In this study, a rapid and simple analytical method was proposed, based on protein precipitation as sample preparation for simultaneous determination of tetracycline, oxytetracycline, penicillin G and ceftiofur in raw milk by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The method was applied to raw milk samples from dairy cows medicated with tetracycline for subclinical mastitis. Samples were collected from the adjacent teat to the teat treated with tetracycline of eight different cows at 24, 48, 72 and 96 h after treatment. The limits of quantification of the proposed method ranged between 1 and 5 ng g-1 and limits of detection ranged between 0.1 and 0.5 ng g-1. The recoveries ranged from 61 to 111% and the linear range was 1 to 2064 ng g-1 for tetracycline and oxytetracycline, and 5 to 2064 ng g-1 for penicillin G and ceftiofur. Approximately 75 and 63% of the treated animals revealed more tetracycline than legally recommended at 72 and 96 h since last treatment, respectively.

The investigation of the distribution of antioxidant compounds between emulsions phases, employing natural sources of these compounds directly in the emulsions, is rarely addressed. The use of ultra performance liquid chromatography coupled to a mass spectrometer (UPLC-MS), combined with accelerated oxidation tests and oxygen radical absorbance capacity method (ORAC), using the fluorescein (FL) decay curve (ORACFL) assay, enable an improved evaluation of the distribution of the antioxidant compounds and their lipid protection abilities. The lipid protection tendency observed was in agreement with the polar paradox theory. The ORACFL results reported here are higher than other reported in the literature, even when performing a sample extraction directly into one of the emulsion phases, thus demonstrating the effectiveness of this direct addition regarding the antioxidant activity. The analysis of the mass spectra of the emulsions enabled to verify the existence and distribution of some phenolic compounds in both phases. The direct extraction in the aqueous and oil phases of the emulsion increased, in a general way, the amount of identified compounds in each phase.

This study evaluated the incorporation of β-carotene, lutein and lycopene into tilapia (genetically improved farmed tilapia, GIFT) fillets supplemented through 0, 20 and 40 days, and their influence on the fatty acid composition and nutritional quality of raw and grilled fillets. A control diet and a diet containing those carotenoids were elaborated with the same lipid source (soybean oil). For carotenoids analysis, the extraction was performed according to the literature, employing acetone and hexane. The relative intensities of m/z ratios of those carotenoids ions were obtained by ultraperformance liquid chromatography-tandem mass spectrometry with chemical ionization at atmospheric pressure (UPLC-APCI MS/MS), and an increase of carotenoid concentration in the supplemented fillets was observed, especially after the grilling process (180 ºC for 15 min). An increase in the concentration of total carotenoids in grilled fillets (75 and 35% higher than raw fillets, for 20 and 40 days of supplementation, respectively, corresponding to 8.32 and 2.42 µg β-carotene g-1 sample) was also observed. Therefore, the carotenoids promoted the stability of lipid oxidation in grilled samples; fact that can be correlated with antioxidant effect of these compounds, it can be also explained by the breakdown of carotenoids physical barrier and the conditions used in the grilling process. Moreover, acceptable n-6/n-3 indices and recommended polyunsaturated fatty acids/saturated fatty acids (PUFA/SFA) values were observed in supplemented fillets. Consequently, lutein, β-carotene and lycopene were considered viable as additive on fish diet, since the supplementation promoted the increase of food quality, even after preparation for consumption.

Omega-3 fish oil supplements are widely consumed as source of eicosapentaenoic (EPA) and docosahexaenoic (DHA) acids, presenting beneficial effects on human health. This study aimed to evaluate fifteen brands of omega-3 fish oil supplements available in Brazilian market in order to estimate the Brazilian reality regarding those supplements. Twelve fatty acids were quantified by gas chromatography with a flame ionization detector (GC-FID), and lipid profile were obtained via mass spectrometry fingerprinting using direct electrospray ionization mass spectrometry (ESI-MS) to assess the form in which fatty acids are present as well as the possible fraud existence. Among all analyzed samples, thirteen brands were revealed as EPA and DHA sources (90.2-440.3 and 77.8-302.3 mg g-1lipid, respectively) in triacylglycerols (TAG) or ethyl esters (EE) form. However, two brands were discovered with addition of large amounts of soybean oil, leading the final consumer to ingest this low-cost oil believing that they are consuming adequate doses of EPA and DHA.

The objective was identifying three different anthocyanidins and to quantify them in six different berries. Results from the conventional method (using extraction with hydrochloric acid) were compared with data from the proposed method (without acid extraction). The following figures of merit were used: linearity, accuracy, linear range, limits of detection and quantification, using an ultra performance liquid chromatography (UPLC) coupled to a triple quadrupole mass spectrometer equipped with an electrospray ionization source. The separation of anthocyanidins can be achieved in a much smaller period of time (1.30 min) and the cyanidin from Morus nigra L., Rubus idaeus L. and Vaccinium myrtillus L. was found in higher amounts in extracts obtained from the proposed method. Proposed mechanisms of mass spectrometry (MS/MS) collisional induced dissociation for pelargonidin, cyanidin and delphinidin were obtained and this is the first time that concentrations of anthocyanidins present in fruits of Solanum americanum Mill. were reported.

