title: High-performance liquid chromatographic determination of pesticides in tomatoes using laboratory-made NH2 and C18 solid-phase extraction materials.
abstract: A method for high-performance liquid chromatographic (HPLC) multiresidue determination of six pesticides in tomatoes was developed and validated. Silica-based C18 (octadecyl) and NH2 (aminopropyl) solid-phase extraction (SPE) sorbents, made in our laboratory, were used for sample preparation. The SPE materials were obtained by thermal immobilization of appropriate polysiloxanes onto 40 microm silica surfaces and were used in sample preparation for multiresidue analysis of the following pesticides: tebuthiuron and diuron (urea herbicides), simazine, atrazine and ametryn (triazines herbicides) and benomyl (benzimidazol fungicide). The results were compared with similar commercial materials. Reversed-phase high-performance liquid chromatography (RP-HPLC) using a Purospher RP-18 5 microm column and ACN: 0.01% aqueous NH4OH, pH 8.4 (35:65, v/v) as mobile phase, at 0.7 mlmin(-1), with 235 nm UV detection, was used for separation and quantification of the pesticides. Method validation was performed at three fortification levels (100, 200, 1000 microg l(-1)). Limits of detection and quantification show that the methods developed can be used to detect the pesticides in concentrations below the maximum residue levels (MRL) established by the Codex Alimentarius, USA, European Union and Brazilian legislations. The results showed that aminopropyl materials have a better performance than the octadecyl sorbents. Laboratory-made materials give results similar to commercial sorbents, with recoveries and precisions in agreement with directives for method validation in residue analysis.
authors.affiliation: School of Chemical Engineering, State University of Campinas, P.O. Box 6066, 13084-971 Campinas, SP, Brazil. lmelo@unicamp.br
authors.forename: Lucio F C
authors.initials: LF
authors.lastname: Melo
authors.forename: Carol H
authors.initials: CH
authors.lastname: Collins
authors.forename: Isabel C S F
authors.initials: IC
authors.lastname: Jardim
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation* / Q000379:methods; D018551:Solanum lycopersicum / Q000737:chemistry*; D010573:Pesticide Residues / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013056:Spectrophotometry, Ultraviolet
chemical_list: D010573:Pesticide Residues