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1、2016年10月Vol.34No.10October2016ChineseJournalofChromatography1005~1010研究論文DOI:10.3724/SP.J.1123.2016.05026氣相色譜法測定蘋果和土壤中的高效氯氟氰菊酯1#1#1211?陳姣姣,張靜,吳思卓,張廣龍,張侃侃,胡德禹(1.貴州大學(xué)精細化工研究開發(fā)中心,綠色農(nóng)藥與農(nóng)業(yè)生物工程國家重點實驗室培育基地和教育部重點實驗室,貴州貴陽550025;2.貴陽市環(huán)境監(jiān)測中心站,貴州貴陽550002)摘要:建立了改進的QuEChERS?氣相色譜檢測蘋果和土壤中高效氯
2、氟氰菊酯殘留的分析方法,考察和評價了蘋果和土壤兩種基質(zhì)對高效氯氟氰菊酯的基質(zhì)效應(yīng)。蘋果和土壤樣品均用乙腈提取,經(jīng)石墨化碳黑(GCB)凈化后直接進樣分析。結(jié)果表明:在優(yōu)化后的QuEChERS條件下,高效氯氟氰菊酯在0?05~10mg/L范圍內(nèi)線性關(guān)系良好,相2關(guān)系數(shù)(R)大于0?999,檢出限為0?12~0?15μg/kg,定量限為0?38~0?50μg/kg。用基質(zhì)標準曲線定量時,高效氯氟氰菊酯在土壤和蘋果中的回收率分別為88?29%~97?65%和80?70%~98?69%。蘋果和土壤樣品對高效氯氟氰菊酯都表現(xiàn)出基質(zhì)增強效應(yīng)。該方法的回收率均
3、能達到殘留分析要求,用基質(zhì)配制標準溶液能夠有效、方便地校正氣相色譜?電子捕獲檢測器測定高效氯氟氰菊酯殘留時的基質(zhì)效應(yīng),且能應(yīng)用于蘋果和土壤實際樣品的檢測。關(guān)鍵詞:氣相色譜;基質(zhì)效應(yīng);高效氯氟氰菊酯;蘋果;土壤中圖分類號:O658文獻標識碼:A文章編號:1000?8713(2016)10?1005?06Determinationoflambda?cyhalothrininapplesandsoilbygaschromatography1#1#12CHENJiaojiao,ZHANGJing,WUSizhuo,ZHANGGuanglong,11?Z
4、HANGKankan,HUDeyu(1.ResearchandDevelopmentCenterforFineChemicals,StateKeyLaboratoryBreedingBaseofGreenPesticideandAgriculturalBioengineering,KeyLaboratoryofGreenPesticideandAgriculturalBioengineering,MinistryofEducation,GuizhouUniversity,Guiyang550025,China;2.GuiyangEnvironm
5、entalMonitoringCenter,Guiyang550002,China)Abstract:AmodifiedQuEChERS?gaschromatographymethodwasdevelopedtodeterminetheresiduesoflambda?cyhalothrininapplesandsoil.Moreover,thematrixeffectsinapplesandsoilwereinvestigatedandevaluated.Theappleandsoilsampleswereextractedwithaceto
6、ni?trileandpurifiedbygraphitizedcarbonblack(GCB).Thelinearityoflambda?cyhalothrinwas2goodintherangeof0?05-10mg/Lwithcorrelationcoefficients(R)morethan0?999.Thelimitsofdetectionandlimitsofquantificationwere0?12-0?15μg/kgand0?38-0?50μg/kg,respectively.Withthematrix?matchedcali
7、bration,therecoverieswere88?29%-97?65%and80?70%-98?69%insoilandapples,respectively,whichwereintheacceptablerange.Matrixenhancementeffectswereobservedintheappleandsoilsamples.Theestablishedmethodcanbeappliedontheresidualanalysisoflambda?cyhalothrininactualappleandsoilsamples.
8、Thematrix?matchedcalibrationsolutioncanefficientlycompensatethematrixeffect