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An effective method for pesticide residues determination in tobacco by GC-MS/MS and UHPLC-MS/MS employing acetonitrile extraction with low-temperature precipitation and d-SPE clean-up

Author:
Bernardi, Gabrieli, Kemmerich, Magali, Ribeiro, Lucila C., Adaime, Martha B., Zanella, Renato, Prestes, Osmar D.
Source:
Talanta 2016 v.161 pp. 40-47
ISSN:
0039-9140
Subject:
acetonitrile, gas chromatography, isofenphos, pesticide residues, solid phase extraction, statistical analysis, tandem mass spectrometry, tobacco, ultra-performance liquid chromatography
Abstract:
An effective method has been developed and validated for the determination of residues of 55 pesticides in tobacco. The proposed sample preparation method is based on acetonitrile extraction, low-temperature precipitation (LTP) and dispersive solid phase extraction (d-SPE) clean-up. Gas chromatography and ultra-high performance liquid chromatography analysis, both coupled to tandem mass spectrometry (GC-MS/MS and UHPLC-MS/MS), were used for determination. LTP is easy to perform and was crucial to obtain a clean extract. Method quantification limit for the pesticides were between 25 and 75µgkg−1. Extraction recoveries obtained for blank samples spiked at 25, 75, 125 and 250µgkg−1 levels ranged from 63 to 161% with relative standard deviations (RSD)≤20%. The method was successfully applied to the analysis of thirteen different tobacco samples, providing to be a robust procedure for routine analysis. The compounds pirimiphos methyl and isofenphos presented residues in the range of 35–51µgkg−1.
Agid:
5566329