Determination of Triazine Herbicides and Diuron in Mud from Olive Washing Devices and Soils Using Gas Chromatography with Selective Detectors

• Published in: Analytical letters 2006-04, Vol.39 (4), p.835-850
• Main Authors: Rubio, M. Guardia, Font, V. Banegas, Díaz, A. Molina, Cañada, M. J. Ayora
• Format: Article
• Language: English
• Subjects: atrazine; diuron; liquid-solid extraction; simazine; Simultaneous detection; terbuthylazine; terbutrin
• ISSN: 0003-2719; 1532-236X
• DOI: 10.1080/00032710600611608

In the present work, a method for the simultaneous determination of five herbicides, diuron, simazine, atrazine, terbuthylazine and terbutryn by GC-electron capture detection (ECD) and GC-thermoionic specific detector (TSD) in soil and mud samples (from olives washing devices) has been developed. Extraction of the herbicides from soil samples was carried out by liquid-solid extraction with ciclohexane/acetone under sonication. In addition, a clean-up step by solid phase extraction (SPE) using alumina was necessary for mud samples to remove fat residues in the extracts. Spiked soil standards were used for calibration. Limit of detection (LOD) values ranged between 0.2-1.4 ng g −1 and limit of quantitation (LOQ) between 1.4-2.0 ng g −1 . The precision of the method was satisfactory for all the herbicides analyzed, with RSD values ranging between 7.5%-32.3% and 8.5%-17.8% for 10 and 100 ng g −1 spiking levels, respectively. The accuracy of the method was checked at three spiking levels (10, 50, and 100 ng g −1 ) with recovery values ranging from 74.2%-129.1%. In the case of mud samples, mean recovery values (100 ng g −1 spiking level) were acceptable for diuron (69.5%) and more satisfactory in the case of triazine herbicides (81.0%-123.0%). Diuron and terbuthylazine were the herbicides most frequently detected in the analyzed samples.