PMID- 23510960 OWN - NLM STAT- MEDLINE DCOM- 20130826 LR - 20151119 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1286 DP - 2013 Apr 19 TI - Magnetic solid-phase extraction based on magnetic multi-walled carbon nanotubes for the determination of phthalate monoesters in urine samples. PG - 22-8 LID - S0021-9673(13)00377-4 [pii] LID - 10.1016/j.chroma.2013.02.070 [doi] AB - In this study, magnetic carbon nanotubes (MCNTs) were prepared by assembling magnetic nanoparticles onto the acid-treated multiwall carbon nanotubes (MWCNTs). Due to their excellent adsorption capability, the MCNTs were used as adsorbent of magnetic solid-phase extraction (MSPE) to extract phthalate monoesters (PMEs), the main biomarkers of phthalate exposure, from human urine. By coupling MSPE with gas chromatography-mass spectrometry (GC-MS), a reliable, sensitive and cost-effective method for the simultaneous determination of five main PMEs including monomethyl phthalate (MMP), monoethyl phthalate (MEP), mono n-butyl phthalate (MBP), mono-(2-ethylhexyl) phthalate (MEHP) and monobenzyl phthalate (MBzP) was developed. The factors that could influence the extraction, including the amount of magnetic nanoparticles, pH of sample solution, extraction and desorption time, the amount of salt addition, the type and volume of desorption solvent were investigated in detail. Under optimized conditions, the LODs and LOQs achieved were in the range of 0.025-0.050 and 0.125-0.250 ng mL(-1) respectively. And calibration curves were linear (r(2)>/=0.992) over the concentration ranges from 0.250 to 250 ng mL(-1). In addition, a satisfying reproducibility was achieved by evaluating the intra- and inter-day precisions with relative standard deviations (RSDs) less than 11.2% and 11.4%, respectively. The recoveries of the five PMEs ranged from 92.6% to 98.8% with the RSDs less than 10.7%. Finally, the established MSPE-GC-MS method was successfully applied to determine PMEs in human urine samples. MMP, MEP, MBP and MEHP were detected in most of the samples with the median concentration of 8.46, 9.26, 13.60, and 5.95 ng mL(-1) respectively. MBzP was detected in 58.3% of the samples with the median concentration of 3.05 ng mL(-1). Taken together, the MSPE-GC-MS method developed in current study provides a new option for the determination of PMEs in human urine. CI - Copyright (c) 2013 Elsevier B.V. All rights reserved. FAU - Rastkari, Noushin AU - Rastkari N AD - Center for Air Pollution Research (CAPR), Institute for Environmental Research (IER), Tehran University of Medical Sciences, Tehran 1417614411, Iran. nr_rastkari@yahoo.com FAU - Ahmadkhaniha, Reza AU - Ahmadkhaniha R LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20130227 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Biomarkers) RN - 0 (Magnetite Nanoparticles) RN - 0 (Nanotubes, Carbon) RN - 0 (Phthalic Acids) RN - 451W47IQ8X (Sodium Chloride) SB - IM MH - Biomarkers/urine MH - Gas Chromatography-Mass Spectrometry MH - Humans MH - Limit of Detection MH - Magnetite Nanoparticles/*chemistry MH - Male MH - Nanotubes, Carbon/*chemistry MH - Phthalic Acids/*isolation & purification/*urine MH - Reproducibility of Results MH - Sodium Chloride/chemistry MH - Solid Phase Extraction/*methods MH - Young Adult EDAT- 2013/03/21 06:00 MHDA- 2013/08/27 06:00 CRDT- 2013/03/21 06:00 PHST- 2012/11/27 00:00 [received] PHST- 2013/02/20 00:00 [revised] PHST- 2013/02/21 00:00 [accepted] PHST- 2013/03/21 06:00 [entrez] PHST- 2013/03/21 06:00 [pubmed] PHST- 2013/08/27 06:00 [medline] AID - S0021-9673(13)00377-4 [pii] AID - 10.1016/j.chroma.2013.02.070 [doi] PST - ppublish SO - J Chromatogr A. 2013 Apr 19;1286:22-8. doi: 10.1016/j.chroma.2013.02.070. Epub 2013 Feb 27.