基于通过型固相萃取-高效液相色谱-串联质谱法同时测定水产品中的氯霉素和红霉素

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1、基于通过型固相萃取-高效液相色谱-串联质谱法同时测定水产品中的氯霉素和红霉素柯庆青李诗言周凡郑重莺贝亦江王鼎南王扬浙江省水产质量检测中心建立通过型固和萃取-高效液和色谱-串联质谱同时快速测定水产品中氯霉素和红霉素的分析方法。样品通过乙腈提取，OasisPRiMEHLB小柱一步法净化，采用高效液相色谱-串联质谱仪多反应监测扫描模式检测和同位素内标定量。检测水产品屮的氯霉素和红霉素定量限分别为0.1ug/kg和0.5ug/kg。不同水产品（鱼、虾和蟹）在3个添加水平的平均回收率在86.7%'02.6%之间，相对标准偏差小于5%（n=6）。本方法简单易行、灵敏度较高，在日常检测方面

2、存在一定优势。关键词：固相萃取;高效液相色谱-串联质谱;水产品;氯霉素;红霉素;E~mai1:wangyangruanfeng@l63.基金：浙江省2013年农业标准化研宂项ASimultaneousDeterminationofChloramphenicolandErythromycinResiduesinAquaticProductsbyHighPerformanceLiquidChromatography-TandemMassSpectrometrywithOasisPRiMEHLBSolidPhaseExtractionCleanupKEQingqingLIShiya

3、nZHOUFanZHENGChongyingBEIYijiangWANGDingnanWANGYangAquaticProductsQualityInspectionCenterofZhejiangProvince;Abstract：Arapidmethodwasdevelopedforthesimultaneousdeterminationofchloramphenicolanderythromycinresiduesinaquaticproductsbyhighperformanceliquidchromatography-tandemmassspectrometrywi

4、thsolidphaseextraction(SPE).SampleswereextractedwithacetonitrileandtheextractwasthenpurifiedbyanOasisPRiMEIILBSPEcartridge.Theanalytesweredetectedinthemulti-reactionmonitoring(MRM)modeandquantifiedbytheisotopeinternalstandardmethod.Thelimitsofquantification(LOQ)forchloramphenicolanderythrom

5、ycinwere0.1and0.5Pg/kg,respectively.Theaveragerecoveriesofthe2analytesrangedfrom86.7%to102.6%withrelativestandarddeviationsoflessthan5%inaquaticproducts(fish,shrimpandcrab)atthreespikedlevels(n=6).Thisproposedmethodwasadvantageousinroutinedetectionofantibioticresiduesinaquaticproductsforits

6、simplicityandhighsensibility.Keyword：solidphaseextraction;highperformanceliquidchromatography-tandemmassspectrometry;aquaticproducts;chloramphenicol;erythromycin;柯庆青，李诗言，周凡，等.基于通过型固相萃取-高效液相色谱-串联质谱法同时测定水产品中的氯霉素和红霉素[J].食品科学，2017,38(24):241-246.D01:10.7506/spkxl002-6630_201724039..spkx.netKEQi

7、ngqing,LIShiyan,ZHOUFan,etal.Simultaneousdeterminationofchloramphenicolanderythromycinresiduesinaquaticproductsbyhighperformanceliquidchromatography-tandemmassspectrometrywithOasisPRiMEIlLBsolidphaseextractioncleanup［J］.FoodScience,2017,38(24):241-246.(i