PH12 Analytical Environmental Chemistry of POPs
Exhibit Hall
8:00 AM - Thursday, 13 November 2003
(PH129) New Method for the Rapid Determination of Triazine Herbicides and Irgarol 1051 in Soils and Sediment by ASE-SPE-GC/MS.
Wu, J1, Gardinali, P1, 1 Florida International University, Department Chemistry/SERC, Miami, Florida, USA
ABSTRACT- A simple multiresidue method has been developed for the determination of common triazine based herbicides and Irgarol1051, a new boosting agent in antifouling paints, in sediment and soil samples. The herbicides studied were: atraton, simazine, atrazine, propazine, terbuthylazine, simetryne, ametryne, prometryne and terbutryne. The analytes are directly extracted from unproccessed sediments using Accelerated Solvent Extraction (ASE) with a mixture methanol/water mixture (90:10) at 100oC and 1500 psi. Upon removal of the methanol, the reconstituted water based extracts (50ml) are loaded onto 300mg preconditioned Oasis HLB cartridges to concentrate the analytes. The herbicides are then eluted with 10 ml of methylene chloride and, upon solvent reduction, are analyzed by GC/MS in selected ion monitoring (SIM) mode using Atrazine-d5 as the internal standard. Recovery of fortified samples were in excess of 86% (RSDs < 9%) for all analytes and above 60% (RSDs <12) for M1(Irgarol 1051 major metabolite). Since no sample drying is required, typical detection limits range in the low parts per billion (1 -2 ng/g) for a 40g sample. The method was tested for the analysis of sediment and soil samples from South Florida environments including Everglades National Park, Biscayne Bay and the FKNMS. Besides low concentrations of common herbicides such as atrazine and ametryne, the most significant detection was of IRGAROL 1051. The antifoluant was detected in samples collected at the Miami River, Coconut Grove Marina, and Port Largo (Key largo) at concentration levels ranging from 1.32 to 31.3ng/g. To the authors knowledge this is the first report of IRAGROL 1051 in sediments from US coastal areas since its registration in 1998.
Key words: ASE, triazine herbicides, irgarol 1051, sediments, South Florida