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Mycotoxins' exposure by inhalation and/or dermal contact can occur in different branches of industry especially where heavily dusty settings are present and the handling of dusty commodities is performed. This study aims to explore the possible contribution of the occupational exposure to aflatoxins by analysing urine samples for the presence of aflatoxins B 1 and M 1 and aflatoxin B 1 -N 7 -guanine adduct. The study was conducted in 2017 on two groups of volunteers, the workers group, composed by personnel employed in an Italian feed plant (n = 32), and a control group (n = 29), composed by the administrative employees of the same feed plant; a total of 120 urine samples were collected and analysed. A screening method and a quantitative method with high-resolution mass spectrometry determination were developed and fully validated. Limits of detections were 0.8 and 1.5 pg/mL urine for aflatoxin B 1 and M 1 , respectively. No quantitative determination was possible for the adduct aflatoxin B 1 -N 7 -guanine. Aflatoxin B 1 and its adduct were not detected in the analysed samples, and aflatoxin M 1 , instead, was found in 14 samples (12%) within the range 1.9-10.5 pg/mL urine . Only one sample showed a value above the limit of quantification (10.5 pg/mL urine ). The absence of a statistical difference between the mean values for workers and the control group which were compared suggests that in this specific setting, no professional exposure occurs. Furthermore, considering the very low level of aflatoxin M 1 in the collected urine samples, the contribution from the diet to the overall exposure is to be considered negligible.

A liquid chromatographic-tandem mass spectrometric (LC-MS-MS) method has been developed for the determination of trenbolone in bovine urine and serum. The aim was a control of the misuse of trenbolone in food-producing animals. The procedure involved, in both cases, a preliminary solid-phase clean-up followed by a liquid-liquid extraction for urine samples after a preliminary enzymatic hydrolysis. The extracts have been directly analysed by reversed-phase LC-MS-MS in selected reaction monitoring (SRM), acquiring two diagnostic product ions from the chosen precursor [M+H](+). The procedures were validated across the concentration range of 1-1500 ng/ml. The linearity, the inter- and intra-day accuracy and precision have been determined. The procedure was specific and the accuracy values were better than 20% at the limit of quantitation of spiked samples. The limit of quantification (LOQ) and the limit of detection (LOD) were, respectively, 1 ng/ml and 350 pg/ml for urine and serum. According to the draft, SANCO/1805/2000, we determined the decision limit CCalpha and the detection capability CCbeta. The recovery values for urine ranged from 87 to 128%, and for plasma the recovery was 70+/-4%. The procedure proved to be simple and suitable for routine and confirmatory purposes such as those developed for residue studies.

Abstract: In this work hydroxycinnamic acid esters of tartaric acid (mono-p-coumaroyl tartaric acid, monocaffeoyl tartaric acid, monoferuloyl tartaric acid esters) were separated, identified and quantified in several red wines by high performance liquid chromatography coupled with tandem mass spectrometry. The method features direct analysis of wines with no preparation and analysis of grape juice with minimum sample manipulation. For the identification was used both a triple quadrupole and a quadrupole–Tof, while for the quantification a triple quadrupole. At the same time two impurities, due to interfering substances coming from methanol (stored in bottles with polypropylene tops without Teflon protection), were characterised. These impurities had the same molecular weight as the investigated compounds. [Copyright &y& Elsevier]

Abstract: Boldenone is an androgenic anabolic steroid (AAS) intensively used for growth promoting purposes in animals destined for meat production and as a performance enhancer in athletics. Therefore its use is officially banned either in animals intended for consumption or in humans. Because most anabolic steroids are completely metabolized and usually no parent steroid is excreted, metabolite identification is crucial to detect the illegal use of anabolic steroids either in humans or in livestock. The aim of this work is the investigation of 17β-boldenone and its main metabolites, 17β-sulphate, 17β-glucuronide, 5β-androst-1-en-17β-ol-3-one and 17α-boldenone, in human and bovine urine developing a multiresidue analysis. After solid phase extraction of urine samples, detection is carried out by high performance liquid chromatography–tandem mass spectrometry in multiple reaction monitoring. The average recovery for all the investigated compounds is above 70%. The developed method is very easy, quick and highly specific. Linearity, precision, decision limit and detection capability were also evaluated. [Copyright &y& Elsevier]