AXYS Develops Hi Res Method for Pyrethroids in Sediment and Water

Pyrethroids, pyrethrins, and piperonyl butoxide in sediments by high-resolution gas chromatography/high-resolution mass spectrometry

Million B. Woudneh a,*, Daniel R. Oros b

a AXYS Analytical Services Ltd., 2045 Mills Road West, Sidney, B.C., Canada V8L 3S8b San Francisco Estuary Institute, 7770 Pardee Lane, 2nd Floor, Oakland, CA 94621, USA

Available at ScienceDirect.com

Abstract

A new method for determination of pyrethroids, pyrethrins, and piperonyl butoxide (PBO) by high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS) was developed for aquatic sediments. The method detection limits for pyrethroids (15 compounds), pyrethrins, and PBO ranged from 0.16 to 1.50 ng/g sediment, which was suitable for detecting these chemicals at environmentally relevant concentrations (low ng/L range) that are toxicologically significant to benthic organisms. Recovery of the analytes from a low level spiked sediment ranged from 89.7% to 135%. Resmethrin showed the lowest recovery at 23.5% and pyrethrins showed the highest recovery at 154%. To confirm the utility of this new method for environmental applications, sediment samples collected from five tributaries of the San Francisco Bay, California were analyzed. Individual pyrethroids were detected in concentrations of up to 17.6 ng/g, while PBO was detected in all sediment samples in concentrations of 0.010–0.215 ng/g. Pyrethrins were not found in the sediment samples.

© 2006 Elsevier B.V. All rights reserved.

 

Quantitative Determination of Pyrethroids, Pyrethrins, and Piperonyl Butoxide in Surface Water by High-Resolution Gas Chromatography/High-Resolution Mass Spectrometry

Million Bekele Woundneh*

AXYS Analytical Services Ltd., 2045 Mills Road West, Sidney, British Columbia V8L 3S8, Canada

Daniel Ray Oros

San Francisco Estuary Institute, 7770 Pardee Lane, 2nd Floor, Oakland, California 94621

Available at ACS Publications

Abstract

A new method for determination of pyrethroids, pyrethrins, and piperonyl butoxide (PBO) by highresolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS) was developed for surface water samples. The method is based on sampling 100 L of ambient surface water with a solid phase extraction (SPE) technique that uses both wound glass fiber filters for collecting the particulate-associated chemicals and XAD-2 resin for collecting the dissolved chemicals. The method detection limits of the analytes ranged from 0.58 to 8.16 ng/sample, which is equivalent to a detection limit range of 0.0058-0.082 ng/L for a 100 L water sample collected by the SPE technique. The SPE when coupled with HRGC/HRMS was a suitable match for detecting these chemicals at subnanogram per liter ranges that are toxicologically significant to aquatic organisms. To confirm the utility of this method for environmental applications, pyrethroids and PBO were found at subnanogram per liter concentrations in surface water samples collected from five tributaries (primarily urban creeks)of the San Francisco Bay, California.

© 2006 American Chemical Society