title: Feasibility of ultra-high performance liquid and gas chromatography coupled to mass spectrometry for accurate determination of primary and secondary phthalate metabolites in urine samples.
abstract: Phthalates (PAEs) are ubiquitous toxic chemical compounds. During the last few years, some phthalate metabolites (MPAEs) have been proposed as appropriate biomarkers in human urine samples to determine PAE human intake and exposure. So, it is necessary to have fast, easy, robust and validated analytical methods to determine selected MPAEs in urine human samples. Two different instrumental methods based on gas (GC) and ultra-high performance liquid (UHPLC) chromatography coupled to mass spectrometry (MS) have been optimized, characterized and validated for the simultaneous determination of nine primary and secondary phthalate metabolites in urine samples. Both instrumental methods have similar sensitivity (detection limits ranged from 0.03 to 8.89 pg μL(-1) and from 0.06 to 0.49 pg μL(-1) in GC-MS and UHPLC-MS(2), respectively), precision (repeatability, expressed as relative standard deviation, which was lower than 8.4% in both systems, except for 5OH-MEHP in the case of GC-MS) and accuracy. But some advantages of the UHPLC-MS(2) method, such as more selectivity and lower time in the chromatographic runs (6.8 min vs. 28.5 min), have caused the UHPLC-MS(2) method to be chosen to analyze the twenty one human urine samples from the general Spanish population. Regarding these samples, MEP showed the highest median concentration (68.6 μg L(-1)), followed by MiBP (23.3 μg L(-1)), 5cx-MEPP (22.5 μg L(-1)) and MBP (19.3μgL(-1)). MMP (6.99 μg L(-1)), 5oxo-MEHP (6.15 μg L(-1)), 5OH-MEHP (5.30 μg L(-1)) and MEHP (4.40 μg L(-1)) showed intermediate levels. Finally, the lowest levels were found for MBzP (2.55 μg L(-1)). These data are within the same order of magnitude as those found in other similar populations.
authors.affiliation: General Organic Chemistry Institute, CSIC, Juan de la Cierva 3, 28006 Madrid, Spain.
authors.forename: Laura
authors.initials: L
authors.lastname: Herrero
authors.affiliation: General Organic Chemistry Institute, CSIC, Juan de la Cierva 3, 28006 Madrid, Spain.
authors.forename: Sagrario
authors.initials: S
authors.lastname: Calvarro
authors.affiliation: General Organic Chemistry Institute, CSIC, Juan de la Cierva 3, 28006 Madrid, Spain.
authors.forename: Mario A
authors.initials: MA
authors.lastname: Fernández
authors.affiliation: General Organic Chemistry Institute, CSIC, Juan de la Cierva 3, 28006 Madrid, Spain.
authors.forename: Jesús Eduardo
authors.initials: JE
authors.lastname: Quintanilla-López
authors.affiliation: General Organic Chemistry Institute, CSIC, Juan de la Cierva 3, 28006 Madrid, Spain.
authors.forename: María José
authors.initials: MJ
authors.lastname: González
authors.affiliation: General Organic Chemistry Institute, CSIC, Juan de la Cierva 3, 28006 Madrid, Spain. Electronic address: bgomara@iqog.csic.es.
authors.forename: Belén
authors.initials: B
authors.lastname: Gómara
mesh_terms: D000328:Adult; D002851:Chromatography, High Pressure Liquid; D005240:Feasibility Studies; D005260:Female; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D008297:Male; D008875:Middle Aged; D010795:Phthalic Acids / Q000378:metabolism / Q000652:urine*; D021241:Spectrometry, Mass, Electrospray Ionization
chemical_list: D010795:Phthalic Acids; C032279:phthalic acid
keywords: Gas chromatography; Mass spectrometry; Phthalate metabolites; Ultra-high performance liquid chromatography; Urine