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Barbarossa A.,University of Bologna | Masetti R.,University of Bologna | Gazzotti T.,University of Bologna | Zama D.,University of Bologna | And 4 more authors.
Environment International | Year: 2013

Due to their widespread diffusion, perfluoroalkyl substances (PFASs) have been frequently found in the environment and in several animal species. It has been demonstrated that they can easily reach also humans, mainly through diet. Being lactation a major route of elimination of these contaminants, their occurrence in human milk is of particular interest, especially considering that it generally represents the unique food source for newborns. Perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA), the two most important compounds of this family, have been frequently found in human milk at variable concentrations, but still limited data are available. The present study, the first conducted in Italy capable to detect these pollutants at ultra-trace levels by UPLC-MS/MS, confirmed the role of lactation as a relevant source of exposure for breastfed children. The measured concentrations ranged between 15 and 288 ng/L for PFOS and between 24 and 241 ng/L for PFOA. Moreover, mean concentrations and frequencies of both analytes resulted higher in milk samples provided by primiparous women, suggesting that the risk of intake might be higher for first-borns. Finally, comparing these results with previous data, PFOS gradual decrease over time since year 2000 was confirmed. © 2012 Elsevier Ltd. Source


Vanhaecke L.,Ghent University | Antignac J.-P.,USC 2013 LABERCA | Antignac J.-P.,French National Institute for Agricultural Research | Courtheyn D.,Federal Laboratory for the Safety of the Food Chain | And 2 more authors.
Steroids | Year: 2011

Corticosteroids are hormonal substances widely used in human and veterinary medicine for their anti-inflammatory properties. Among the numerous existing artificial corticosteroids, dexamethasone remains the most commonly used, mainly throughout esterified forms such as acetate or phosphate. An experimental study was designed to assess its drug residue levels in urine and feces, as well as its fixation in bovine hair following a single administration of 0.15 mg/kg b.w. dexamethasone acetate and 0.12 mg/kg b.w. dexamethasone sodium phosphate. Different analytical methods based on GC-MS or LC-MS/MS were used for measuring dexamethasone and its esterified forms, which were implemented in 3 different European laboratories in the field that collaborated for this study. The obtained results confirmed the high and rapid urinary excretion rate of dexamethasone, with a maximal concentration (267 μg/L) measured one day after administration and 98% elimination within 3 days. The concentrations obtained with the GC-NCI-MS procedure (using chemical oxidation as derivatization) were found significantly higher than the ones obtained with LC-ESI-MS/MS, indicating a possible contribution of dexamethasone phase I and/or II metabolites to the monitored signal. Fecal elimination was also found rapid (95% elimination within 3 days) with a maximum concentration level (28.5 μg/kg) observed one day after administration. Detectable levels of dexamethasone in hair appeared on day 2 (11.5 μg/kg), reached a maximum around one week, and could be identified until 22 days upon treatment, establishing the suitability of hair as a biological matrix for medium to long-term residue controls of dexamethasone. © 2010 Elsevier Inc. All rights reserved. Source


Kadar H.,USC 2013 LABERCA | Veyrand B.,USC 2013 LABERCA | Barbarossa A.,University of Bologna | Pagliuca G.,University of Bologna | And 9 more authors.
Chemosphere | Year: 2011

Perfluorinated compounds (PFCs) are man-made chemicals for which endocrine disrupting properties and related possible side effects on human health have been reported, particularly in the case of an exposure during the early stages of development, (notably the perinatal period). Existing analytical methods dedicated to PFCs monitoring in food and/or human fluids are currently based on liquid chromatography coupled to tandem mass spectrometry, and were recently demonstrated to present some limitations in terms of sensitivity and/or specificity. An alternative strategy dedicated to the analysis of fourteen PFCs in human breast milk was proposed, based on an effective sample preparation followed by a liquid chromatography coupled to high resolution mass spectrometry measurement (LC-HRMS). This methodology confirmed the high interest for HRMS after negative ionization for such halogenated substances, and finally permitted to reach detection limits around the pgmL -1 range with an outstanding signal specificity compared to LC-MS/MS. The proposed method was applied to a first set of 30 breast milk samples from French women. The main PFCs detected in all these samples were PFOS and PFOA with respective median values of 74 (range from 24 to 171) and 57 (range from 18 to 102) pgmL -1, respectively. These exposure data appeared in the same range as other reported values for European countries. © 2011 Elsevier Ltd. Source


