《食品工业》2023年第44卷第2期311分析检测固相萃取-气相色谱质谱法测定食糖中丙烯酰胺李海霞，陈克云，李霞，梁秀清，陈倩倩，刘艳明*山东省食品药品检验研究院，国家市场监管重点实验室（肉及肉制品监管技术），山东省特殊医学用途配方食品质量控制工程技术研究中心，山东省食品药品安全检测工程技术研究中心（济南250101）摘要建立快速测定食糖中丙烯酰胺含量的分析方法。食糖样品经水溶解提取,CleanertACA固相萃取小柱净化后,采用气相色谱质谱法(GC-MS)检测,内标法定量。结果表明,丙烯酰胺在10~1000μg/L范围内线性关系良好,相关系数大于0.999,方法检出限为10μg/kg,定量限为20μg/kg。白糖样品在20,200和1000μg/kg3个质量分数水平下的加标回收率为90.42%~106.70%;红糖样品在200,400和1000μg/kg3个质量分数水平下的加标回收率为97.00%~113.93%,相对标准偏差为3.25%~5.13%。该方法简化了样品前处理过程,具有样品处理操作简单、分析周期短、净化效果好等优点,可以满足食糖中丙烯酰胺的测定。关键词食糖;丙烯酰胺;固相萃取;CleanertACA;气相色谱-质谱法DeterminationofAcrylamideinSugarbySoildPhaseExtractionCoupledwithGasChromatography-MassSpectrometryLIHaixia,CHENKeyun,LIXia,LIANGXiuqing,CHENQianqian,LIUYanming*ShandongInstituteforFoodandDrugControl,KeyLaboratoryofSupervisingTechnologyforMeatandMeatProductsforStateMarketRegulation,ShandongResearchCenterofEngineeringandTechnologyforQualityControlofFoodforSpecialMedicalPurposes,ShandongResearchCenterofEngineeringandTechnologyforSafetyInspectionofFoodandDrug(Jinan250101)AbstractArapiddeterminationmethodfortheacrylamideinsugarwasestablished.AcrylamidewasextractedfromsampleswithwaterandtheextractwascleanedupbyCleanertACAcolumn.ThetargetcompoundsweredetectedbyGC-MSandquantifiedbyaninternalstandardmethod.Theresultsshowedthatthecalibrationcurvesforacrylamideinsugarshowedgoodlinearityandwithacorrelationof0.999.Thelimitofdetection(SLOD)was10μg/kg,andthelimitofquantitative(SLOQ)was30μg/kg.Therecoveriesofwhitesugarat20,200and1000μg/kgwere90.42%-106.70%.Therecoveriesofbrownsugaratthelevelsof200,400and1000μg/kgwere97.00%to113.93%withrelativestandarddeviations(SRSD)of3.25%-5.13%(n=6).Themethodsimplifie...