<p>As farmácias de manipulação têm sido citadas por alguns atletas como sendo responsáveis pela manipulação de cápsulas contaminadas com fármacos proibidos pelo Comitê Olímpico Internacional (COI). Portanto, o presente estudo foi realizado para quantificar o montante de resíduo remanescente nos equipamentos e utensílios usados para manipular cápsulas após o procedimento padrão de limpeza. Para este propósito, o captopril (CAP) e o ácido acetilsalicílico (ASA) foram usados por serem fármacos de difícil remoção e a hidroclorotiazida (HTZ), por ser um fármaco proibido pelo COI. As quantidades de resíduos encontradas nos equipamentos após a limpeza foram 181,0 ± 91,8, 1208 ± 483,8 e 431,7 ± 71,3 ppm para ASA, CAP e HTZ, respectivamente. A manipulação contínua dos fármacos seguida pelo procedimento de limpeza mostrou acúmulo de resíduo linear para ASA (r²=0,96) e CAP (r²=0,88). A quantidade de resíduo de CAP foi maior que o limite de impureza sugerido pelo FDA (>0,1%), mas não para HTZ, mas mesmo assim, o resíduo de HTZ pode ser detectado na urina dos atletas submetidos aos testes do COI. Em conclusão, as farmácias de manipulação deveriam, portanto, melhorar o procedimentos de limpeza e testá-los para que alcancem limites abaixo de 10 ppm para evitar contaminação nos outros produtos.</p>

<p>Compounding pharmacies have been cited by some athletes as being responsible for compounding capsules contaminated with drugs banned by the International Olympic Committee (IOC). Therefore, the present study was carried out to quantify the amount of residue remaining in the equipment and utensils used for compounding capsules after standard cleaning procedures. For this purpose, captopril (CAP) and acetylsalicylic acid (ASA) were used since these are hard to clean, in addition to hydrochlorothiazide (HTZ) as a banned drug by the IOC. The amounts of residues found in the equipment were: 181.0 ± 91.8, 1208 ± 483.8 and 431.7 ± 71.3 ppm for ASA, CAP and HTZ, respectively. The continuous compounding of these drugs, followed each time by the standard cleaning procedure, showed a linear accumulation of residues for ASA (r²=0.96) and CAP (r²= 0.88). The residues quantified were greater than the FDA limit for impurities for CAP (>0.1%) but not for HTZ. However, the HTZ residue may be detected in the urine of athletes on IOC tests. Therefore, it was concluded that compounding pharmacies should therefore improve their cleaning procedures and test these in order to attain limits below 10 ppm, thereby avoiding the contamination of other products.</p>

O uso de cateter venoso central (CVC) e antibióticos de amplo espectro estão entre os principais fatores de risco para o desenvolvimento da candidemia em pacientes internados em unidades de terapia intensiva (UTI). É conhecido que alguns antibióticos aumentam a resistência das leveduras aos antifúngicos azólicos. Assim, o objetivo deste estudo foi avaliar se leveduras presentes em colonização de CVC expostas a antibióticos que atuam em parede celular se beneficiam de uma redução na suscetibilidade ao fluconazol e voriconazol e se obtêm maior capacidade de formar biofilme. Candida albicans, C. tropicalis, C. glabrata,C. parapsilosis e C. guilhermondii foram semeadas em placas de Mueller-Hinton Agar, com gradientes de antibióticos (cefepima, meropenem, vancomicina e piperacilina-tazobactam). A suscetibilidade e a formação de biofilme das leveduras foram testadas antes e após a exposição aos antibióticos. Nenhum dos antibióticos provocou alterações detectáveis in vitro sobre a suscetibilidade das leveduras aos antifúngicos ou à capacidade de formar biofilme. Estes resultados sugerem que o aumento da candidemia na UTI não seria atribuído a possíveis alterações provocadas nas leveduras e sim pelo enfraquecimento da condição geral do paciente após longa exposição à infecção.

The use of central venous catheters (CVC) and broad-spectrum antibacterials are among the main risk factors for the development of candidemia in patients admitted to intensive care units (ICU). It is known that some antibacterials increase the resistance of these yeasts to azole antifungals. Thus, the aim of this research was to determine whether yeast present in CVC colonizations previously exposed to cell-wall targeted antibacterials benefit from a reduction in susceptibility to fluconazole and voriconazole, facilitating their ability to form biofilms. Candida albicans, C. tropicalis, C. glabrata, C. parapsilosis and C. guilhermondii were seeded into antibacterial (cefepime, meropenem, vancomycin, and piperacillin-tazobactam) gradient plates produced in Mueller-Hinton Agar. The susceptibility to fluconazole and voriconazole and the biofilm formation of the yeasts were tested before and after exposure to the antibacterials. None of the antibacterials exerted a significant effect on the in vitro susceptibility of the yeasts to the antifungal agents or on their ability to form biofilms. These results suggest that increased candidemia in ICU patients is not attributable to possible alterations in the yeasts, but is more likely caused by a weakening of the patient's general condition after long exposure to infection.