Effect of sample matrix on sensitivity of mercury and methylmercury quantitation in human urine, saliva, and serum using GC‐MS

Abstract

A rapid and sensitive method has been developed for the simultaneous determination of monomethylmercury (MMHg) and inorganic mercury (iHg) in human body fluids. The procedure is based on in situ derivatization of MMHg and iHg with sodium tetraethylborate (NaBEt(4)) directly in aqueous solutions followed by headspace solid phase microextraction (HS-SPME). The extracted species from spiked human urine, saliva, and serum are separated by capillary gas chromatography and detected by quadrupole MS (GC-MS). The optimization of the HS-SPME conditions like temperature, sample volume, extraction duration, and amount of alkylation agent, was performed in urinary solutions and aqueous solutions similarly buffered. The gas chromatographic conditions like injection temperature, helium flow rate, temperature program, and pressure conditions were also optimized. The recovery was ranged between 85 and 96% for MMHg and 88 and 98% for iHg. The LODs achieved were 10 and 15 ng/L for iHg and MMHg in urine, respectively, 54 and 60 ng/L for iHg and MMHg in saliva, respectively, and 61 and 81 ng/L for iHg and MMHg in serum, respectively. The RSD was ranged between 6.2 and 9.2% for MMHg and 5.0 and 8.2% for iHg.

Comparative determination of methyl mercury in whole blood samples using GC–ICP-MS and GC–MS techniques

“…Recently, Zachariadis et al have published a method for the determination of MeHg in human body fluids. The method was applied to the analysis of two serum samples, however, the MeHg concentrations in these samples were below the limit of detection [18]. Nevertheless, whether the measured concentrations represent "true" values remains unclear, as long as certified reference material (CRM) for MeHg in blood samples is not available.…”

Ultrasensitive determination of mercury in human saliva by atomic fluorescence spectrometry based on solidified floating organic drop microextraction

“…So, it is significant and necessary to develop new methods for the enrichment of mercury in some special samples before analysis [22][23][24][25]. Normally, the level of mercury in human saliva is low and the reports about mercury analysis in human saliva were very scarce [26,27]. Saliva is viscous since it contains proteins.…”

A Simple and Robust Method for Determination of Alkylmercury in Seawater and Industrial Wastewater by Phenylation Pretreatment Combined with GC-MS

“…Gas chromatography (GC) is preferable due to the high separation performance of alkylmercury and has been widely used in conjunction with electron-capture detection (ECD), 4,5 atomic emission spectrometry (AES), 6 atomic fluorescence spectrometry (AFS), [6][7][8] electron ionization mass spectrometry (EI-MS) 9,10 and inductively coupled plasma mass spectrometry (ICP-MS). 7,11 However, GC-ECD in conjunction with direct extraction of MeHg into toluene without derivatization 12 was not applicable to river water and seawater samples because of the severe interferences from co-extracted substances.…”