Optimisation of the headspace‐solid phase microextraction for organomercury and organotin compound determination in sediment and biota

Abstract

Headspace solid-phase microextraction was optimised for the simultaneous preconcentration of methylmercury (MeHg+), monobutyltin, dibutyltin, tributyltin, monophenyltin (MPhT), diphenyltin (DPhT), and triphenyltin (TPhT) from sediments and biota. Extraction time (3-24 min), extraction temperature (20-90 degrees C), desorption time (1-10.4 min), desorption temperature (152-260 degrees C), and sample volume (5-22 mL) were simultaneously optimised, while variables such as fibre type (30 microm polydimethylsiloxane, PDMS), pH (acetic acid/sodium acetate, HOAc/NaOAc, 2 mol/L, pH approximately 4.8), the concentration of the derivatisation agent (sodium tetraethylborate, NaBEt4, 0.1% m/v), and the ionic strength (fixed by the buffer solution) were kept constant. The variables were optimised according to the experiments proposed by the MultiSimplex program and the responses were considered in order to establish the optimum conditions. The repeatability (relative standard deviation, RSD, 5-20.6%) and limits of detection (LODs, 0.05-0.97 ng/g) of the overall method were also estimated. The lowest precisions were obtained for DPhT and TPhT. The optimised preconcentration method was applied to the determination of MeHg+), butyl- and phenyltins in certified reference materials (IAEA-405 MeHg+) in estuarine sediment, BCR-646 butyl- and phenyltins in marine sediment, BCR-463 MeHg+ in tuna fish, DOLT-2 MeHg+ in dogfish liver, and BCR-477 butyltins in mussel tissue) by GC with microwave-induced plasma/atomic-emission detection.

Cold vapor-solid phase microextraction using amalgamation in different Pd-based substrates combined with direct thermal desorption in a modified absorption cell for the determination of Hg by atomic absorption spectrometry

“…Different procedures have been developed for the determination of organometallic and inorganic compounds of tin, mercury, selenium, arsenic, lead, manganese and other metals [20][21][22][23][24][25][26][27][28][29][30][31]. Mercury is one of the most toxic elements impacting on human and ecosystem health and therefore is one of the most studied environmental pollutants.…”

MultiSimplex optimization of chromatographic separation and dansyl derivatization conditions in the ultra performance liquid chromatography–tandem mass spectrometry analysis of risperidone, 9-hydroxyrisperidone, monoamine and amino acid neurotransmitters in human urine

“…It is easy to follow and has been used in several analytical applications [6,7]. The aim of this work was to further optimize the factors affecting chromatographic separation and dansyl derivatization by MultiSimplex, and to apply the method for simultaneous measurement of RIP, 9-OH-RIP and the NTs in human urine samples.…”

Fast and effective low‐temperature freezing extraction technique to determine organotin compounds in edible vegetable oil

“…Numerous studies have been reported for the determination of organotin compounds in sediment , bodily fluids , seawater , and marine biota samples . Little has been reported so far on tin speciation in different kinds of edible vegetable oils.…”