分散液液微萃取／气相色谱-质谱法测定蜂蜜中六六六和滴滴涕类农药残留.pdf

分散液液微萃取／气相色谱-质谱法测定蜂蜜中六六六和滴滴

涕类农药残留

王东;侯传金;赵尔成;贾春虹

【摘要】建立了分散液液微萃取（DLLME）与气相色谱-质谱法（GC-MS）联

用快速检测蜂蜜中六六六（BHC）和滴滴涕（DDT）类农药残留的分析方法。使

用三氯甲烷为萃取剂，通过涡旋、离心使分析物富集到微量三氯甲烷中，采用气相

色谱-质谱进行分析。实验对影响DLLME萃取效率的因素，如萃取剂种类和体积、

分散剂种类和体积、萃取时间等进行了考察，同时对方法的基质效应和性能进行了

评估。结果显示：由于基质效应，8种六六六和滴滴涕类农药都出现信号增强现象。

8种六六六和滴滴涕类农药在2~500μg／L范围内线性关系良好，相关系数（r2）

为0.991~0.998，方法富集倍数为74~96；当试样的加标水平为20、50和

100μg／kg时，8种六六六和滴滴涕类农药的回收率为61.0％~100.1％，相对标

准偏差（RSD，n=5）为2.2％~19.5％。8种六六六和滴滴涕类农药的最低检测

浓度均为20μg／kg，最小检出量皆为1.0ng。该方法简单、快速、高效，适用

于蜂蜜中六六六和滴滴涕类农药的残留检测。%Agaschromatography-mass

spectrometry(GC-MS)methodforthedeterminationof

hexachlorocyclohexane(BHC)and

dichlorodiphenyltrichloroethane(DDT)residuesinhoneywasdeveloped

usingdispersiveliquid-liquidmicroextraction(DLLME)assample

preparationmethod.Thesampleswereextractedwithchloroform,and

concentratedintochloroformbyvortexandcentrifuging.Theanalytes

wereanalyzedbyGC-MS.Thefactorsaffectingtheextrac-tionefficiency

wereinvestigated,suchasthetypeandvolumeofextractionanddispersive

sol-vent,extractiontime,etc.Thematrixeffectsandmethodperformance

wereevaluatedatthesametime.Theresultsindicatedthatalltheeight

BHCandDDTpesticidesdisplayedtheenhancementofsignalsduetothe

matrixeffects.Thecalibrationcurveswerelinearintherangeof2-500μg/L

andthecorrelationcoefficientswere0.991-0.998fortheeightBHCand

DDTpesticides.Theenrichmentfactors(EF)were74-96fortheeight

pesticides.Therecover-iesoftheeightBHCandDDTpesticidesatthree

spikedlevelsof20,50and100μg/kgwere61.0%-100.1%,whiletheRSDs

were2.2%-19.5%.Thelimitsofquantificationfortheeightpesticides

were20μg/kg,andthelimitsofdetectionwere1.0ng.Thedeveloped

methodisnbsp;easy,quickandwithhighperformance.Itisapplicablefor

thedeterminationofBHCandDDTresiduesinhon