Development of a solid phase extraction method for agricultural pesticides in large-volume water samples

An analytical method using solid phase extraction (SPE) and analysis by gas chromatography/mass spectrometry (GC–MS) was developed to determine trace levels of a variety of 41 agricultural pesticides and selected transformation products in high-elevation surface waters. Large-volume water sampling (up to 100 L) was employed because it was anticipated that pesticide contamination, if present, would be at very low levels. The target compounds comprise pesticides (and selected oxygen transformation products) known to have been extensively used in agriculture in the San Joaquin Valley, CA, USA. Solid phase extraction using the polymeric resin Abselut Nexus was optimized to extract the pesticide analytes from water samples. A single determinative method using GC–MS with electron ionization was used for all the analytes. Recoveries from 100 L of reagent water at 100 pg/L and 1 ng/L concentrations were generally greater than 75%, although dimethoate, disulfoton, and phorate were not recovered. Analysis of the extracts without cleanup yielded detection limits for the remaining 38 analytes between 0.1 and 30 ng/L. A silica cleanup with separate analysis of 3 eluant fractions improved detection limits for 37 of the compounds to between 6 and 600 pg/L in high-elevation surface waters.