Determination of ochratoxin A (OTA) in wines requires a cleanup step using solid phase extraction (SPE). Immunoaffinity columns are commonly the columns of choice but due to its high cost, other SPE columns have been assayed without optimal results. The present work reports an optimized and validated liquid chromatographic method for a fast and selective quantification of OTA in wines using C18 columns for cleanup. Chromatographic conditions were optimized using a central composite design, establishing the following optimal conditions: acetonitrile/water/acetic acid (59.5:39.5:1.0 v/v/v) as mobile phase, flow rate of 1.2 mL min?1, and column temperature of 30 °C. With these conditions, OTA had a retention time (~4 min) up to five times lower than those reported earlier. Regarding validation, calibration data (n?=?8) fitted a linear regression model with a determination coefficient (R2) of 0.9992. Repeatability (relative standard deviation (RSD)) and intermediate precision (RSD) in matrix showed values of 1.3 % (n?=?6) and 0.8 % (n?=?3), respectively. Recoveries at five levels ranged from 87.2 to 118.9 % (mean RSD of 7.4 %). Fifty-three samples from different origins were analyzed, finding only seven samples (13 %) with quantifiable OTA content (0.15–0.26 μg L?1). According to the levels found, the contribution of wine consumption to OTA daily intake was at least 58 times lower than the current tolerable daily intake. In view of optimization and validation results as well as its applicability to real samples, this method could be considered a good alternative for routine analysis of OTA in wines. 相似文献
A synthetic gene coding for human growth hormone was expressed in Lactococcus lactis. The presence of the recombinant protein was assayed and quantified using ELISA tests. Human growth hormone was detected at high concentrations and displayed a biological activity similar to the one shown by commercial human growth hormone. 相似文献
This paper studies the synthesis of structured triacylglycerols (STAGs) rich in palmitic and docosahexaenoic acids (PA and DHA) at sn-2 position and oleic acid (OA) at sn-1,3 positions by a four step process. First, triacylglycerols (TAGs) were obtained with 63–66 mol PA/100 mol total fatty acids and 10 mol DHA/100 mol by acidolysis of tuna oil and commercial PA, catalyzed by the non-positionally specific lipase Novozym 435. Then these TAGs were purified neutralizing the free fatty acids (FFAs) by KOH hydroethanolic solutions and extracting TAGs with hexane; these TAGs were completely recovered as pure TAGs (without FFAs). The third step involved the displacement of fatty acids located at sn-1,3 positions by acidolysis of PA and DHA enriched TAGs with OA rich FFAs, catalyzed by the sn-1,3 specific lipase DF from Rhizopus oryzae, immobilized on Accurel MP-1000; TAGs with 67 mol OA/100 mol at sn-1,3 positions and 52.1 and 15.4 mol PA and DHA, respectively, per 100 mol at sn-2 position were obtained. Both acidolysis reactions were carried out in stirred tank reactors (STRs) with lipase both dispersed in the reaction medium and contained in a cartridge filter attached to the stirrer rod. Finally STAGs were purified and obtained with yields of over 80 mol STAGs/100 mol STAGs in the reaction product (no FFAs were detected). 相似文献
A dietary rosemary extract (RE) was tested to extend the shelf life of raw lamb meat. Lambs were supplemented with 0.6 mg kg−1 RE during fattening (from 13 to 25 kg live weight). Meat spoilage (total viable counts, psycrophilic bacteria, Enterobacteriaceae, molds and yeasts), TBARS, CIE L*a*b* color and the sensory traits of lamb cuts were analyzed on days 0, 7, 14 or 21 under retail display conditions (70/30 O2/CO2 atmosphere, 2 °C temperature and 1600 lx lighting). Supplementation of the lamb diet with RE was effective (P < 0.05) in prolonging the time chilled-packed lamb cuts could be kept under retail display conditions. Dietary rosemary clearly inhibited lipid oxidation and rancidity, and was moderately efficient in preventing sensory deterioration and microbial spoilage. Although the results concerning meat preservation were limited, the dietary use of rosemary extracts in lambs seems to be promising as a nutritional strategy for improving meat quality. 相似文献
The visualization of microtubules by combining optical and electron microscopy techniques provides valuable information to understand correlated intracellular activities. However, the lack of appropriate probes to bridge both microscopic resolutions restricts the areas and structures that can be comprehended within such highly assembled structures. Here, a versatile cyclometalated iridium (III) complex is designed that achieves synchronous fluorescence–electron microscopy correlation. The selective insertion of the probe into a microtubule triggers remarkable fluorescence enhancement and promising electron contrast. The long-life, highly photostable probe allows live-cell super-resolution imaging of tubulin localization and motion with a resolution of ≈30 nm. Furthermore, correlative light–electron microscopy and energy-filtered transmission electron microscopy reveal the well-associated optical and electron signal at a high specificity, with an interspace of ≈41 Å of microtubule monomer in cells. 相似文献
To prepare an efficient supercapacitor, an activated carbon from agave wastes was prepared and their electrochemical performance was evaluated as a novel electrode for supercapacitor. The carbon was prepared by two thermal pyrolysis processes under nitrogen atmosphere. The first pyrolysis was achieved at 500 °C until the charring of the bagasse; in the second pyrolysis step, the char was impregnated with different mass ratios of KOH (1:2–1:4) and thermally treated at 800 or 900 °C, for 1 h under N2 flow. The textural analysis showed that the activated carbon had a specific surface area of 1462 m2 g?1 and depicted a type I isotherm (IUPAC) characteristic of a microporous carbon. Raman spectroscopy and XRD measurements confirm that the activated carbon contains a small graphitization degree and a disordered structure. The electrochemical study of the symmetric carbon supercapacitor was carried out in 1 M Li2SO4 solution as the electrolyte. The electrochemical performance of the coin cell supercapacitor was evaluated under an accelerated aging floating test consisting of potentiostatic steps at different voltages (1.5, 1.6 and 1.8 V) for 10 h followed by galvanostatic charge/discharge sequences, and the overall procedure summarized a floating time up to 200 h. The highest capacitance was observed at a floating voltage of 1.5 V, with a large initial specific capacitance of 297 F g?1.
Today in reliability analysis, the most used distribution to describe the behavior of devices is the Weibull distribution. Nonetheless, the Weibull distribution does not provide an excellent fit to lifetime datasets that exhibit bathtub shaped or upside‐down bathtub shaped (unimodal) failure rates, which are often encountered in the performance of products such as electronic devices (ED). In this paper, a reliability model based on the exponentiated Weibull distribution and the inverse power law model is proposed, this new model provides a better approach to model the performance and fit of the lifetimes of electronic devices. A case study based on the lifetime of a surface‐mounted electrolytic capacitor is presented in this paper. Besides, it was found that the estimation of the proposed model differs from the Weibull classical model and that affects the mean time to failure (MTTF) of the capacitor under analysis. 相似文献