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The procedure is based on <jats:italic>in situ<\/jats:italic> derivatization of MMHg and iHg with sodium tetraethylborate (NaBEt<jats:sub>4<\/jats:sub>) directly in aqueous solutions followed by headspace solid phase microextraction (HS\u2010SPME). The extracted species from spiked human urine, saliva, and serum are separated by capillary gas chromatography and detected by quadrupole MS (GC\u2010MS). The optimization of the HS\u2010SPME 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.<\/jats:p>","DOI":"10.1002\/jssc.200800345","type":"journal-article","created":{"date-parts":[[2008,11,19]],"date-time":"2008-11-19T07:50:17Z","timestamp":1227081017000},"page":"3884-3893","source":"Crossref","is-referenced-by-count":25,"title":["Effect of sample matrix on sensitivity of mercury and methylmercury quantitation in human urine, saliva, and serum using GC\u2010MS"],"prefix":"10.1002","volume":"31","author":[{"given":"George A.","family":"Zachariadis","sequence":"first","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Dimitra C.","family":"Kapsimali","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"311","published-online":{"date-parts":[[2008,12,8]]},"reference":[{"key":"e_1_2_1_2_2","unstructured":"Jenkins R. O. Craig P. J. Francesconi K. A. Harrington C. F. 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