Freitas Luciana Gomides, Götz Christian W, Ruff Matthias, Singer Heinz P, Müller Stephan R
Swiss Federal Institute for Environmental Science and Technology (EAWAG), Uberlandstrasse 133, CH-8600 Dübendorf, Switzerland.
J Chromatogr A. 2004 Mar 5;1028(2):277-86. doi: 10.1016/j.chroma.2003.11.094.
The LC/ESI/MSMS method allows the trace quantification (ng/l) of the new triketone herbicides, i.e. sulcotrione and mesotrione, and important herbicides and metabolites, in natural waters. Solid phase extraction (SPE) for sample enrichment is performed with OASIS (recoveries 94-112% for parent herbicides). Neutral and acidic compounds were analyzed separately with ESI in positive and negative mode, respectively. Quantification limits varied between 0.5 and 10 ng/l. The acidic herbicides detection was improved by a neutralizing post-column addition solution. The influence of ion suppression on quantification is discussed in detail. It is shown that we could overcome this problem and achieve reliable quantification using isotope labeled internal standards (ILIS) for every single analyte. The methods performance is illustrated with samples from a lake depth profile.
液相色谱/电喷雾串联质谱法可对天然水中的新型三酮类除草剂(即磺草酮和硝磺草酮)以及重要除草剂和代谢物进行痕量定量分析(纳克/升)。采用OASIS进行固相萃取(SPE)以富集样品(母体除草剂的回收率为94 - 112%)。中性和酸性化合物分别以正离子和负离子模式通过电喷雾电离(ESI)进行分析。定量限在0.5至10纳克/升之间。通过柱后添加中和溶液提高了酸性除草剂的检测效果。详细讨论了离子抑制对定量的影响。结果表明,我们可以通过为每种分析物使用同位素标记内标(ILIS)来克服这一问题并实现可靠的定量。通过湖泊深度剖面的样品说明了该方法的性能。