《食品工业》2023年第44卷第2期277分析检测HPLC-MS/MS测定油菜花蜂蜜中20种磺酰脲类除草剂田亚，张淑霞，孙转莲，王向军*郑州海关技术中心（郑州450016）摘要建立一种基于QuEChERS(QuichEasyCheapEffecetiveRuggedandSafe)前处理技术和高效液相色谱-串联质谱法同时测定油菜花蜂蜜中20种磺酰脲类除草剂残留量的方法。样品经1%甲酸乙腈溶液提取后,上清液采用PSA、C18(50mg、25mg)进行净化,以0.01%甲酸-2mmol/L甲酸铵甲醇溶液与0.01%甲酸-2mmol/L甲酸铵水溶液为流动相,采用Agilent超高压快速分离色谱柱RRHDEclipsePlusC18(2.1mm×50mm,1.8μm)进行分离,在电喷雾正离子模式下,以多反应监测(MRM)方式采集,采用基质匹配的标准曲线进行外标法定量。结果表明,20种磺酰脲化合物分别在0.2~200μg/L和0.5~200μg/L的线性范围内呈良好关系,相关系数均不小于0.9991,检出限为0.5~1.0μg/kg,定量限为1.0~2.5μg/kg。在10,50和100μg/kg添加水平下的回收率为77.9%~104.1%,相对标准偏差(n=6)为1.0%~6.5%。该方法操作简单,准确灵敏,适用于油菜花蜂蜜中20种磺酰脲类除草剂残留量的同时检测。关键词QuEChERS;高效液相色谱-串联质谱;油菜花蜂蜜;磺酰脲类除草剂Determinationof20SulfonylureaHerbicideinRapeHoneybyHPLC-MS/MSTIANYa,ZHANGShuxia,SUNZhuanlian,WANGXiangjun*ZhengzhouCustomsTechnologyCenter(Zhengzhou450016)AbstractAmethodbasedonQuEChERS(QuichEasyCheapEffecetiveRuggedandSafe)pretreatmenttechniqueandHPLC-MS/MSwasexploitedforthesynchronouslytestingof20sulfonylureaherbicidevestigitalinrapehoney.Samplesafter1%formicacidacetonitrilesolutionextraction,supernatantusingPSA,C18(50mg,25mg)forpurification,withmethanol(0.01%formicacid-2mmol/Lammoniumformate)andwater(0.01%formicacid-2mmol/Lammoniumformate)asmobilephase,usingAgilentEclipsePlusC18RRHD(2.1mm×50mm,1.8μm)chromatographiccolumnseparation,usingamatrix-matchedstandardcurve,andquantitativeusingexternalstandardmethod.Theresultsshowedthatthereweregoodrelationshipwithintheirrespectivelinearrangeof0.2-200μg/Land0.5-200μg/L,thecorrelationcoefficients(r)werenotlessthan0.9991,detectionlimitrangewas0.5-1.0μg/kg,andquantitativelimitrangewas1.0-2.5μg/kg.Therecoveryatfortificationlevelsof10,50and100μg/kginrapehoneywas77.9%to104....
