Facultade de Fisioterapia

Headspace single drop microextraction of methylpentadyenil-manganese tricarbonyl from water samples followed by gas chromatography-mass spectrometry

Authors: F.J. Pena-Pereira, Carlos Bendicho, N. Kalogerakis, E. Psillakis

Journal: Talanta, 74: 47-51, 11/2007

DOI: http://dx.doi.org/10.1016/j.talanta.2007.05.024


Headspace single drop microextraction coupled to gas chromatography–mass spectrometry yielded a simple, fast and virtually solventless analytical protocol used for the headspace analysis of aqueous samples contaminated with methylcyclopentadienyl-manganese tricarbonyl (MMT). Initially, several experimental parameters were controlled and optimized and the optimum conditions found were 2.5 μl octane microdrop exposed for 20 min to the headspace of a 10 ml aqueous sample (15 ml vial) containing 20% (w/v) NaCl and stirred at 1250 rpm. The calculated calibration curves gave a high level of linearity for MMT with correlation coefficients >0.9995 after conducting a 3-day study. The limit of detection was calculated to be 0.21 μg l−1. The proposed method achieved an enrichment factor of the order of 2100 and a 53% recovery after extracting the spiked aqueous solution for 20 min under the optimized experimental conditions. The repeatability and intra-day reproducibility of the proposed method, expressed as relative standard deviation were 8.4 and 6.4%, respectively. Finally, analysis of spiked tap and wastewater samples revealed that matrix had little effect upon extraction.