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当前位置:首页 > 商业/管理/HR > 项目/工程管理 > 咪鲜胺及其代谢产物在橙汁中的残留检测方法研究
PesticideScienceandAdministration2011,32(6),,,,(//,550025)DeterminationofResiduceofProchlorazandItsMetaboliteinOrangeJuiceGaoJie,HuDeyu,ZhangYuping,LiHongqin,GuoQingqing(ResearchandDevelopmentCenterforFineChemicals,GuizhouUniversity,Guiyang550025,China)Abstract:AGCmethodforthedeterminationofresidueofprochlorazanditsmetaboliteinor-angejuicewasdescribedinthispaper.Thesampleswereextractedwithpetroleumether-acetone(8∶2,byvol),theextractantthenre-extractedwithpetroleumetherbyliquid-liquidextraction.prochlorazandmetabolitereactedwithpyridinechlorideathightemperature,theproduct2,4,6-trichlorophenolwasdetected.Thelimitofdetectionofthemethodwas10-11g,thelimitofconcentrationdetectedwas0.01mg/kg.Therecoveriesofprochlorazinorangejuicewerebe-tween72.5%and109.1%,withacoefficientofvariationbetween5.7%and9.7%,whichmetwiththerequirementsofpesticideresidueanalysis.Theresultsshowedthatthehalf-livesofprochlorazinroomtemperatureandfreezingenvironmentconditionwere56.4dand105.0dre-spectively,itshowedthatthedegradationofprochlorazwasslowinfreeze.Themethodde-scribedherewithoptimizationofthederivationandpurificationofprochlorazismoreaccurateandsensitivethanthatofthepreviousprocedures.Keywords:prochloraz;residueorangejuice;GC-ECD;analysis:(GC-ECD),:(8∶2,V/V),,,2,4,6-。10-11g,0.01mg/kg,72.5~109.1%,5.7~9.7%,。,:56.3d105.0d。。,、、、。:;;;:S481+.8;O657.7+1:A:1002-5480(2011)06-35-05:2011-01-04:(2008F376):(1985-),,,。:(1965-),,,。:0851-3620521;E-mail:fcc.dyhu@gzu.edu.cn。35--PesticideScienceandAdministration2011,32(6)(prochloraz)[1],,,。[2~4],N--N[2-(2,4,6-)]、N--N--N[2-(2,4,6-)]N--2-(2,4,6-)()[4],2,4,6-(1)[2]。FAO/WHO(CCPR)[5],,。。,Paoli[6],;[7]。。Lafuente[8];[9]。。,,2,4,6-,GC-ECD,。。11.1Agilent6890N(ECD),RF-2000();N-ELAPTM;HY-4();SHZ-III(),DF-101S(),KQ-250E()。(98.5%,);2,4,6-(99.0%,);、、、,;,,,。1.21.2.1(0.0001g)100mL,,,208μg/mL。1.2.220mL150mL,∶=8∶2(V/V)50mL,0.5h10min,,20mL,,,40mL×3,,2gNaCl,,,,3mL,10mL,。。1.2.32g,,220~240℃1.5h,,20mL2,。1.2.440mL×2,,136--PesticideScienceandAdministration2011,32(6),,,2mL,。1.2.5Agilent6890(μECD-Ni63,);:HP-5,60m×0.32mm×0.25μm;:140℃;:300℃;:250℃;:N2(),:2.0mL/min;:147.2kPa;:60∶1;::140℃5min,15℃/min280℃10min,:1μL。,2,4,6-8.0min,0.005mg/kg(0.01mg/kg)。22.12.1.12,4,6-,208μg/mL,0.0520、0.520、5.20、10.4、20.8μg/mL5,1.2.5,1.0μL。A,C,。0.0520~20.8μg/mL,0.9996,y=80554x+20093,(2)。2.1.2,3,0.01、0.1、1mg/kg,5。,72.5~109.1%,。(1)。(3、4)。2.1.31,0.01~1mg/kg,5.7~9.7%,3(LOD),LOD10-11g,0.01mg/kg。32,4,6-(Rt)=8.006min41(n=5)(mg/kg)(%)(%)(%)123450.0193.672.592.186.689.486.89.70.1107.4109.191.8106.4107.2104.46.8180.289.893.590.890.288.95.7237--PesticideScienceandAdministration2011,32(6)2.2[10、11],。,,。。210℃,。10mL,,,。。,、。2.3,2,4,6-,。,,,1.2.2、1.2.3,1.2.5,(1)。,。2.4,,-20℃()25℃(),。3,(6、7)。5(Rt)=8.102min22,4,6-(μg)(μg)(μg)230.500.550.520.470.51103.06.39.509.519.539.489.51100.14.9(μg)1(μg)3(d)(mg/kg)(mg/kg)(%)01.021.0230.965.90.983.950.8417.60.9413.770.8219.60.8816.7100.8021.60.8516.7140.7922.50.8219.6210.7229.40.8219.6300.6833.30.7823.6500.5150.00.7130.3(%)38--PesticideScienceandAdministration2011,32(6)673,,,,,。,,pH,、、。,。1.()[J].,1995,17(3):63~65.2ANDREASHR,ROBERTK,MUFITB.Investigationsonthemetabolicfateofprochlorazinsoilunderfieldandlaboratoryconditions[J].PesticSci,1999,55:531~538.3,,.[J].,2003,22(6):749~753.4MICHAELE,FERRERI,JERRYA,etal.Discoveringmetabolitesofpost-harvestfungicidesincitruswithliquidchromatography/time-of-flightmassspectrometryandiontraptandemmassspectrometry[J].JChromatA,2005,1082:71~80.5,.[J].,2004,23(6):704~706.6PAOLIM,TACCHEOBM,DAMIANOV,etal.Simplifieddeterminationofcombinedresiduesofprochlorazanditsmetabolitesinvegetable,fruitandwheatsamplesbygaschromatography[J].JChromatA,1997,765:127~131.7,,.[J].,2005,7(1):54~58.8LAFUENTEMT,TADEOJL.Residuesanalysisofpost-harvestimidazolefungicidesincitrusfruitbyHPLCandGLC[J].EnvironAnalChem,1985,22:99~108.9,,.[J].,2006,28(3):354~357.10,,.[J].,2007,13(3):15~17.11.()[M].:,2005:363~369.39--
本文标题:咪鲜胺及其代谢产物在橙汁中的残留检测方法研究
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