Headspace single drop microextraction of methylcyclopentadienyl-manganese tricarbonyl from water samples followed by gas chromatography-mass spectrometry.
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 microl 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 microg 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.
Pereira
Francisco Javier Pena
FJ
Departamento de Química Analítica y Alimentaria, Facultad de Ciencias de Vigo, Universidad de Vigo As Lagoas-Marcosende, E-36200 Vigo, Spain.
Bendicho
Carlos
C
Kalogerakis
Nicolas
N
Psillakis
Elefteria
E
D008401:Gas Chromatography-Mass Spectrometry; D009942:Organometallic Compounds / Q000032:analysis*; D014874:Water Pollutants, Chemical / Q000032:analysis*
D009942:Organometallic Compounds; D014874:Water Pollutants, Chemical; C009907:2-methylcyclopentadienyl manganese tricarbonyl