Multi-residue analysis of N-methylcarbamate pesticides and their hydrolytic metabolites in environmental waters by use of solid-phase extraction and micellar electrokinetic chromatography A method for the simultaneous separation and determination of N-methylcarbamate pesticides and their hydrolytic
Multi-residue analysis of pesticide residues in mangoes using solid-phase microextraction coupled to liquid chromatography and UV–Vis detection
✍ Scribed by Adalberto M. Filho; Fábio N. dos Santos; Pedro A. de Paula Pereira
- Publisher
- John Wiley and Sons
- Year
- 2011
- Tongue
- English
- Weight
- 139 KB
- Volume
- 34
- Category
- Article
- ISSN
- 1615-9306
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✦ Synopsis
Abstract
A sensitive and efficient solid‐phase microextraction method, based on liquid chromatography and UV–Vis detection, was developed and validated as an alternative method for sample screening prior to LC‐MS analysis. It enables the simultaneous determination of ten pesticides in mango fruits. The fiber used was polydimethylsiloxane while optimum SPME conditions employed have been developed and optimized in a previous work. The desorption process was performed in static mode, using acetonitrile as a solvent. The results indicate that the DI‐SPME/HPLC/UV–Vis procedure resulted in good linear range, accuracy, precision and sensibility and is adequate for analyzing pesticide residues in mango fruits. The limits of detection (0.6–3.3 μg/kg) and quantification (2.0–10.0 μg/kg) were achieved with values lower than the maximum residue levels (MRLs) established by Brazilian legislation for all pesticides in this study. The average recovery rates obtained for each pesticide ranged from 71.6 to 104.3% at three fortification levels, with the relative standard deviation ranging from 4.3 to 18.6%. The proposed method was applied for the determination of the aforementioned compounds in commercial mango samples and residues of azoxystrobin, fenthion, permethrin, abamectin and bifenthrin were detected in the mango samples, although below the MRLs established by Brazilian legislation.
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An on-line technique coupling preconcentration via a microprecolumn Ž . with microcolumn-liquid chromatography micro-LC on a 1-mm inner diameter Ž . i.d. analytical column was investigated. The system was found to be very simple, fast, and efficient for the trace-level determination of some natural