Sample pretreatment for the measurement of phthalate esters in complex matrices

Abstract

Sample pretreatment methods for the measurement of phthalate esters (PAEs) by gas chromatography-mass spectrometry (GC-MS) in various complex matrices, including sediment, soil, suspended particle matter, urban surface dust, Sinonovacula Constricta, cosmet- ic, leather, plastic and coastal/estuarine seawater, were proposed. The pretreatment which was appropriate for GC-MS detection was focused on the investigation and optimization of oper- ating parameters for the extraction and purification, such as the extraction solvent, the eluant and the adsorbent of solid phase extraction. The results of the study of pretreatment for various complex matrices showed that methylene chloride was the best solvent for the ultrasonic extraction when solid-liquid extraction was used; silica gel was the economical and practical adsorbent for solid-phase extraction for purification; C18 was the most commonly adsorbent for preconcentration of PAE in coastal/estuarine seawater sample; the mixed solution of n-hexane and ethyl acetate with a certain proportion was the suitable SPE eluent. Under the optimized conditions, the spiked recoveries were above 58% and the relative standard deviations (RSDs) were less than 10.5% (n = 6). The detection limits (DL, 3σ) were in the range of 0.3 μg/kg (dibutyl phthalate)--5.2 μg/kg ( diisononyl phthalate) for sediment, and 6 ng/L (dipropyl phthalate)--67 ng/L (diisodecyl phthalate) for costal/estuarine seawater. The pretreatment meth- od for various complex matrices is prominent for the measurement of the 16 PAEs with GC-MS.