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《凝膠滲透色譜-氣相色譜-質(zhì)譜方法測(cè)定茶葉中五種高毒有機(jī)磷農(nóng)藥殘留》由會(huì)員上傳分享,免費(fèi)在線閱讀,更多相關(guān)內(nèi)容在行業(yè)資料-天天文庫(kù)。
1、2011年第10期廣東化工第38卷總第222期www.gdchem.com135凝膠滲透色譜.氣相色譜.質(zhì)譜方法測(cè)定茶葉中五種高毒有機(jī)磷農(nóng)藥殘留鄒孝1.,高熹,劉小文肖昭競(jìng),段云鵬,胡羽2,吳國(guó)星,葉敏,肖春,李正躍(1.云南農(nóng)業(yè)大學(xué)植物保護(hù)學(xué)院,云南昆明650201;2.重慶市計(jì)量質(zhì)量檢測(cè)研究院,重慶400200)[摘要]本研究建立了以凝膠滲透色譜(gelpermeationchromatography,GPC)為樣品前處理方法,同時(shí)以氣相色譜-質(zhì)譜聯(lián)用(gaschromatography—massspectrometry,GC—MS)技術(shù)分析茶葉中五種高毒有機(jī)磷農(nóng)藥殘留
2、量的方法。樣品用丙酮提取,共提物用乙酸乙酯:環(huán)己烷(1:1,v,v)作流動(dòng)相的GPC凈化,脫水濃縮定容,采用氣相色譜.質(zhì)譜聯(lián)用,在選擇離子監(jiān)測(cè)模式下進(jìn)行檢測(cè),用外標(biāo)法定量。結(jié)果表明,濃度與其峰面積在O.005-0.500mg/L范圍內(nèi)具有良好的線性關(guān)系,3個(gè)添加水平的平均回收率分別為:99.68%~106.31%,94.14%~9811%,93.86%~98-21%,相對(duì)標(biāo)準(zhǔn)偏差(RSD)均小于l0%,檢出限為0.0005-4).0020mgg[關(guān)鍵詞】凝膠滲透色譜:氣相色譜一質(zhì)譜聯(lián)用;茶葉;高毒有機(jī)磷農(nóng)藥;多殘留[中圖分類號(hào)]0657[文獻(xiàn)標(biāo)識(shí)碼1A[文章編號(hào)]1007—
3、1865(2011)10—0135—02DeterminationofFiveHigh-toxicOrganicPhosphorusPesticidesResiduesinTeabyGelPermeationChromatographyandGasChromatography—massSpectrometryZouXiao,GaoXi,LiuXiaowen,XiaoZhaojing,DuanYunpeng,HuYu,WuGuoxing,YeMin,XiaoChun,LiZhengyue(1PlantProtectionInstitute,YunnanAgricultural
4、University,Kunming650201;2.ChongqingAcademyofMetrologyandQualityInspection,Chongqing400200,China)Abstract:Amultiresiduemethodbasedongelpermeationchromatography(GPC)forthesamplepreparationandgaschromatography-massspectrometryanalysiswasdevelopedtodeterminefivehigh-toxicorganicphosphoruspest
5、icidesresiduesinteaThesamplewereextractedusingacetoneThentheextractswereelutedwithethylacetate/cyclohexane(1:1)byGPC.Afierdehydratedandconcentratedtoadefinitevolume,thepesticideswerefinallydeterminedbygaschromatography—massspectrometryinselective—ionMonitor(SIM1simultaneously,andquantified
6、byextemalstandardmethod.Theresultsshowedagood1inearrelationshipwasobtainedbetweenconcentrationandpeakareawithinthe0.005-0.500mg/Lrange.Averagerecoveriesof5pesticidesatthreefo~ifiedlevelswere9968%~l0631%,94.14%-9811%and9386%-9821%respectively.Therelativestandarddeviationofthemethodwaslessth
7、an10%ineverycase.respectively.Thelimitsofdetectionof5pesticideswererangin~from0.0005-00020mg/kg.Keywords:gelpermeationchromatography:gaschromatography·massspectrometry;tea;high·toxicorganicphosphoruspesticides;multiresidue甲胺磷、甲基對(duì)硫磷、對(duì)硫磷、久效磷、磷胺等五種高毒有mg/L、0.250mg