Chemija / Chemistry
 ISSN 0235-7216 ISSN 2424-4538 (online) |
2011 m. Nr. 4 Solid phase extraction and gas chromatographic – mass spectrometric analysis of phthalates in surface water:method development and validation
The aim of the research was to apply and optimize the solid phase extraction (SPE) and gas chromatographic – mass spectrometric (GC–MS) method for the analysis of phthalates in surface water and carry out the necessary method validation steps.
Two standard mixtures of phthalates were used: the self-composed diethyl phthalate (DEP) and di(n-butyl) phthalate (DnBP) standard mixture (EBS), and EPA506 standard mixture consisting of seven phthalates. Detection limits for EPA506 varied in the range 45–500 ng/L, depending on the compound. The linear dependence of the EPA506 standard mixture components was in the range 0.1–54 μg/L. SPE was performed using a column filled with C-18 silicagel adsorbent in a system isolated from atmospheric contamination. The recovery values of EBS components when using a 1 : 1 mixture of ethyl acetate and dichlormethane as an eluent were 79 ± 5% for DEP and 97 ± 11% for DnBP. The background signals of DnBP and di(2-ethylhexyl) phthalate were determined. The method was applied for the analysis of samples from the Venta river (Lithuania) in 2010 and 2011. The variation of pollutant concentrations was determined. DnBP in December 2010, January, March, and April 2011 were 0.14 μg/L, 2.7 μg/L, 1.45 μg/L, and 2.2 μg/L, respectively; DEHP concentration in January 2011 was 2.1 μg/L, in April 0.23 μg/L, and DEP concentration in March 2011 was 0.61 μg/L. Keywords: surface water, phthalates, solid phase extraction, gas chromatography – mass spectrometry |
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