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.

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