http://dx.doi.org/10.5935/sc.2018.001
Multiresidue determination of pesticides in sweet peppers by LC-MS/MS using Si-Al(PMTDS) as a sorbent for extraction by MSPD
Morais EHC et al.
Palavras-chave: liquid chromatography-tandem mass spectrometry; matrix solid phase dispersion; sweet peppers; pesticides; validation
Resumo: UA fast, effective and environmentally safe method for multiresidue determination of pesticides in samples of sweet green peppers using matrix solid phase dispersion with a new dispersant, poly(methyltetradecylsiloxane) thermally immobilized onto alumina coated silica, Si-Al(PMTDS), with determination by liquid chromatography coupled to tandem mass spectrometry was developed and validated. The performance of the new dispersant was compared with others, such as C18 and SiO
2. Acetonitrile and ethyl acetate were evaluated as extraction solvents. The Si-Al(PMTDS)-based sorbent gave results similar to the commercial sorbents tested in relation to recovery. However, only the lab-made polymeric sorbent assured selectivity of the separation. With Si-Al(PMTDS) extraction, recoveries for almost all analytes were in the range of 70-120% with coefficients of variation less than 20%, acceptable values for the analysis of pesticide residues in complex samples, demonstrating accuracy and precision of results for these analytes. All quantification limits were below the listed maximum residues limits for the analyzed pesticides. The developed method was applied to sweet green pepper samples, in which some authorized pesticides were found, but at concentration levels lower than the maximum residue limits. However, several unauthorized pesticides were also encountered. The preparation of the sorbent Si-Al(PMTDS) is simple, reproducible, and the cost is compatible with commercially available sorbents used in matrix solid phase dispersion.
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