Multiresidue determination of 11 new fungicides in grapes and wines by liquid–liquid extraction/clean-up and programmable temperature vaporization injection with analyte protectants/gas chromatography/ion trap mass spectrometry Rosa M. González-Rodríguez, Beatriz Cancho-Grande and Jesús Simal-GándaraJournal of Chromatography AVolume 1216, Issue 32, 7 August 2009, Pages 6033-6042 AbstractA gas chromatographic ion trap mass spectrometry (GC-ITMS) method was developed for the determination of 11 new generation fungicides (benalaxyl, benalaxyl-M, boscalid, cyazofamid, famoxadone, fenamidone, fluquinconazole, iprovalicarb, pyraclostrobin, trifloxystrobin and zoxamide) in grapes and wines. Samples were extracted with ethyl acetate:hexane (1:1, v/v) and cleaned-up with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. The addition of analyte protectants (3-ethoxy-1,2-propanediol, d-sorbitol and l-gulonic acid γ-lactone) in the final extracts allowed to avoid the matrix-induced response enhancement effect on quantitation process with absolute recoveries ca. 100%. Precision (expressed as relative standard deviation) was lower than 16% for all fungicides. Limits of detection and quantitation were lower than 0.01 mg/kg or mg/L, except for cyazofamid, much smaller in all cases than maximum residue levels (MRLs) established by European Union for grapes and by Switzerland and Italy for wines. The proposed method was applied to determine fungicide residues in three different white grapes for vinification produced in Ribeiro area in Galicia (NW Spain), as well as in their corresponding final wines.

我是用乙腈提取，然后过活性炭和氨基小柱，先用丙酮淋洗，然后丙酮和正己烷过柱，接收，甲氧基丙烯酸酯中醚菌酯和烯肟菌酯的回收效果都很好，就是唑菌胺酯出不来，回收率几乎很低，我现在是做醚菌酯和烯肟菌酯以及唑菌胺酯的多残留。按照《气相色谱质谱法测定甲氧烯丙烯酸酯》的那个方法做，也是唑菌胺酯提取不出来，我现在没有凝胶色谱。主要是过spe小柱的方法，现在不知道唑菌胺酯哪里出了问题。请高手指导