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  • Determination of phthalates and organophosphate esters in particulated material from harbour air samples by pressurised liquid extraction and gas chromatography-mass spectrometry.

Determination of phthalates and organophosphate esters in particulated material from harbour air samples by pressurised liquid extraction and gas chromatography-mass spectrometry.

Talanta (2012-11-20)
M Aragón, R M Marcé, F Borrull
ABSTRACT

A method based on gas chromatography-mass spectrometry (GC-MS) combined with a pressurised liquid extraction (PLE) to determine four organophosphates, seven phthalate esters and bis(2-ethylhexyl) adipate in particulated material of harbour air samples has been developed. Some studies show that these compounds may cause hormone disrupting effects on human health. Moreover, the U.S. Environmental Protection Agency (EPA) has classified benzyl butyl phthalate and di(2-ethylhexyl) phthalate as possible human carcinogens.The chromatographic time per run analysis is less than 15 min and the complete separation of all compounds is achieved. The PLE was optimised with recoveries above 90% and the repeatability of the method with real samples is less than 11% (%RSD, n=4). The MDLs (0.004-0.4 ng m(-3)) and MQLs (0.02-2 ng m(-3)) are limited by the fact of some compounds are present in low levels in sampling blank filters.The method was successfully applied in several samples and most of the compounds under study were found. The most relevant values were the high concentration of di-iso-butyl phthalate (between 28 and 529 ng m(-3)) and the significant concentration of di(2-ethylhexyl) phthalate (between MQL and 22 ng m(-3)). In addition, benzyl butyl phthalate was also detected in some samples but at low concentration levels (between MQL to 0.2 ng m(-3)).

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Potassium hydrogen phthalate, BioXtra, ≥99.95%
Sigma-Aldrich
Phthalic acid, reagent grade, 98%
Sigma-Aldrich
Phthalic acid, ACS reagent, ≥99.5%
Supelco
Potassium phthalate monobasic, reference material for titrimetry, certified by BAM, >99.5%
Sigma-Aldrich
Potassium phthalate monobasic, ACS reagent, acidimetric standard
Sigma-Aldrich
Potassium phthalate monobasic, puriss. p.a., ≥99.5% (T)