Glyphosate and AMPA Analysis in Sewage Sludge by LC-ESI-MS/MS after FMOC Derivatization on Strong Anion-Exchange Resin as Solid Support

详细信息    查看全文

• 作者：Aline Ghanem ; Philippe Bados ; Lucien Kerhoas ; Jacqueline Dubroca ; Jacques Einhorn
• 刊名：Analytical Chemistry
• 出版年：2007
• 出版时间：May 15, 2007
• 年：2007
• 卷：79
• 期：10
• 页码：3794 - 3801
• 全文大小：165K
• 年卷期：v.79,no.10(May 15, 2007)
• ISSN：1520-6882

文摘

An innovative analytical method has been developed forthe determination of glyphosate and aminomethylphosphonic acid (AMPA), its major metabolite, in sewagesludge. This method involved an alkaline extraction fromsludge and purification on a strong anion-exchange resin.While the analytes remained fixed by ionic interactions,an "on-solid support" derivatization by FMOC-Cl wascarried out. This versatile approach allowed a 10 minreaction and simple elimination of the excess of reagent.The resulting derivatives remained retained by ionic andhydrophobic interactions with the resin until being elutedby a mixed NaCl water/acetonitrile, 70/30, v/v, solution.After an appropriate dilution and adjustment of the pH,the sample was concentrated on an Oasis HLB solid-phase cartridge. For quality analysis of traces in complexmatrixes, LC-ESI-MS/MS in the multiple reaction monitoring positive mode was used fulfilling the EuropeanUnion requirements (Decision 2002/657/CE). To overcome the matrix effects, stable isotopically labeled standards were added to the sludge extracts as internalstandards and were thus derivatized during the procedurein parallel to the analytes. Mean recovery values were 70%± 7% for glyphosate and 63% ± 3% for AMPA. Limits ofdetection (20 and 30 ppb dw) and limits of quantification(35 and 50 ppb dw) for glyphosate and AMPA, respectively, were sufficient to monitor samples taken from Ile-de-France wastewater treatment plants where contamination currently reached 0.1-3 ppm and 2-35 ppm dwfor glyphosate and AMPA, respectively.