Acceptance Criteria for Ultratrace HPLC−Tandem Mass Spectrometry: Quantitative and Qualitative Determination of Sulfonylurea Herbicides in Soil

Abstract

Eight commonly used sulfonylureas (SUs: nicosulfuron, thifensulfuron methyl, metsulfuron methyl, sulfometuron methyl, chlorsulfuron, bensulfuron methyl, tribenuron methyl, and chlorimuron methyl) and deuterium-labeled nicosulfuron (nicosulfuron-d(6)), used as an internal standard, were isolated from soil by solvent extraction and identified under quantitative and qualitative ion spray LC/MS/MS conditions using the selected reaction monitoring (SRM) mode of acquisition. The lower level of quantitation for these SUs in soil was determined at the 0.05 ppb level using a TurboIonSpray adapted LC/MS interface without a precolumn split and optimizing MS/MS tuning conditions for individual SUs. The eight SUs were qualitatively identified and quantitatively determined in soil. The standard curve for each SU was linear from 0.05 to 10 ppb. This SRM LC/MS method demonstrates high sensitivity and high specificity for these SUs in soil and shows at least a 400-fold improvement in sensitivity over previous reports. Acceptance criteria for forensically valid data are suggested for qualitative SRM LC/MS experiments. These include HPLC retention time reproducibility (±2%), at least two and preferably three precursor-product ions selected, and relative abundance criteria for selected ions (±20% absolute).