《食品工业》2023年第44卷第2期332分析检测UPLC-MS/MS测定桂皮中的氨基甲酸酯类农药残留吴晓萍福建中检华日食品安全检测有限公司(福州350028)摘要建立桂皮中8种氨基甲酸酯类农药的QuEChER-超高效液相色谱-串联质谱检测方法。样品经乙腈提取并由混合净化剂(PSA、MWCNTs和无水硫酸镁)净化,色谱柱分离,在多反应监测模式下进行测定。在0.001~0.5μg/mL范围内,8种氨基甲酸酯类农药在桂皮中的峰面积与其质量浓度呈良好线性关系(R2>0.99)。在0.02,0.04和0.20mg/kg添加水平下重复6次试验,8种氨基甲酸酯类农药回收率为71.0%~110.7%,相对标准偏差(SRSD)为1.7%~10.3%,定量限(SLOQ)为0.02mg/kg。试验方法简捷、灵敏、稳定,可满足实际检测需求。关键词QuEChERS;高效液相色谱-串联质谱;桂皮;氨基甲酸酯SimultaneoueDeterminationofCarbamatePesticideinCinnamomumcassiabyUPLC-MS/MSWUXiaopingFujianCCIC-FairreachFoodSafetyTestingCo.,Ltd.(Fuzhou350028)AbstractAnanalyticalmethodforthedeterminationof8carbamatepesticidesinCinnamomumcassiausingultraperformanceliquidchromatography-tandemmassspectrometry(UPLC-MS/MS)matchingaQuEChERSprocedurewasdeveloped.Thesampleswereextractedwithacetonitrileandcleaned-upbyprimarysecondaryamine(PSA),multi-walledcarbonnanotubes(MWCNTs)andMgSO4assorbentinCinnamomumcassia.TheanalyteswereseparatedbyacolumnofC18connectedtoanelectrosprayionizationsourceinpositivemode(ESI+)andmonitoring(MRM)mode.Eightpesticidesshowedgoodlinearityintherange0.001-0.5μg/mLwithcorrelationcoefficientshigherthan0.99.Theaveragerecoveriesrangedfrom71.0%to110.7%inCinnamomumcassiaatthreelevels(0.02,0.04and0.20mg/kg)andtherelativestandarddeviation(SRSD)was1.7%-10.3%(n=6).TheSLOQwas0.02mg/kg.Themethodwassimple,sensitiveandstable,meetingtherequirementsofpracticaldetection.KeywordsQuEChERS;ultraperformanceliquidchromatography-tandemmassspectrometry(UPLC-MS/MS);Cinnamomumcassia;carbamate桂皮(或肉桂、官桂或香桂)常被用作中药、香料和调料。但近年来,随着食品安全要求的提高和农药的不合理使用,使得各个国家对这类产品制定严格的限量。农药残留问题影响我国桂皮的出口,故有必要建立一种能快速检测桂皮中农药残留的方法。关于桂皮中农药残留的检测方法主要有气相色谱量上...