Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimioupolis Zografou, 157 71 Athens, Greece.
J Am Soc Mass Spectrom. 2011 Oct;22(10):1826-38. doi: 10.1007/s13361-011-0191-z. Epub 2011 Jul 6.
A systematic and detailed optimization strategy for the development of atmospheric pressure ionization (API) LC-MS/MS methods for the determination of Irgarol 1051, Diuron, and their degradation products (M1, DCPMU, DCPU, and DCA) in water, sediment, and mussel is described. Experimental design was applied for the optimization of the ion sources parameters. Comparison of ESI and APCI was performed in positive- and negative-ion mode, and the effect of the mobile phase on ionization was studied for both techniques. Special attention was drawn to the ionization of DCA, which presents particular difficulty in API techniques. Satisfactory ionization of this small molecule is achieved only with ESI positive-ion mode using acetonitrile in the mobile phase; the instrumental detection limit is 0.11 ng/mL. Signal suppression was qualitatively estimated by using purified and non-purified samples. The sample preparation for sediments and mussels is direct and simple, comprising only solvent extraction. Mean recoveries ranged from 71% to 110%, and the corresponding (%) RSDs ranged between 4.1 and 14%. The method limits of detection ranged between 0.6 and 3.5 ng/g for sediment and mussel and from 1.3 to 1.8 ng/L for sea water. The method was applied to sea water, marine sediment, and mussels, which were obtained from marinas in Attiki, Greece. Ion ratio confirmation was used for the identification of the compounds.
描述了一种系统而详细的优化策略，用于开发大气压电离（API）LC-MS/MS 方法，以测定水中、沉积物中和贻贝中的 Irgarol 1051、敌草隆及其降解产物（M1、DCPMU、DCPU 和 DCA）。实验设计用于优化离子源参数。在正离子和负离子模式下比较了 ESI 和 APCI，并研究了两种技术中流动相对离子化的影响。特别关注 DCA 的离子化，它在 API 技术中存在特殊困难。只有在 ESI 正离子模式下使用流动相中的乙腈，才能实现这种小分子的满意离子化；仪器检测限为 0.11ng/mL。通过使用纯化和非纯化样品定性估计了信号抑制。沉积物和贻贝的样品制备直接而简单，仅包括溶剂萃取。平均回收率在 71%至 110%之间，相应的（%）RSD 在 4.1%至 14%之间。沉积物和贻贝的方法检测限范围在 0.6 至 3.5ng/g 之间，海水的方法检测限范围在 1.3 至 1.8ng/L 之间。该方法应用于来自希腊阿提卡地区码头的海水、海洋沉积物和贻贝。离子比确认用于鉴定化合物。
