Methylmercury determination in biota by solid-phase microextraction matrix effect evaluation.
Aqueous-phase alkylation followed by, headspace solid-phase microextraction (SPME) for mercury speciation in biota, was developed a decade ago. Despite this, matrix effects in this technique have not yet been addressed. In this paper, the importance of these effects has been assessed and overcome by standard addition calibration. Furthermore, improvements were made in the extraction of methylmercury (MeHg) from biological matrixes by optimizing the matrix digestion procedure (temperature and digestion time) and the SPME parameters (aliquot volume of digested samples, extraction temperature and fibre coating), which aimed to minimize the matrix effects. Accordingly, samples were alkaline digested (KOH, 25%, w/v, 60 degrees C, 180 min) and an aliquot was propylated using an aqueous NaBPr(4) solution, headspace SPME sampling and, finally, by using GC-pyrolysis (Py)-atomic fluorescence spectrometry (AFS) determination. The procedure developed was validated using dogfish muscle reference material NRCC DORM-2.
Carrasco
Luis
L
Environmental Chemistry Department, IIQAB-CSIC, Jordi Girona, 18-26, E-08034 Barcelona, Spain.
Díez
Sergi
S
Bayona
Josep M
JM
D000818:Animals; D044822:Biodiversity; D002138:Calibration; D002849:Chromatography, Gas; D004284:Dogfish; D004784:Environmental Monitoring; D008767:Methylmercury Compounds / Q000032:analysis* / Q000302:isolation & purification; D012015:Reference Standards; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000379:methods*; D013696:Temperature; D013997:Time Factors
D008767:Methylmercury Compounds