83 research outputs found

    Development and validation of a liquid chromatography/tandem mass spectrometry method for quantitative determination of amoxicillin in bovine muscle

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    A simple, quick and economical liquid chromatographic/tandem mass spectrometry (LC–MS/MS) method for the quantitative determination of amoxicillin in bovine muscle was developed and validated. The sample preparation procedure involved a liquid extraction with water, followed by a protein precipitation step with acetonitrile. The extract was purified by a liquid–liquid partition with dichloromethane and the upper aqueous layer was directly injected into the LC–MS/MS system. Chromatographic separation was achieved on a reversed phase column, using a mixture of acetonitrile, water and 0.005% formic acid in water as mobile phase. Gradient elution was performed at a flow rate of 0.2 mL/min. Amoxicillin was detected using positive electrospray ionization in selected reaction monitoring (SRM) mode and was quantified using terbutaline as internal standard. The responses for standards prepared in solvent and in matrix were equivalent and additionally the absence of signal suppression was confirmed by the post column infusion technique. Amoxicillin stability in standard solution and in matrix was investigated at different times and storage conditions. Amoxicillin standards prepared in water were stable on storage up to 20 days at -20°C. Amoxicillin stability in matrix (spiked bovine muscle samples) was assessed up to 15 days at -20°C. The method was validated according to the parameters requested by European Commission Decision 2002/657/EC in terms of specificity, linearity, trueness, precision, decision limit (CC) and detection capability (CC). All the trueness values fell within a range between 14.5% and 6.3%. Precision values for all levels of concentration tested were lower than the relative limit calculated by the Horwitz equation. The amoxicillin MRL is set at 50 g/kg and the CC and CC of the method were 61.2 g/kg and 72.4 g/kg, respectively

    Immunogenicity, reactogenicity and adherence to a combined hepatitis A and B vaccine in illicit drug users

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    Aims The use of illegal drugs is associated with an increase in infective risk for the hepatitis viruses, against which the vaccination of drug users (DUs) is recommended unanimously. The aim of the study was to determine tolerability, adherence and immune response of a combined vaccine providing dual protection against hepatitis A virus (HAV) and hepatitis B virus (HBV). Methods The vaccine was administered to 38 DU, attending three public health centres for drug users in northern Italy, with a three-dose schedule (at 0, 1 and 6 months). The vaccine was well tolerated: only one adverse reaction (fever) was recorded after the 110 doses administered (0.9%). The vaccine schedule was completed successfully in 35 cases (92.1%). At month 8, in 34 subjects (89.5%) antibody response was evaluated: all showed seroprotection for HAV and in 33 subjects (97.1%) for HBV. Conclusions The vaccine, studied for the first time in DUs, proved to be safe, well accepted and immunogenic; anti-HAV response was 1272 mIU/ml and 1726 mIU/ml for anti-HBV, titres lower than reported in literature for the general population. This study suggests that DUs who are HAV/HBV-negative could be vaccinated with combined vaccine

    The significance of mycotoxins in aquaculture and commercial pet foods.

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    The contamination of feedstuffs with mycotoxins poses a serious threat to the health of both companion and farm animals. Despite the carnivorous habits of pet animals such as dogs and cats as well as of most farm fishes, the increasing utilization of vegetable feedstuffs has considerably increased the exposure of these animals to mycotoxins

    Figli di nessuno: lo smoking status dei tossicodipendenti da eroina in terapia sostitutiva. Confronto con i fumatori della popolazione generale intenzionati smettere.

