中華人民共和國出入境檢驗檢疫行業標準進出口糧谷中咪唑磺隆殘留量檢測方法液相色譜法Determinationofimazosulfuronr2007-04-06發布國家質量監督檢驗檢疫總局進出口糧谷中咪唑磺隆殘留量檢測方法液相色譜法 (資料性附錄)標準品色譜圖圖A.1咪唑磺隆標準品液相色譜圖Determinationofimazforimportandexport—LiquidchromatoThisstandardspecifiesthemethodsofsamplepThisstandardisapplicabletothedTheimazosulfuronresiduewereextractedwithdichloromethane,acbyCnSPEcolumn.determinatedbyHPLCwithUhlessotherwisespeclfied,allreagentsusedshouldbeanalyticall2.2.51mol/LAmmonia;Pipet2.2.6CSPEcolumn:3mL/200mg,condition2.2.7Extractsolvent:Dichloromethane+Acetonitrile+1mol/LAmmonia(4+15+1.V/V/V).2.2.8Eluant;Methanol+water(1+1,V2.2.9Imazosulfuronstandard(C?H?CIN,O,S,CA:122548-33-8):Purity>99%.2.2.10Imazosulfuranstandardsolutian:Weighappropriateimazosulfandprepareasolutionof100rg/mLstocksolutiontotherequiredconcentrationasthestandard2.3.1HPLC;EquippedwithUV-d2.3.4Nitrogenevaporat2.3.5SolidphaseReducethesampletoca1kgbyquamixthoroughlyanddivideThetestsampleshallbestoredbelowration.precautionmustbetakentoaviodcontamisalvent(2.2,7),Itwascoverdandshakedfor30merlenmeyerflake.Repeatedaboveoperation.Then.thanetothesameerlenmeyerflake,Rotaryevaporatethresicueswith4mLacetonitrile,tranfertoTransferabovesolutiontothecartridge.Washcartridgewith5(2.2.8)tocartridge,rotaryevaporatetheelutionliquidat40Accordingtotheexperimentaldata,thefortifying0.50mg/kg,and