Development, validation and comparison of three methods of sample preparation used for identification and quantification of 2,4,6-trinitrotoluene and products of its degradation in sediments by GC-MS/MS

Abstract

Large amounts of ammunition were dumped in seas and oceans after World War II. After more than 70 years, these munitions still pose a threat to marine environments and humans. In this study, methods used for the analysis of 2,4,6-trinitrotoluene (TNT) and its degradation products from environmental samples were successfully developed, validated and compared. Three sample preparation techniques were selected: solid–liquid extraction, accelerated solvent extraction and Soxhlet extraction. Due to the short process time and lack of need to use complicated equipment, the method recommend for the analysis of explosives in bottom sediments is solid–liquid extraction. The detection (LOD) and quantification (LOQ) limits of TNT and its degradation products determined with GC-MS/MS range from 0.3 ng mL⁻¹ to 173.4 ng mL⁻¹. 4-Nitrotoluene is characterized by the lowest LOQ and LOD, respectively, of 0.9 ng mL⁻¹ and 0.3 ng mL⁻¹. The analyte recoveries of all compounds ranged from 64.6% to 91.8%, with good accuracies (from 96.7% to 103.1%) and good precision, expressed as the coefficient of variation (CV, from 2.1% to 6.4%).