Krynitsky A J
U.S. Environmental Protection Agency, Analytical Chemistry Laboratory, Beltsville, MD 20705, USA.
J AOAC Int. 1997 Mar-Apr;80(2):392-400.
A capillary electrophoresis (CE) method and an electrospray ionization (ESI) liquid chromatography/mass spectrometry (LC/MS) confirmatory method were developed to analyze 12 sulfonylurea herbicides and one sulfonamide (Flumetsulam) in runoff water. The water used for fortification was collected from a local marsh that contained high levels of potentially interfering compounds. Good recoveries and adequate sensitivity at the 0.2 ppb level (limit of quantitation) were obtained. A portion of the water was acidified and extracted with reversed-phase solid-phase extraction (SPE). Extracts were cleaned up with a tandem system consisting of a strong-anion exchange SPE cartridge stacked on an alumina SPE cartridge. CE/ultraviolet quantitation was achieved by capillary zone electrophoresis at pH 4.75 with 50 mM ammonium acetate buffer and an acetonitrile modifier. ESI LC/MS quantitation was achieved by using a time-scheduled selective-ion monitoring (positive mode) of the M + H ions for each compound. The extraction/cleanup procedure provided extracts such that in-source collision-induced dissociation gave product ions for confirmation at the 0.2 ppb fortification level.
开发了一种毛细管电泳(CE)方法和一种电喷雾电离(ESI)液相色谱/质谱(LC/MS)确证方法,用于分析径流水中的12种磺酰脲类除草剂和1种磺酰胺(氟嘧磺隆)。用于加标的水取自当地一个含有高浓度潜在干扰化合物的沼泽。在0.2 ppb水平(定量限)获得了良好的回收率和足够的灵敏度。将一部分水样酸化,并用反相固相萃取(SPE)进行萃取。萃取物用串联系统净化,该系统由堆叠在氧化铝SPE柱上的强阴离子交换SPE柱组成。通过在pH 4.75下使用50 mM醋酸铵缓冲液和乙腈改性剂的毛细管区带电泳实现CE/紫外定量。ESI LC/MS定量通过对每种化合物的M + H离子进行定时选择性离子监测(正模式)来实现。萃取/净化程序提供的萃取物使得源内碰撞诱导解离产生产物离子,用于在0.2 ppb加标水平进行确证。