改良QuEChERS法结合气相色谱串联质谱测定果蔬中20种杀菌剂.pdf

第4卷第1期食品安全质量检测学报Vol.4No.1
2013年2月JournalofFoodSafetyandQualityFeb.,2013

改良QuEChERS法结合气相色谱串联质谱
测定果蔬中20种杀菌剂

谢建军1*,陈捷1,李菊2,袁震宇1,谢玉珊1

(1.广东出入境检验检疫局,广州510623;
2.东莞出入境检验检疫局,东莞523000)

摘要:目的建立果蔬中20种杀菌剂(三环唑、五氯硝基苯、嘧霉胺、乙烯菌核利、百菌清、三唑酮、戊菌
唑、腐霉利、三唑醇、多效唑、稻瘟灵、抑霉唑、咯菌腈、氟硅唑、腈菌唑、肟菌酯、丙环唑、咪鲜胺、腈
苯唑、苯醚甲环唑)残留量的QuEChERS-GC/MS快速测定方法。方法以生菜、毛瓜、葡萄、李子为原料,样

品经乙腈提取,PSA粉50.0mg、Al2O3粉50.0mg和NH2粉30.0mg除杂净化后,用GC/MS外标法定量。结果
三环唑等20种杀菌剂在0.025~0.250mg/L的质量浓度范围内线性关系良好,相关系数为0.9974~1.0000。添加
水平为0.05、0.1、0.2mg/kg时,除百菌清外,其余19种杀菌剂平均回收率范围均处于83%~112%之间,相对
标准偏差(RSD)小于11.0%,方法的检出限(LOD)为0.2~11.8μg/kg之间。结论本方法具有灵敏、快速、简便
等特点,能满足果蔬中三环唑等20种农药杀菌剂的检测要求。
关键词:气相色谱/质谱法;QuEChERS;杀菌剂;残留测定

Determinationof20kindsoffungicideresiduesinvegetablesandfruitsbygas
chromatography-massspectrometrycombinedmodifiedQuEChERSmethod

XIEJian-Jun1*,CHENJie1,LIJu2,YUANZhen-Yu1,XIEYu-Shan1

(1.GuangdongEntry-ExitInspectionandQuarantineBureau,Guangzhou510623,China;
2.DongguanEntry-ExitInspectionandQuarantineBureau,Dongguan523000,China)

ABSTRACT:ObjectiveTodevelopaQuEChERSmethodcombinedwithgaschromatographymassspec-
trometry(GC/MS)forthedeterminationof20kindsoffungicideresidues(tricyclazole,quintozene,pyrimetha-
nil,vinclozolin,chlorothalonil,triadimefon,penconazole,procymidone,triadimenol,paclobutrazol,iso-
prothiolane,imazalil,fludioxonil,flusilazole,myclobutanil,trifloxystrobin,propiconazol,prochloraz,fenbu-
conazoleanddifenoconazole)invegetablesandfruits.MethodsTwentykindsoffungicidesresidueswere
extractedfromthesamples(lettuce,hairysquash,grapeandplum)withacetonitrile,andthendetectedby

GC/MSwithexternalstandardmethodafterbeingcleanedupwiththreesorbents(PSA50.0mg,Al2O350.0mg

andNH230.0mg).ResultsThemethodshowedagoodlinearityovertherangeof0.025~0.250mg/Lwith
correlationcoefficientsof0.9974~1.0000.Therecoveriesoffungicides,exceptChlorothalonil,wereinthe
rangeof83%~112%withthespikedlevelsof0.05,0.1and0.2mg/kgintofourvegetablesandfruitsmatrixes,
andtherelativestandarddeviations(RSDs)werealmostnotmorethan11.0%.Thelimitsofdetections(LODs)