Simultaneous Sample Preparation and Species-Specific Isotope Dilution Mass Spectrometry Analysis of Monomethylmercury and Tributyltin in a Certified Oyster Tissue

• Published in: Analytical chemistry (Washington) 2003-08, Vol.75 (16), p.4095-4102
• Main Authors: Monperrus, M, Rodriguez Martin-Doimeadios, R. C, Scancar, J, Amouroux, D, Donard, O. F. X
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Animals; Chemical Sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Environmental Pollutants - analysis; Environmental Pollutants - isolation & purification; Exact sciences and technology; Gas chromatographic methods; Gas Chromatography-Mass Spectrometry - methods; Isotopes; Marine; Mercury Isotopes; Methylmercury Compounds - analysis; Methylmercury Compounds - isolation & purification; Methylmercury Compounds - standards; Microwaves; Ostreidae; Ostreidae - chemistry; Oysters; Reference Standards; Samples; Spectrometric and optical methods; Spectrum analysis; Tin Radioisotopes; Tissues; Trialkyltin Compounds - analysis; Trialkyltin Compounds - isolation & purification; Trialkyltin Compounds - standards
• ISSN: 0003-2700; 1520-6882
• DOI: 10.1021/ac0263871

A rapid, accurate, sensitive, and simple method for simultaneous speciation analysis of mercury and tin in biological samples has been developed. Integrated simultaneous sample preparation for tin and mercury species includes open focused microwave extraction and derivatization via ethylation. Capillary gas chromatography−inductively plasma mass spectrometry (CGC−ICPMS) conditions and parameters affecting the analytical performance were carefully optimized both for species-specific isotope dilution analysis of MMHg and TBT and for conventional analysis of MBT and DBT. 201Hg-enriched monomethylmercury and 117Sn-enriched tributyltin were used for species-specific isotope dilution mass spectrometry (SIDMS) analysis. As important, accurate isotope dilution analysis requires equilibration between the spike and the analyte to achieve successful analytical procedures. Since the spike stabilization and solubilization are the most critical and time-consuming steps in isotope dilution analysis, different spiking procedures were tested. Simultaneous microwave-assisted spike stabilization and solubilization can be achieved within less than 5 min. This study originally introduces a method for the simultaneous speciation and isotope dilution of mercury and tin in biological tissues. The sample throughput of the procedure was drastically reduced by fastening sample preparation and GC separation steps. The accuracy of the method was tested by both external calibration analysis and species-specific isotope dilution analysis using the first biological reference material certified for multielemental speciation (oyster tissue, CRM 710, IRMM). The results obtained demonstrate that isotope dilution analysis is a powerful method allowing the simultaneous speciation of TBT and MMHg with high precision and excellent accuracy. Analytical problems related to low recovery during sample preparation are thus minimized by SIDMS. In addition, a rapid procedure allows us to establish a performant routine method using CGC−ICPMS technique.