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    Tobacco addiction, a major world-wide health problem, is widely recognized as a chronic, relapsing mental disorder, disproportionaltely affecting people with psychiatric comorbidity that smoke and develop smoke-related diseases more than smokers without mental illness. Paradoxically, these patients receive fewer invitations to stop and less support in the process of smoking cessation. The treatment of smoking addiction may give good results in these patients if properly performed. First-line drugs proved to be effective also for these patients. Aim of this review is to present scientific data in the literature in order to make a breach in the wall of neglect that too often surrounds people nicotine dependent with mental illness and to give an opportunity to these patients, generally suffering of severe smoking dependence. Even more hoped would be that the local mental health services to take charge of this serious problem by providing pharmacological treatment and behavioral support to their own patients

    Fumonisin B1 and B2 in dry dog food: preliminary study on commercial samples

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    A reliable liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the identification and quantification of fumonisin B1 (FB1) and fumonisin B2 (FB2) in complete and complementary formulations of dry dog foods has been optimized and validated. The sample preparation consists of an extraction step followed by immunoaffinity clean-up. Method performance characteristics were evaluated spiking blank samples on multiple levels in four replicates. The method showed appropriate performance characteristic: good values of recovery (> 95.9 %) and precision (RSD < 6.8 %), as well as satisfying linearity of calibration curves (r2 ≥ 0.99). The limits of quantification (LOQs) and detection (LODs) were 0.100 μg/g and 0.005 μg/g, respectively, both in complete and complementary dry dog foods and both for FB1 and FB2. This method was applied to 41 commercial samples in order to tests its efficacy and gain some preliminary data about fumonisins contamination in dog foods available in the Italian market. Fumonisin FB1 and FB2 were detected in all samples analyzed and in particular 63.41 % and 56.10 % of the samples showed concentrations above the LOQs of FB1 and FB2, respectively. The levels of contamination quantified ranged between LOQs and 5.87 μg/g and 2.93 μg/g for FB1 and FB2, respectively. Among the complete dry dog foods, standard formulations generally showed an average fumonisins contamination higher than premium formulations. The guidance value of 5 μg/g set by Commission Recommendation 2006/576/EC for the sum of FB1 and FB2 was exceeded in two samples: one standard complete dry dog food showed a total fumonisins contamination of 5.19 μg/g and one complementary food a contamination of 8.80 μg/g

    Optimization and validation of an UPLC-MS/MS method for determination of vitamin B12 in milk and dairy products

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    An ULPC-MS/MS method was optimized in order to measure cobalamins in naturally enriched raw milk and to evaluate their fate during thermal treatments and along the process of cheese making. After addition of methotrexate as internal standard, samples were submitted to heat treatment in presence of cyanide that converts all the less stable cobalamins in cyanocobalamin; then a purification was performed by a solid phase extraction (SPE) step. Reverse phase UPLC separation coupled to tandem mass spectrometry provides a fast and reliable determination

    Preliminary investigation on perfluorinated compounds presence in italian and french cow milk by means of a newly developed and validated LC-MS/MS method

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    Perfluorinated compounds (PFCs) are fully-fluorinated man-made substances largely employed in a wide range of industrial and consumer applications, such as food packaging, fire fighting foams, detergents and non-stick cookware. Even if the introduction of these chemicals dates back to the 1950s, little attention has been given to their potential effects on both environment and human health, but the increasing interest on these substances has recently raised serious concerns about their carcinogenic activity, effects on reproduction and liver and kidney toxicity. Human exposure to PFCs is mainly through diet, for this reason the European Union issued the Commission Recommendation 2010/161/EU on the monitoring of these contaminants in food in the Member States. Perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA) are the two most important and investigated compounds of this group, being added to the POPs (Persistent Organic Pollutants) listing on the Stockholm Convention. Aim of this work was to carry out a preliminary monitoring on the presence of these two molecules in cow milks commercially available in Italy and France. The cooperation between the two laboratories has led to the development of an efficient method for the detection of various PFCs in milk, based on a liquid- liquid extraction with organic solvent followed by two purification steps through SPE cartridges and injection in LCMS/ MS system. The application of this method to several milk samples from Italy and France has shown similar results in the two countries, with PFOS and PFOA detected in most cases and at similar concentrations. However, these levels of contamination were sensibly lower than the ones observed in various studies on breast milk, and even more if compared to the data available on fish and seafood monitoring. In consideration of the above, cow milk seems not to be a major source of PFCs exposure in human die
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