水_土壤和蔬菜中毒死蜱_甲基毒死蜱残留检测前处理方法_张超

AGROCHEMICALSVol.49,No.5May2010(210095)LC18(21)LC18LC180.1~8.0mg/L0.99960.9994105μg/L80.5%~81.0%88.8%~92.4%0.5%~1.4%2.1%~4.6%80.7%~98.0%85.0%~95.5%0.4%~1.0%1.1%~3.9%80.4%~84.4%80.7%~83.7%0.8%~3.0%1.8%~3.3%TQ450.2A1006-0413(2010)05-0367-04PreparationforDeterminationofChlorpyrifosandChlorpyrifos-methylinWater,SoilandVegetableZHANGChao,YANGHong(SchoolofScience,NanjingAgriaulturalUniversity,Nanjing210095,China)Abstract:Apreparationmethodforsimultaneousdeterminationofpesticideschlorpyrifosandchlorpyrifos-methylinwater,soilandvegetablebyhigh-performanceliquidchromatography(HPLC)wasdeveloped.Watersampleswereexactedandcollectedbysolid-phaseextractionLC-18column.Soilsampleswereextractedbyethylacetate-petroleumether(2:1,byvol)andpurifiedandcollectedbysolid-phaseextractionLC-18column.Vegetablesamplewasextractedbyacetonitrileandpurifiedandcollectedbysolid-phaseextractionLC-18column.Thecalibrationcurvesofthemethodweredeterminedintherangeof0.1to8.0mg/Lbothchlorpyrifosandchlorpyrifos-methyl,withthecorrelationcoefficients(r2)were0.9996and0.9994respectively.Withtheminimaldetectionlimitsbeing10and5μg/L.Thespikedrecoveriesofchlorpyrifosandchlorpyrifos-methylinwatersamplerangedfrom80.5to81.0%and88.8to92.4%,thesoilsamplefrom80.7to98.0%and85.0to95.5%,thevegetablesamplefrom80.4to84.4%and80.7to83.7%,respectively.Withtherelativestandarddeviations(RSD)inwater,soilandvegetablesampleswerefrom0.5to1.4%and2.1to4.6%,0.4to1.0%and1.1to3.9%,0.8to3.0%and1.8to3.3%respectively.Keywords:chlorpyrifos;chlorpyrifos-methyl;residues;preparation;HPLC(chlorpyrifos)[1][2][3-4](chlorpyrifosmethyl)(DowAgroSciences)[5][6-8][9-10]SPEC18HPLCUVDSPEC18HPLCUVDSPEC18HPLCUVD2010011920100314(8632008AA10Z421)(1987)[e-mail]11.1(Waters)248751577251WD35(BuCHI)KH500()BS31(JeioTECH)TD1(Agilent)SPESupelcleanTMLC18(300mg/3mLSUPEL)()(TEDIA)(99%)(99%)1.21.2.1ODS(250mm4.6mmi.d.5μm)(85:15)0.6mL/min240nm20μL1.2.210.0mg25mL1.2.3S0~20cm1mm10.0g250mL20mL(2:1)3201510min2.0g20mL(21)240(SPE)5mL5mLSPEC181mL50mL12mL40HPLC1.2.410.0g250mL20mL3201510min3min1.0g2.0g5mL340(SPE)SPEC18HPLC1.2.31.2.55mL5mLLC182.5mL/min50mLLC18HPLC1.2.31.2.6248mg/L0.40.81.6mg/kg31.2.31.2.42410mg/L0.20.41.0mg/kg31.2.522.1(901085158020)0.6mL/min(9010)5min(8020)21min(8515)9.614min(8515)11(a)(b)(2.0mg/L)2.28.04.02.01.00.50.1mg/Ly=1348040.2072x95423.8219(r2=0.9996)y=1657520.7678x121485.6962(r2=0.9994)(S/N)3105μg/L2.32.3.1311.2.32310.0g250mL40mL20min20mL22.0g20105mL3222.0g405.0g2.0g0.5g10mL21mL(2)30mL(595)4035.0g403mL2mL2mL3mL2~32%5mL22.5g403(21)23140mL(21)SPEC18(1.2.3)12121.6mg/kg2(a)(b)2.3.2(41)SPELC18LC1860mL310mL232//%(mg·kg1)123/%0.481.380.179.780.41.10.881.482.681.781.90.81.684.581.886.984.43.00.482.682.186.483.72.80.879.281.082.080.71.81.681.085.380.382.23.31//%(mg·kg1)123/%0.498.498.896.998.01.00.881.582.881.682.00.91.680.481.080.780.70.40.482.888.883.385.03.90.896.194.196.495.51.31.688.990.490.790.01.1121.6mg/kg3(a)(b)2.3.3AGROCHEMICALSSPELC183LC185mL5mLLC1810mL5mL5mLLC1810mL1.2.540%60%80%343//%(mg·kg1)123/%0.280.279.681.880.51.40.480.080.780.880.50.51.081.080.481.781.00.80.290.489.286.788.82.10.495.487.393.792.14.61.093.089.295.192.43.20.4%~1.0%1.1%~3.9%80.4%~84.4%80.7%~83.7%0.8%~3.0%1.8%~3.3%[11-12]3[1].[M].:,1999:73.[2],旻,,.[J].,2007,6(2):6-9.[3].[M].:,1993:84-86[4].()[D].:,2000.[5],,,.[J].,2005,27(6):654-657.[6],,.[J].,1993,32(5):20-21.[7],.[J].,2008,14(1):30-32.[8],,,.[J].,2005,27(2):142-144.[9],,.[J].,1991,30(2):20-21.[10],.[J].,1998,37(1):23-25.[11],,,.[J].,2009,48(2):120-122.[12],.[J].,2005,15(2):242-246.120.2mg/kg4(a)(b)2.41~380.5%~81.0%88.8%~92.4%0.5%~1.4%2.1%~4.6%80.7%~98.0%85.0%~95.5%[1],.Strobilurin[J].,2002,24(2):l6-l9.[2].[M].:,2000:46-49.[3],.[M].:,2000.[4]..()[S].:,2000:26-29.[5],,.[J].,2004,43(6):281-282.