Abstract
Previously published methods for the analysis of metaldehyde were adapted for its reliable quantification in soil extracts. Varied methanol-water extraction solvents were trialed, but the use of pure methanol proved to be the most reliable approach for the scaled down methodology. Analysis of metaldehyde was done using LC-MS. Initially the method had problems with matrix suppression of the signal. The method was therefore further developed to overcome this challenge to avoid the costs and time demands of laborious clean-up protocols. This modification to the method involved use of the BEH Phenyl column instead of the C18 column initially used, and optimization of the gradient flow of the mobile phase. The optimized LC-MS method was validated and used for further research applications. In brief,•We investigated the recovery of metaldehyde from spiked soil samples.•The optimized LC-MS method achieved acceptable metaldehyde recoveries (100–132%, 109% on average) for a range of soil types.•The optimized method was suitable for high through-put analyzes.
Highlights
Method ArticleAnalytical method development and validation for the quantification of metaldehyde in soil
Previously published methods for the analysis of metaldehyde were adapted for its reliable quantification in soil extracts
We investigated the recovery of metaldehyde from spiked soil samples
Summary
Analytical method development and validation for the quantification of metaldehyde in soil. Extraction of metaldehyde comprised the addition of methanol (100 ml, analytical grade from Sigma Aldrich), shaking the containers at 200 rpm for 30 min on a side-to-side shaker, followed by centrifuging (Beckman Coulter, Allegra) for 5 min at 3500 rpm and decanting the supernatant into a centrifuge tube This process was repeated in a second extraction using methanol (50 ml) and the second extract was stored separately. The samples were spiked with metaldehyde at two fortification levels (1.5 and 0.15 mg kg soil−1), thoroughly mixed with a spatula, and extracted with 25 ml methanol on a side-to-side shaker (200 rpm for 30 min), centrifuged (5 min at 3500 rpm) and the supernatant poured off and stored in a vial (Extract A) This process was repeated for a second sequential extraction (extract B). Further validation samples were produced at a one-hundredth dose (0.015 mg kg−1), to test the limits of detection
Sign-in/Register to view highlights & summary Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have
Schedule a callDisclaimer: All third-party content on this website/platform is and will remain the property of their respective owners and is provided on "as is" basis without any warranties, express or implied. Use of third-party content does not indicate any affiliation, sponsorship with or endorsement by them. Any references to third-party content is to identify the corresponding services and shall be considered fair use under The CopyrightLaw.
