Multiresidue screening of endocrine-disrupting chemicals and pharmaceuticals in aqueous samples by multi-stir bar sorptive extraction–single desorption–capillary gas chromatography/mass spectrometry

Abstract

A multiresidue method for screening endocrine-disrupting chemicals (EDCs) and pharmaceuticals in aqueous samples is presented. Four 10-mL aliquots of water were taken for stir bar sorptive extraction (SBSE) and they were treated in the following way. In sample one, in situ derivatization was performed with acetic acid anhydride to improve the extraction efficiencies and chromatographic analysis of phenolic compounds. For the same reasons, aliquot two was treated with ethyl chloroformate to improve amine and acid extraction and analysis, and aliquot three with tetraethylborate to enhance organotin compound extraction and analysis. Methanol was added to sample four to stop adsorption of apolar solutes on the wall. After SBSE, the four stir bars, together with a plug of glass wool impregnated with bis(trimethylylsilyl)trifluoroacetamide (BSTFA) to derivatize hydroxyl functionalities, were introduced into the same thermal desorption tube, heat-desorbed, and analyzed simultaneously by capillary GC/MS. The figures of merit of the method were evaluated with an EDC model mixture. In scan-mode MS, the limits of detection (LODs) were in the range 1-500 ng/L, while the LODs dropped by a factor of 50-100 when ion monitoring MS was applied to the targets. The performance of the method was illustrated by analysing some real-world water samples.

An overview of sample preparation and extraction of synthetic pyrethroids from water, sediment and soil

“…A comprehensive review on stir bar sorptive extraction has been published [140], in which practical aspects and applications of SBSE were discussed. Low recoveries for highly apolar compounds such as polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) were observed with SPME and SBSE due to adsorption on glass walls [141][142][143][144] and because pyrethroids exhibit log K ow values larger than 5.6, similar behavior could be expected. Hence, optimization of an SBSE method for extraction of pyrethroids must take into account the high affinity of pyrethroids to adsorb onto surfaces of extraction apparatus.…”

Development of a molecularly imprinted polymer for selective extraction of bisphenol A in water samples

“…The multishot approach [17] was adopted because it enables to analyze all model EDCs investigated in the present study simultaneously with good recoveries.…”

Development of a functionalized polymeric ionic liquid monolith for solid-phase microextraction of polar endocrine disrupting chemicals in aqueous samples coupled to high-performance liquid chromatography

“…A number of sample preparation techniques including solid-phase extraction (SPE) [15], magnetic molecularly imprinted polymers extraction [16], stir bar sorptive extraction [17][18][19], liquid-phase microextraction (LPME) [20,21], SPME [22][23][24], etc. have been proved to be efficient for the determination of EDCs in aquatic environment systems.…”