Antignac J.-P.,USC 2013 LABERCA | Antignac J.-P.,French National Institute for Agricultural Research | Courant F.,USC 2013 LABERCA | Pinel G.,USC 2013 LABERCA | And 4 more authors.
TrAC - Trends in Analytical Chemistry | Year: 2011

Mass spectrometry (MS)-based metabolomics is emerging as an important field of research in many scientific areas, including chemical safety of food. A particular strength of this approach is its potential to reveal some physiological effects induced by complex mixtures of chemicals present at trace concentrations. The limitations of other analytical approaches currently employed to detect low-dose and mixture effects of chemicals make detection very problematic. Besides this basic technical challenge, numerous analytical choices have to be made at each step of a metabolomics study, and each step can have a direct impact on the final results obtained and their interpretation (i.e. sample preparation, sample introduction, ionization, signal acquisition, data processing, and data analysis). As the application of metabolomics to chemical analysis of food is still in its infancy, no consensus has yet been reached on defining many of these important parameters. In this context, the aim of the present study is to review all these aspects of MS-based approaches to metabolomics, and to give a comprehensive, critical overview of the current state of the art, possible pitfalls, and future challenges and trends linked to this emerging field. © 2010 Elsevier Ltd. Source


Kadar H.,USC 2013 LABERCA | Kadar H.,University of Nantes | Veyrand B.,USC 2013 LABERCA | Veyrand B.,University of Nantes | And 8 more authors.
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment | Year: 2011

Perfluorinated compounds (PFCs) are usually monitored by high-performance liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) on triple quadrupole instruments. Although not yet widely implemented in the field, high-resolution mass spectrometry (HRMS) today appears as a valuable alternative for these halogenated chemicals due to their significant mass defect. Indeed, this second approach offers a way to cope with particular matrix effects caused by co-eluting and isobaric interferences affecting the measurement of some PFCs in fish. The present study compares three different LC-MS-related instruments and various signal acquisition modes, from low-resolution full-scan and selected ion-monitoring (SIM) mode on a triple quadrupole (QqQ) instrument to high-resolution full-scan or product ion-scan mode on orbital trap (LTQ-Orbitrap) or quadrupole-time-of-flight (Q-TOF) devices. Performances are compared for seven model compounds belonging to seven PFCs subclasses: perfluoralkylsulfonate, perfluoroalkylcarboxylate, perfluoroalkylsulfinate, perfluoroalkyl-sulfonamide, fluorotelomer saturated acid, fluorotelomer unsaturated acid and perfluoroalkylphosphonic acid. Low-resolution MS/MS was found to be unsurprisingly reliable for extended multi-residue monitoring. However, the high stability of PFCs leads to a relatively poor and non-specific fragmentation pathway in MS/MS. In addition, biliary acid-interfering compounds (e.g. taurochenodeoxycholic acid), which where encountered in the present case in fish samples but that may be present in other biological samples, were found particularly disturbing in low-resolution MS/MS. Indeed, these interferences presented the same retention time and diagnostic signals as PFOS, leading to a possible overestimation of the PFOS quantification in LC-MS/MS. On the other hand, high-resolution MS and MS/MS (LTQ-Orbitrap and Q-TOF) provided better results in terms of signal specificity and sensitivity. For instance, the estimated limits of detection (LOD) reached for PFOS on QqQ, Q-TOF and LTQ-Orbitrap instruments were 3.8, 0.7 and 0.5 pg injected, respectively. © 2011 Taylor & Francis. Source

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