Arsenosugar extracted from algae: Assessment of countercurrent chromatography for isolation.

Arsenosugars are the predominant species of arsenic in most seaweed. The analysis of these compounds is hampered by the lack of calibration standards needed in their unambiguous identification and quantification. This affects the availability of reliable information on their potential toxicity, which is scarce and controversial.

Search for Biomarkers for the LC-ESI-QqQ Determination of Phenoxymethylpenicillin Treatment in Raw or Cooked Chicken Meat Samples.

The high standards required for food safety make it necessary to trace unambiguously raw or cooked food products coming from medicated animals. Nevertheless, considering the lability of β-lactams and their degradation, the detection of the presence of antibiotics in meat either raw or submitted to a cooking process is not easily affordable. To achieve this goal, an evaluation of the effect of common domestic cooking procedures, such as boiling and grilling, on the fate of phenoxymethylpenicillin (PENV) residues was performed.

Survey of arsenic content in edible seaweeds and their health risk assessment.

Since humans are especially sensitive to arsenic exposure, predominantly through diet, a strict control of the most widely consumed seaweeds is mandatory. Total arsenic contents and arsenic species in twenty-five different seaweeds from five different origins were studied. Seaweeds selected, included Phaeophyta (brown seaweed), Chlorophyta (green seaweed) and Rhodophyta (red seaweed) genera.

Arsenosugar extracted from algae: Isolation by anionic exchange solid-phase extraction.

Obtaining reliable speciation data for evaluating dietary exposure, and increasing understanding of arsenic biochemistry in algae, are hindered by the availability of suitable standards of arsenosugars, the major species in these types of samples. Moreover, chemical syntheses of such compounds have been reported to be complex and tedious. The aim of this work was to investigate the feasibility of the anionic exchange SPE cartridges (SAX and WAX) as an easy and quick alternative for the isolation and preconcentration of arsenosugars.

Metabolites in Milk after Enrofloxacin Treatment and Their Persistence to Temperature.

In this work, metabolomic profile changes in milk from cows affected by mastitis and treated with enrofloxacin (ENR) have been studied using LC-HRMS techniques. Principal component analysis was applied to the obtained results, and the interest was focused on changes affecting compounds without a structural relationship to ENR. Most of the compounds, whose concentrations were modified as a result of the pharmacological treatment and/or the pathological status, were related to amino acids and peptides.

Determination of quinolone residues in raw cow milk. Application of polar stir-bars and ultra-high performance liquid chromatography-tandem mass spectrometry.

Seventeen quinolone antibiotics were determined in cows' milk. A method of high sensitivity, selectivity and accuracy was developed. Accuracy (trueness and precision), linearity, sensitivity, selectivity, decision limit and detection capability were established following the recommendations of the Commission Decision 2002/657/EC and the Food and Drug Administration (FDA) guideline.

Occurrence of veterinary pharmaceuticals in golden eagle nestlings: Unnoticed scavenging on livestock carcasses and other potential exposure routes.

Wildlife exposure to pharmaceuticals can occur through contaminated water, and through the excreta and carcasses of medicated livestock, with potential for bioaccumulation and transfer through food webs. We evaluated whether nestling exposure to pharmaceuticals can occur from food delivered to nests in the golden eagle (Aquila chrysaetos), a top predator and facultative scavenger. Despite the fact that diet analysis suggests an apparently low dependence on livestock carcasses reduced to two piglets remains (1.

Food safety in scavenger conservation: Diet-associated exposure to livestock pharmaceuticals and opportunist mycoses in threatened Cinereous and Egyptian vultures.

Pharmaceuticals from veterinary treatments may enter terrestrial food webs when medicated livestock are available to wildlife in supplementary feeding stations aimed at the conservation of endangered scavengers. Here, we hypothesized that the exposure risk to livestock fluoroquinolones, as indicators of pharmaceutical burden in food, is related to the variable reliance of scavengers on domestic versus wild animal carcasses. Since the misuse of broad-spectrum antibiotics is a major predisposing factor for opportunistic mycoses, we evaluated disease signs potentially associated with diet-dependent drug exposure in nestlings of two threatened vultures.

Wildlife contamination with fluoroquinolones from livestock: Widespread occurrence of enrofloxacin and marbofloxacin in vultures.

