進(jìn)出口糧谷中咪唑磺隆殘留量檢測方法 液相色譜法

中華人民共和國出入境檢驗(yàn)檢疫行業(yè)標(biāo)準(zhǔn)進(jìn)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(fā)布國家質(zhì)量監(jiān)督檢驗(yàn)檢疫總局進(jìn)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(biāo)準(zhǔn)品色譜圖圖A.1咪唑磺隆標(biāo)準(zhǔn)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