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Optimization of matrix solid‐phase dispersion conditions for organic fungicides determination in soil samples
Author(s) -
Carpinteiro Inmaculada,
Casado Jorge,
Rodríguez Isaac,
Ramil María,
Cela Rafael
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.201101036
Subject(s) - solid phase extraction , extraction (chemistry) , matrix (chemical analysis) , chromatography , soil water , chemistry , detection limit , dispersion (optics) , analytical chemistry (journal) , sample preparation , gas chromatography–mass spectrometry , gas chromatography , solid phase microextraction , soil test , analyte , vineyard , standard solution , polypropylene , standard addition , mass spectrometry , environmental science , soil science , physics , organic chemistry , optics , history , archaeology
A simplified sample preparation method, based on the matrix solid‐phase dispersion technique, is proposed for the sensitive determination of 15 organic fungicides in vineyard soils by gas chromatography–mass spectrometry ( GC – MS ). Under final working conditions, sieved samples (0.5 g) were blended and dispersed with 2 g of C 18 and transferred to a polypropylene syringe containing 1 g of diatomaceous earth. Analytes were recovered using 10 m L of ethyl acetate, this extract was concentrated to 1 m L and fungicides determined by GC – MS , without additional cleanup. The method provided recoveries in the range from 74 to 122% for soils with total carbon contents up to 5.5% and it allowed the use of external standard as quantification technique. Inter‐day precision, given as relative standard deviations, stayed between 3 and 13%, and the limits of quantification were comprised between 0.6 and 15 ng g −1 . Several fungicides were found in the top layer of vineyard soils with the highest detection frequency and maximum concentration corresponding to iprovalicarb. Some real samples were also submitted to pressurized liquid extraction. Measured concentrations were in excellent agreement with those obtained by matrix solid‐phase dispersion, which reinforces the accuracy of the latter methodology.