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Determination of trace levels of aquaculture chemotherapeutants in seawater samples by SPME‐GC‐MS/MS
Author(s) -
GarcíaRodríguez Diego,
Carro Antonia M.,
Lorenzo Rosa A.,
Fernández Fátima,
Cela Rafael
Publication year - 2008
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.200800268
Subject(s) - chromatography , chemistry , extraction (chemistry) , detection limit , seawater , sample preparation , solid phase microextraction , quechers , gas chromatography–mass spectrometry , mass spectrometry , pesticide residue , pesticide , oceanography , agronomy , biology , geology
A sensitive and efficient solid‐phase microextraction (SPME) method for the determination of organophosphorous (OPPs) and pyrethroid pesticides (Pyrs) in aquaculture‐seawater samples by using GC with MS/MS (GC‐MS/MS) was developed. Dichlorvos and chlorpyrifos (OPPs); permethrin, α‐cypermethrin and deltamethrin (Pyrs) were selected according to their use as chemotherapeutants in the aquaculture industry. Different parameters affecting extraction efficiency such as fibre coating, agitation, pH and extraction time profiles were investigated. An experimental central composite design (α = 1) and desirability functions were used for the simultaneous optimization of extraction temperature and sample volume. Finally, a method based on direct SPME in 40 min at 75°C using 100‐μm‐thick poly(dimethyl)siloxane (PDMS) fibre and 20 mL of sample volume is proposed. The method was validated, exhibiting good linearity, precision and accuracy parameters with picogram per millilitre LODs. The proposed methodology was applied to determine the ultratrace levels of OPPs and Pyrs in aquaculture‐seawater samples by the standard addition approach, which proved to be reliable and sensitive, in addition to requiring only small amounts of sample.