SNT 3649-2013 饲料中氟喹诺酮类药物含量的检测方法 液相色谱-质谱质谱法

饲料中氟喹诺酮类药物含量的检测方法液相色谱-质谱/质谱法11饲料中氟喹诺酮类药物含量的检测方法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测定时间乙腈%甲醇%%123456允许的最大偏差4根据试样中被测物的含量情况，选取响应值相近的标准工作液一起进行色谱分析。标准工作液和待测液中13种氟喹诺酮类药物的响应值应在仪器线性响应范围内。对标准工作液和样液等体积参插进行测定。在上述色谱条件下13种氟喹诺酮类药物的参考保留时间见附录B.13种氟喹诺酮类药物的标准溶液的多反应监测(MRM)色谱图参见图D.1。7.3.4空白试验称取阴性样品1g(精确至0.01g),按7.1和7.2操作。8结果计算X₁——试样中13种氟喹诺酮类药物含量，单位为毫克每千克(mg/kg);c——从标准工作曲线得到的13种氟喹诺酮类药物溶液浓度，单位为微克每升(pg/L);v—样品溶液最终定容体积，单位内毫升(mL);9.1测定低限本方法的测定低限为0.5mg/kg.9.2回收率饲料中13种氟喹诺酮类药物的添加浓度及其同收率的实验数据见表3。表313种氟喹诺酮类药物的添加浓度及其回收率5表3(续)回收率/%司帕沙星奥比沙星6相关信息中文名称CAS号12345甲磺酸单诺沙星C.H₂FN,O.S678司帕沙星9DifloxacinHydrochlo7保留时间VV12345678司帕沙星9奥比沙星8(资料性附录)表C.1参考质谱参数辅助加热气温度/℃9Intensity/cpsACDIntensity/cpsACD0B1KM0sa0说明：B——环丙沙星；E———单诺沙星；H——司帕沙星；K——氟罗沙星；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