There is much recent interest in the presence and impact of veterinary pharmaceuticals in wildlife. Livestock carcasses are often disposed of in supplementary feeding stations for avian scavengers, as a management and conservation tool for these species worldwide. In feeding stations, vultures and other scavengers can consume carcasses almost immediately after disposal, which implies the potential ingestion of veterinary pharmaceuticals as a non-target consequence of supplementary feeding.

Multiclass method for the determination of quinolones and β-lactams, in raw cow milk using dispersive liquid-liquid microextraction and ultra high performance liquid chromatography-tandem mass spectrometry.

An analytical method based on a sample treatment by dispersive liquid-liquid microextraction (DLLME) followed by ultra high performance liquid chromatography-tandem mass spectrometry analysis (UHPLC-MS/MS) for the determination of 17 quinolones and 14 β-lactams (penicillins and cephalosporins) in raw cow milk, was validated according to the European Commission guidelines as cited in the Decision 2002/657/EC. The extraction efficiency of the DLLME depends on several parameters such as the nature and volumes of extractant and dispersive solvents, pH, concentration of salt, shaking time and time of centrifugation. These variables were accurately optimized using multivariate optimization strategies.

Identification of metabolites and thermal transformation products of quinolones in raw cow's milk by liquid chromatography coupled to high-resolution mass spectrometry.

The presence of residues of antibiotics, metabolites, and thermal transformation products (TPs), produced during thermal treatment to eliminate pathogenic microorganisms in milk, could represent a risk for people. Cow's milk samples spiked with enrofloxacin (ENR), ciprofloxacin (CIP), difloxacin (DIF), and sarafloxacin (SAR) and milk samples from cows medicated with ENR were submitted to several thermal treatments. The milk samples were analyzed by liquid chromatography-mass spectrometry (LC-MS) to find and identify TPs and metabolites.

Modeling the electrophoretic behavior of quinolones in aqueous and hydroorganic media.

The applicability of the classical semiempirical relationships between the electrophoretic mobility and charge-to-mass ratio (m(e) versus q/M(alpha)) has been investigated to describe migration behavior of a series of quinolones in aqueous and hydroorganic media. The Stoke's law (alpha=1/3), the classical polymer model (alpha=1/2) and the Offord's surface law (alpha=2/3) were evaluated in the pH range comprised between 2 and 11 in ACN-water mixtures of 0, 10 and 30% m/m ACN. As accurate acidity constant values were available for charge calculations, correlations were excellent.

Determination of penicillins in milk using LC-UV, LC-MS and LC-MS/MS.

The aim of this work is to establish a method for the simultaneous determination of eight penicillins in milk samples by LC-UV, LC-MS and LC-MS/MS. The procedure involves a step for clean-up and to preconcentrate the analytes by SPE and a subsequent chromatographic analysis. LC-UV, LC-MS and LC-MS/MS have been used for the simultaneous quantification of penicillins in milk.

Determination of fluoroquinolones in chicken tissues by LC-coupled electrospray ionisation and atmospheric pressure chemical ionisation.

The aim of this work was to develop a method for determining seven quinolones (ciprofloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid and flumequine) in chicken muscle by LC coupled to MS. Two ionisation techniques, ESI and atmospheric pressure chemical ionisation (APCI) were compared using standard solutions. LOD and LOQwere determined under the optimised conditions for the two sources.

Effective sorbents for solid-phase extraction in the analysis of quinolones in animal tissues by capillary electrophoresis.

In this work, several commercial sorbents (Zorbax C18, Bond Elut C18, Isolute ENV+, Oasis HLB, Oasis MAX, SDB-RPS, and MPC-SD) were compared for the solid-phase extraction of the series of quinolones regulated by the European Community in chicken tissues in order to establish a method for the determination of this series of quinolones by capillary electrophoresis and diode array detection. Sorbents were chosen in order to achieve maximum recoveries and optimal clean-up efficiency. Better results were obtained using SDB-RPS and Oasis MAX which would provide suitable limits of detection, below of the maximum residue limits (MRLs) regulated.

Determination of residues of enrofloxacin and its metabolite ciprofloxacin in chicken muscle by capillary electrophoresis using laser-induced fluorescence detection.

A method for the residue analysis of the veterinary antimicrobial agent enrofloxacin and its active desethyl metabolite ciprofloxacin in chicken muscle tissue has been developed and validated. The detection of the analytes was performed by laser-induced fluorescence (LIF) detection using a HeCd laser (lambda(ex) = 325 nm) providing an enhancement in sensitivity and selectivity compared to conventional UV detection. The assay has been validated with satisfying results.