CEREAL&FOODINDUSTRYVol.30,2023,No.4粮食与食品工业CerealandFoodIndustry标准与检测超临界流体色谱串联质谱法测定粮食中硫双威的研究谢婷婷福建省粮油质量监测所摘要：本试验在QuEChERS方法前处理粮食样品（稻谷、小麦）的基础上，研究了不同改性剂、makeup溶液、背压、makeup泵流速和色谱柱温度对硫双威质谱响应的影响，建立了超临界流体色谱串联质谱的测定方法并进行方法学考察。结果表明：硫双威浓度在10～500μg/L范围内呈现良好的线性关系（相关系数R²>0.991)，定量限为15μg/kg，分别选取稻谷、小麦进行测定，在添加3个浓度水平下测得加标回收率在71.2%~103.5%，相对标准偏差为2.64%～10.68%（n=6）。采用SFC-MS/MS方法检测硫双威较LC-MS/MS检测更具有环保性（低溶剂）、成本低的优势。关键词：硫双威；超临界流体色谱串联质谱联用技术；超高效液相色谱串联质谱联用技术中图分类号：TS201文章编号：1672-5026(2023)04-048－06Determinationofthiocarbingrainbysupercriticalfluidchromatographytandemmassspectrometry(福州350012)文献标识码：AXieTingtingInstituteofGrainandOilQualitySupervisionandTestofFujianProvince(Fuzhou350012)Abstract:Basedonthepretreatmentofgrainsamples(riceandwheat)withQuEChERSmethod,thisexperimentstudiedtheeffectsofdifferentmodifiers,makeupsolution,backpres-sure,makeuppumpflowrateandcolumntemperatureonthemassspectrumresponseofthiodi-carb.Anewmethodforthedeterminationofthiodicarbingrainbysupercriticalfluidchromatog-raphy-tandemmassspectrometrywasestablishedandthemethodologywasinvestigated.Theresultsshowedthatthecalibrationcurvesforthiodicarbdemonstratedgoodlinearityintherangeof10~500μg/L,withthecorrelationcoefficientsbetterthan0.991,andthequantificationlimitswas15μg/kg.Theaveragerecoveriesofthiodicarbatthespikedlevelsof50,100,200μg/kgrangedfrom71.2%~103.5%withRSDsof2.64%~10.68%(n=6).ConclusionComparedwithLC-MS/MS,theSFC-MS/MSmethodhastheadvantagesofenvironmentalprotection(lowersolvent)andlowercost.Keywords:thiodicarb;supercriticalfluidchromatographymassspectrometry;highperformanceliquidchromatographytandemtriplequadrupolemassspectrometry硫双威（C1oH1sN4O4S，），又名硫双灭多威，是收稿日期：2023-03-22作者简介...
