高分子印记固相萃取-液相色谱质谱法测定水产品中孔雀石绿、结晶紫、亮绿及其代谢产物李晓丽1,2李娜1李鹏1,3刘力2苗虹1（1.中国疾病预防控制中心营养与食品安全所化学污染与健康安全重点实验室，北京100021；2.西南大学动物科技学院，重庆400715；3.中国农业大学动物医学院，北京100193）摘要：目的建立一种高分子印记固相萃取-液相色谱质谱联用(MISPE-HPLC/MS2)测定水产品中孔雀石绿、结晶紫、亮绿及其代谢产物的检测方法。方法样品经乙腈提取后，经中性氧化铝柱和高分子印记固相萃取柱净化，WatersAtlantisT3色谱柱（2.1mm×150mm，3μm）分离，乙腈和0.1%甲酸水等度洗脱，采用选择反应监测（SRM）模式进行正离子扫描，内标法定量。结果待测化合物在0.2μg/L~10μg/L范围内有很好的相关性，相关系数大于0.99，加标水平为1μg/kg、2μg/kg、4μg/kg，孔雀石绿、结晶紫和亮绿的平均回收率分别为93.2%~105.9%、92.7%~107.5%和60.6%~94.4%，相对标准偏差均小于12.5%，孔雀石绿、结晶紫和亮绿的检出限分别为0.02μg/kg、0.03μg/kg、0.03μg/kg，定量限分别为0.07μg/kg、0.10μg/kg、0.10μg/kg。结论本方法前处理净化效果更好、灵敏度更高，同时采用稳定性同位素稀释技术及基质匹配标准曲线，将基质抑制效应降低到最低，适用于大批量鱼类产品中孔雀石绿、结晶紫和亮绿的检测。关键词：孔雀石绿；结晶紫；亮绿；高分子印记固相萃取；液相色谱-质谱法Determinationofmulti-residuesformalachitegreen,crystalviolet,brilliantgreenandtheirmetabolitesinfishbyusingmolecularlyimprintedsolid-phaseextractionfollowedbyhighperformanceliquidchromatography-tandemmassspectrometryLiXiaoli，LiNa,LiPeng,LiuLi,MiaoHong(KeyLaboratoryofChemicalSafetyandHealth,NationalInstituteforNutritionandFoodSafety,ChineseCentreforDiseaseControlandPrevention,Bei激ng100021,China)Abstact:ObjectiveToestablishamethodbasedonmolecularlyimprintedsolid-phaseextractionandliquidchromatography-massspectrometry(MISPE-HPLC/MS2)forthedeterminationofmalachitegreen,crystalviolet,brilliantgreenandtheirmetabolitesinaquatic.MethodsTheaquaticsampleswereextractedwithacetonitrileandtheextractwerecleanedupbyAlu---本文来源于网络，仅供参考，勿照抄，如有侵权请联系删除---mina-Nandmolecularlyimprintedsolid-phaseextractioncatridge（MISPE）.ThesampleswereseparatedonaWatersAtlantisT3column（2.1mm×150mm，3μm）,acetonitrileand0.1%formicacid-waterwereusedasmobilephasesforisocraticelution，ESIpositiveionscanmodewasusedwithselectedreactionmonitoring(SRM,MS2)，andMG-D5andCV-D6wereusedasinternalstandardsforquantification.ResultsTheleanerrelationforthemalachitegreen,crystalvioletandbrilliantgreenwereintherangeof0.2μg/L~10μg/Lwithacorrelationcoefficientnotlessthan0.99.Themeanrecoveriesofspikedsamplesatthelevelof1.0μg/kg,2.0μg/kgand4.0μg/kgwereintherangeof93.2%~105.9%,92.7%~107.5%and60.6%~94.4%formalachitegreen,crystalvioletandbrilliantgreen,respectively,therelativestandarddeviationsalllessthan12.5%.Thedetectionlimitsofmalachitegreen,crystalvioletandbrilliantgreenwere0.02μg/kg,0.03μg/kgand0.03μg/kg,andthequantificationlimitswere0.07μg/kg,0.10μg/kgand0.10μg/kg,respectively.ConclusionThismethodusedthestableisotopedilutiontechniqueandmatrix-matchedcalibrationwasvalidatedtobehighextractionselectivity,sensitivityandbetterpurificationforthedeterminationofmalachitegreen,crystalviolet,brilliantgreenandtheirmetabolitesinalargeofrealaquaticsamples.Keywords:malachitegreen;crystalviolet;brilliantgreen;molecularlyimprintedsolid-phaseextraction;liquidchromatograpy-massspectrometry孔雀石绿（malachitegreen，MG）、结晶紫（crystalviolet，...