproximateconcentrationofanalyteinsamplesolutionthestandardworkingsolutionandthesamplesolutionshallbewithinthelinearrangeoftheinmentdetection.Thestandardworkingsolutionsandthesamplesolutionshallbeinjectedwvolumealternatively.UndertheaboveLC-MS/MSoperatingconditifluoroquinolonesarelistedintable2.MultX,—theresidueoffluoroquinolongsintestsamplec,-theconcentrationoffluo