Fast and simultaneous determination of tin and mercury species using SPME, multicapillary gas chromatography and MIP-AES detection

Botana, Jorge; Rodil, Rosario; Díaz, Antonia María Carro; Ferreira, Ronise; Cela, R.; Pereiro, Isaac Rodríguez

doi:10.1039/b202362h

Cited by 31 publications

(4 citation statements)

References 15 publications

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“…Methylmercury (MeHg + ) and organotins (OTs) are some of the most analysed organometallic compounds due to their toxicity and ubiquity in the environment [1]. While OTs have an anthropogenic source due to their past and present use as catalysts, stabilisers in plastics, wood preservatives, and biocides [2], MeHg + may be formed in the environment by methylation of elemental and ionic mercury in biological processes [3].…”

Section: Introductionmentioning

confidence: 99%

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

Delgado¹,

Usobiaga

Prieto

et al. 2008

J of Separation Science

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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.

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Section: Introductionmentioning

confidence: 99%

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

Delgado¹,

Usobiaga

Prieto

et al. 2008

J of Separation Science

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“…[13][14][15][16] In order to avoid some drawbacks inherent in the use of chromatographic separations (i.e., peak tailing, potential decomposition risks), several strategies have been tried, such as capillary cold trap coupled with microwave induced plasma atomic emission spectrometry (MIP-AES), 17 pervaporation coupled to AAS 18 and flow injection-cold vapor-AAS. 7 Solid phase microextraction (SPME) is an ecofriendly analytical separation/preconcentration method, which has been employed for methylmercury determination by gas chromatographyatomic absorption spectrometry, 19,20 GC-MS, 21,22 GC-ICP-MS, 23 GC-AFS, 24 GC-MIP [25][26][27] and GC-cold vapor-AFS. 28 Recently, methods based on the direct coupling of SPME and a specific detector for several organometallics, including methylmercury, have been reported.…”

Section: Introductionmentioning

confidence: 99%

Direct coupling of solid phase microextraction and quartz tube-atomic absorption spectrometry for selective and sensitive determination of methylmercury in seafood: an assessment of chloride and hydride generation

Fragueiro

Lavilla

Bendicho

2004

J. Anal. At. Spectrom.

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The direct coupling between headspace solid phase microextraction and quartz tube-atomic absorption spectrometry detection has been evaluated for speciation of methylmercury in seafood after volatilization of its hydride or chloride derivative. Following variable optimisation in both procedures, a critical influence of the fibre sorbent material was observed. Liquid-phase coatings such as polydimethylsiloxane (PDMS) and 'solid' phase coatings such as polydimethylsiloxane-divinylbenzene (PDMS/DVB) or fused silica were compared. Best LODs were provided by the silica fibre for CH 3 HgH (0.4 ng mL 21 ) and by the PDMS/DVB fibre for CH 3 HgCl (0.06 ng mL 21 ). In general, repeatability was about 6% for the preconcentration of both Hg derivatives in the different fibre coatings. The affinity to sorption of CH 3 HgH was slightly improved when using silica fibres loaded with L-cysteine or palladium nitrate. Sorption/desorption studies with fused silica fibres allowed us to hypothesise that CH 3 HgH formed upon reaction of MeHg 1 with NaBH 4 -NaOH suffered from decomposition onto the fibre to yield Hg 0 like direct reaction between Hg 21 and NaBH 4 -NaOH. Generation of the chloride derivative showed an enhanced selectivity as compared with generation of the hydride. Nevertheless, experimental evidence of decomposition of the chloride derivative upon heating is also given. For methylmercury determination in seafood, hydride or chloride generation and headspace SPME were applied after ultrasound assisted extraction of methylmercury in 2 mol dm 23 HCl. Validation was carried out against CRM DORM-2 (dogfish muscle) and CRM 464 (Tuna fish), demonstrating good trueness of the methods proposed. A better LOD of MeHg 1 is obtained as compared with other SPME couplings described in the literature.

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“…The fiber was immersed for 30 min in the sample solution with constant stirring to assure proper extraction of the analytes. It is reported that organotins can also be analyzed in the presence of other metals [15,21,24,26,29,32,35,37,38,49].…”

Section: Organotin Compoundsmentioning

confidence: 99%

“…sample volume, NaBPh 4 volume, pH, sorption time, extraction-derivatization temperature, and rate of stirring were studied for optimization of the experimental conditions. Carpinteiro et al [49] described a rapid and accurate method for simultaneous determination of MeHg + , Hg 2+ , monobutyltin (MBT), tributyltin (DBT), and tributyltin (TBT) in water samples by using a multicapillary GC column and MIP-AES detection. The samples are derivatized by ethylation and extracted by SPME.…”

Section: Organomercury Compoundsmentioning

confidence: 99%

Applications of solid phase microextraction for the determination of metallic and organometallic species

Kaur

Malik²,

Verma

2006

J. Sep. Sci.

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Applications of solid phase microextraction for the determination of metallic and organometallic speciesThis paper reviews recent developments of solid phase microextraction (SPME) and its application to the analysis of organometallic species of lead, arsenic, mercury, tin, and selenium by hyphenation with HPLC-GC-atomic spectrometry. In the first part, a background of the technique is given in terms of derivatization, fibers used, extraction and desorption conditions. The second part summarizes typical SPME applications to the determination of organometallic species and the main experimental conditions with the aid of specific examples. Most of the applications comprise alkylation with NaBEt 4 and headspace extraction followed by gas chromatographic separation with a suitable detector.

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Fast and simultaneous determination of tin and mercury species using SPME, multicapillary gas chromatography and MIP-AES detection

Cited by 31 publications

References 15 publications

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

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

Direct coupling of solid phase microextraction and quartz tube-atomic absorption spectrometry for selective and sensitive determination of methylmercury in seafood: an assessment of chloride and hydride generation

Applications of solid phase microextraction for the determination of metallic and organometallic species

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