title: 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.
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-1levels 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.
authors: Laboratory of Pesticide Residue Analysis (LARP), Chemistry Department, Federal University of Santa Maria, Santa Maria, RS, 97105-900 Brazil.
authors: Gabrieli
authors: G
authors: Bernardi
authors: Laboratory of Pesticide Residue Analysis (LARP), Chemistry Department, Federal University of Santa Maria, Santa Maria, RS, 97105-900 Brazil.
authors: Magali
authors: M
authors: Kemmerich
authors: Laboratory of Pesticide Residue Analysis (LARP), Chemistry Department, Federal University of Santa Maria, Santa Maria, RS, 97105-900 Brazil.
authors: Lucila C
authors: LC
authors: Ribeiro
authors: Laboratory of Pesticide Residue Analysis (LARP), Chemistry Department, Federal University of Santa Maria, Santa Maria, RS, 97105-900 Brazil.
authors: Martha B
authors: MB
authors: Adaime
authors: Laboratory of Pesticide Residue Analysis (LARP), Chemistry Department, Federal University of Santa Maria, Santa Maria, RS, 97105-900 Brazil.
authors: Renato
authors: R
authors: Zanella
authors: Laboratory of Pesticide Residue Analysis (LARP), Chemistry Department, Federal University of Santa Maria, Santa Maria, RS, 97105-900 Brazil. Electronic address: osmar.prestes@ufsm.br.
authors: Osmar D
authors: OD
authors: Prestes
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D011232:Chemical Precipitation; D002853:Chromatography, Liquid; D008401:Gas Chromatography-Mass Spectrometry; D010573:Pesticide Residues / Q000032:analysis*; D053719:Tandem Mass Spectrometry; D013696:Temperature; D014026:Nicotiana / Q000737:chemistry*
chemical_list: D000097:Acetonitriles; D010573:Pesticide Residues; C032159:acetonitrile
keywords: Chromatography; Pesticides; Sample preparation; Tobacco