In order to attain a lower detection limit with the HS GC MIP analytical method (Head-Space Gas Chromatography with Microwave-Induced Plasma detection) recently developed for the analysis of methylmercury in biological samples, the quarter-wave Evenson-type cavity used until now was replaced by a TM010 Beenakker-type cavity, which was used with both argon and helium as carrier gas. With an argon plasma, an eightfold increase in detection limit was gained compared with the argon plasma sustained by the Evenson cavity, while only a four-fold increase was gained with the helium plasma. In a second step of the study, the MIP detector was replaced by an AFS (atomic fluorescence) detector (CVAFS Model-2, Brooks Rand Ltd, Seattle, USA). With this AFS detector a detection limit of 1 ng methyl mercury per g biological tissue could be reached; i.e. measurements were 40 times more sensitive than those using the Evenson cavity. This detector has some other advantages compared with MIP detection: it is less expensive and easier to manipulate, while the same precision and accuracy are obtained. The use of AFS as detector in the head-space gas chromatographic system is therefore an important improvement for the analysis of methylmercury in biological samples.