Determination of phthalate esters in cow milk samples using dispersive liquid-liquid microextraction coupled with gas chromatography followed by flame ionization and mass spectrometric detection.
Journal - Journal of separation science
A simple and economic method for the analysis of phthalate esters, dimethyl phthalate, diethyl phthalate, di-iso-butyl phthalate, di-n-butyl phthalate, and di-2-ethylhexyl phthalate in cow milk samples by means of gas chromatography-flame ionization detection and gas chromatography-mass spectrometry has been developed. In this work, NaCl and ACN were added to 5?mL of the milk sample as the salting out agent and extraction solvent, respectively. After manual shaking, the mixture was centrifuged. In the presence of NaCl, a two-phase system was formed: upper phase - acetonitrile containing phthalate esters - and lower phase - aqueous phase containing soluble compounds and the precipitated proteins. After the extraction of phthalate esters from milk, a portion of supernatant phase (acetonitrile) was removed, mixed with 1,2-dibromoethane at microliter level and injected by syringe into NaCl solution. After the extraction of the selected phthalate esters into 1,2-dibromoethane, phase separation was performed by centrifugation and the enriched analytes in the sedimented phase were determined by gas chromatography-flame ionization detection and gas chromatography-mass spectrometry. Under the optimum extraction conditions, low limits of detection and quantification between 1.5-3 and 2.5-11?ng/mL, respectively was observed. Enrichment factors were in the range of 397-499. The relative standard deviations for the extraction of 100?ng/mL of each phthalate ester were in the range of 3-4% (n=6). Finally, some milk samples were successfully analyzed using the proposed method and two analytes, di-n-butyl phthalate and di-2-ethylhyxel phthalate, were determined in them in nanogram per milliliter level.Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Combination of solid-phase extraction-hollow fiber for ultra-preconcentration of some triazole pesticides followed by gas chromatography-flame ionization detection.
Journal - Journal of separation science
In this study, an extraction and preconcentration technique using solid-phase extraction (SPE) along with hollow fiber (HF) has been developed as an ultra-preconcentration technique for some triazole pesticides in aqueous samples. Triazole pesticides were employed as model compounds to assess the method and were monitored by gas chromatography-flame ionization detection (GC-FID). Initially, an aqueous solution of target analytes was passed through an RP-8 SPE cartridge and then the adsorbed analytes were eluted with µL amounts of toluene. The collected elute was slowly introduced into an HF that had one end blocked. This allowed precipitation inside the lumen and pores of the HF. Finally, the obtained HF was mounted on a home-made solid-phase microextraction syringe and entered into the GC injection port for thermal desorption-GC analysis. The effect of various experimental parameters including injection port temperature, desorption time, state of HF, washing solvent, elution solvent and its volume, sample volume, etc. were investigated for finding the optimum conditions. The calibration graphs were linear in the ranges of 2-1000?ng/mL (penconazole and hexaconazole), 5-1000?ng/mL (tebuconazole), 15-1000?ng/mL (triticonazole) and the detection limits (LODs) ranged from 0.6 to 4.5?ng/mL. The enhancement factors were in the range of 870-950. The relative standard deviations (RSD%) for five repeated experiments (C=250?ng/mL of each pesticide) varied from 4.5 to 8.7%. The relative recoveries obtained for analytes in grape juice samples, spiked with different levels of each pesticide, were in the range of 87-119%.Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.