Mercury speciation in seafood samples by LC-ICP-MS with a rapid ultrasound-assisted extraction procedure: Application to the determination of mercury in Brazilian seafood samples

This paper describes a simple method for mercury speciation in seafood samples by LC-ICP-MS with a fast sample preparation procedure. Prior to analysis, mercury species were extracted from food samples with a solution containing mercaptoethanol, L-cysteine and HCl and sonication for 15 min. Separation of mercury species was accomplished in less than 5 min on a C8 reverse phase column with a mobile phase containing 0.05%-v/v mercaptoethanol, 0.4% m/v L-cysteine and 0.06 mol L(-1) ammonium acetate. The method detection limits were found to be 0.25, 0.20 and 0.1 ng g(-1) for inorganic mercury, ethylmercury and methylmercury, respectively. Method accuracy is traceable to Certified Reference Materials (DOLT-3 and DORM-3) from the National Research Council Canada (NRCC). With the proposed method there is a considerable reduction of the time of sample preparation. Finally, the method was applied for the speciation of mercury in seafood samples purchased from the Brazilian market. (C) 2010 Elsevier Ltd. All rights reserved.

Mercury speciation in whole blood by gas chromatography coupled to ICP-MS with a fast microwave-assisted sample preparation procedure

A simple and fast method is described for simultaneous determination of methylmercury (MeHg), ethylmercury (Et-Hg) and inorganic mercury (Ino-Hg) in blood samples by using capillary gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS) after derivatization and alkaline digestion. Closed-vessel microwave assisted digestion conditions with tetramethylammonium hydroxide (TMAH) have been optimized. Derivatization by using ethylation and propylation procedures have also been evaluated and compared. The absolute detection limits (using a 1 mu L injection) obtained by GC-ICP-MS with ethylation were 40 fg for MeHg and Ino-Hg, respectively, and with propylation were 50, 20 and 50 fg for MeHg, Et-Hg and Ino-Hg, respectively. Method accuracy is traceable to Standard Reference Material (SRM) 966 Toxic Metals in Bovine Blood from the National Institute of Standards and Technology (NIST). Additional validation is provided based on the comparison of results obtained for mercury speciation in blood samples with the proposed procedure and with a previously reported LC-ICP-MS method. With the new proposed procedure no tedious clean-up steps are required and a considerable improvement of the time of analysis was achieved compared to other methods using GC separation.

Column connection detail, Kangaroo Point House

Hand-made spotted gum column on edge of outdoor room.

West elevation, Cleveland Point House, Cleveland

Hand-drawn elevation.

Cottage, Cleveland Point House, Cleveland

Beach elevation of renovated existing cottage.

Lattice to boat house, Cleveland Point House, Cleveland

Lattice behind pull-down blind to boat house.

Beachfront elevation, Cleveland Point House, Cleveland

Timber framing to new bath house (centre), with existing buildings to either side.

Bath house, Cleveland Point House, Cleveland

New bath house under construction (centre), with existing buildings to either side.

Bath house, Cleveland Point House, Cleveland

Bath house under construction, as seen looking towards water from deck area.

Bath house, Cleveland Point House, Cleveland

As seen looking towards water from deck area.

Beachfront elevation, Cleveland Point House, Cleveland

New bath house (centre), with existing buildings to either side.

Boat house, Cleveland Point House, Cleveland

Existing boat house undergoing renovations.

Bath house hip rafters, Cleveland Point House, Cleveland

Timber framing to new bath house.

Beachfront elevation, Cleveland Point House, Cleveland

Timber framing to new bath house (centre), with existing buildings to either side.

Bath house section, Cleveland Point House, Cleveland

Section taken through new bath house.