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Optimization of Q u EC h ERS method for the analysis of organochlorine pesticides in soils with diverse organic matter
Author(s) -
CorreiaSá Luísa,
Fernandes Virgínia C.,
Carvalho Manuela,
Calhau Conceição,
Domingues Valentina F.,
DelerueMatos Cristina
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201200087
Subject(s) - quechers , chemistry , detection limit , gas chromatography/tandem mass spectrometry , soil water , chromatography , gas chromatography , gas chromatography–mass spectrometry , matrix (chemical analysis) , mass spectrometry , organic matter , residue (chemistry) , environmental chemistry , pesticide residue , pesticide , environmental science , soil science , agronomy , biology , biochemistry , organic chemistry
A QuEChERS method has been developed for the determination of 14 organochlorine pesticides in 14 soils from different Portuguese regions with wide range composition. The extracts were analysed by GC‐ECD (where GC‐ECD is gas chromatography‐electron‐capture detector) and confirmed by GC‐MS/MS (where MS/MS is tandem mass spectrometry). The organic matter content is a key factor in the process efficiency. An optimization was carried out according to soils organic carbon level, divided in two groups: HS (organic carbon >2.3%) and LS (organic carbon <2.3%). The method was validated through linearity, recovery, precision and accuracy studies. The quantification was carried out using a matrix‐matched calibration to minimize the existence of the matrix effect. Acceptable recoveries were obtained (70–120%) with a relative standard deviation of ≤16% for the three levels of contamination. The ranges of the limits of detection and of the limits of quantification in soils HS were from 3.42 to 23.77 μg kg −1 and from 11.41 to 79.23 μg kg −1 , respectively. For LS soils, the limits of detection ranged from 6.11 to 14.78 μg kg −1 and the limits of quantification from 20.37 to 49.27 μg kg −1 . In the 14 collected soil samples only one showed a residue of dieldrin (45.36 μg kg −1 ) above the limit of quantification. This methodology combines the advantages of QuEChERS, GC‐ECD detection and GC‐MS/MS confirmation producing a very rapid, sensitive and reliable procedure which can be applied in routine analytical laboratories.