进出口粮谷中咪唑磺隆残留量检测方法 液相色谱法

中华人民共和国出入境检验检疫行业标准进出口粮谷中咪唑磺隆残留量检测方法液相色谱法Determinationofimazosulfuronr2007-04-06发布国家质量监督检验检疫总局进出口粮谷中咪唑磺隆残留量检测方法液相色谱法 (资料性附录)标准品色谱图图A.1咪唑磺隆标准品液相色谱图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(C₁H₃CIN,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