Determination of capsaicin and dihydrocapsaicin in capsicum fruits by liquid chromatography-electrospray/time-of-flight mass spectrometry

A simple, highly selective, sensitive, and reproducible liquid chromatography-electrospray ionization/time-of-flight mass spectrometry method has been developed for the direct and simultaneous determination of capsaicin and dihydrocapsaicin in Capsicum fruit extracts. Capsaicin and dihydrocapsaicin are the two major members of the so-called capsaicinoid family, which includes other minor analogues, and usually account for at least 90% of the pungency trait in Capsicum fruits. Chromatographic separation of capsaicin and dihydrocapsaicin was achieved with a reversed-phase chromatography column, using a gradient of methanol and water. Quantification was done using as an internal standard (4,5-dimethoxybenzyl)-4-methyloctamide, a synthetic capsaicin analogue not found in nature. Analytes were base-peak resolved in less than 16 min, and limits of detection were 20 pmol for capsaicin and 4 pmol for dihydrocapsaicin. The intraday repeatability values were lower than 0.5 and 12% for retention time and peak area, respectively, whereas the interday repeatability values were lower than 0.6 and 14% for retention time and peak area, respectively. Analyte recoveries found were 86 and 93% for capsaicin and dihydrocapsaicin, respectively. The method developed has been applied to the identification and quantification of capsaicin and dihydrocapsaicin in fruit extracts from different Capsicum genotypes, and concentrations found ranged from 2 to 6639 mg kg(-1).     

Lipid class composition of the microalga Pavlova lutheri: eicosapentaenoic and docosahexaenoic acids

The lipid classes of Pavlova lutheri, cultivated in semicontinuous mode, were studied by thin-layer chromatography and gas chromatography in attempts to describe the distribution of fatty acid residues within its lipid pool, with special emphasis on eicosapentaenoic (C20:5n-3, EPA) and docosahexaenoic (C22:6n-3, DHA) acids. Neutral lipids and glycolipids were the major constituents and accounted for approximately 57 and 24% of the total fatty acid residues (TFA), respectively. Phospholipids accounted for approximately 10% of TFA. Two lipid classes, acylated steryl glycosides (SG) and diphosphatidylglycerols (DPG), were eventually identified in P. lutheri for the first time. The nonpolar fraction was mainly composed of triacylglycerol (TAG), whereas the polar fraction was mainly composed of monogalactosylacylglycerols (MGDG). The distribution of total EPA and DHA within the lipid pool was calculated in attempts to ascertain the quality of said microalgae as a feed source, as well as the possibility of enhancement of individual fatty acid production and extraction thereafter. EPA was especially concentrated in MGDG (approximately 45%) and TAG (approximately 33%); conversely, DHA was dispersed through various classes, especially within TAG (approximately 27%), DPG (approximately 22%), and betaine lipids (21%).     

Voltammetric assay for the aging of beer

A new method for the evaluation of beer aging, based on a voltammetric analysis of beer distillates, is described. By measuring the current of both acetaldehyde and sulfite voltammetric peaks it is possible to distinguish between fresh, naturally aged, and artificially aged beers. The results obtained for the ratio of acetaldehyde and SO(2) currents correlate well with those given by an expert sensory panel. The kinetics of the combining reaction of sulfite with acetaldehyde was followed for different acetaldehyde/SO(2) molar ratios by using a programmed voltammetric procedure. The formation of an acetaldehyde-sulfite adduct is rapid, and the reaction equilibrium is reached after 30 min, which is in accordance with the results previously obtained by other methods. This voltammetric-based approach seems to be a new attractive tool for detecting chemical equilibria of the addition of sulfite to carbonyls in beer model systems.     

Analysis of ochratoxin a in coffee by solid-phase cleanup and narrow-bore liquid chromatography-fluorescence detector-mass spectrometry

A method for the analysis of ochratoxin A (OTA) in green and roasted coffee has been developed. OTA was extracted from coffee with 1% NaHCO(3), and the extract was filtered and purified by solid-phase cleanup using a polymeric column that exhibits reversed-phase and anion-exchange functionalities. OTA was analyzed on a narrow-bore reversed-phase C(18) HPLC column with acetonitrile/water (0.1% formic acid) (40:60) as mobile phase and quantified with a fluorescence detector. The presence of OTA in coffee was confirmed by single-quadruple mass spectrometry using an electrospray ionization source. The method has been validated, obtaining a recovery of 82.5% and a detection limit of 0.1 ng/g. It has been applied to 20 coffee samples from various countries and different manufacturers with no detection of OTA.     

Changes of pore morphology, infiltration and earthworm community in a loamy soil under different agricultural managements

Earthworm activity produces changes at different scales of soil porosity, including the mesoporosity (between 1.000 and 30 μm eq. dia.) where both water retention and near-saturated infiltration take place. At this scale, the structural changes are poorly described in temperate agricultural systems, so we do not yet fully understand how these changes occur. The present study was conducted to determine the relationships between the morphology of the mesopores, which is mainly affected by earthworm activity, and the hydrodynamic behaviour (near-saturated infiltration) of topsoil under different agricultural managements inducing a large range of earthworm populations.Investigations were carried out at the soil surface in three fields under different management practices giving rise to three different earthworm populations: a continuous maize field where pig slurry was applied, a rye-grass/maize rotation (3/1 year, respectively) also with pig slurry, and an old pasture sown with white clover and rye-grass.Pore space was quantified using a morphological approach and 2D image analysis. Undisturbed soil samples were impregnated with polyester resin containing fluorescent pigment. The images were taken under UV light, yielding a spatial resolution of 42 μm pixel⁻¹. Pores were classified according to their size (which is a function of their area) and their shape. Hydraulic conductivity K(h) was measured using a disc infiltrometer at four water potentials: −0.05, −0.2, −0.6, and −1.5 kPa. The abundance and ecological categories groups of earthworms were also investigated.Continuous soil tillage causes a decrease in both abundance and functional diversity (cf. maize compared with old pasture) when soil tillage every 4 years causes only a decrease in abundance (cf. rotation compared with old pasture). There were no relationships between total porosity and effective porosity at h=−0.05 kPa. Image analysis was useful in distinguishing the functional difference between the three managements. Fewer roots and anecic earthworms resulted in fewer effective tubular voids under maize. There were fewer packing voids in the old pasture due to cattle trampling. Greater hydraulic conductivity in the pasture phase of rotation may arise from a greater functional diversity than in the maize and absence of cattle trampling compared with the pasture. We point to some significant differences between the three types of agricultural management.A better understanding is required of the influence of agricultural management systems on pore morphology. This study provides a new methodology in which we consider the earthworm activity as well as community in order to assess the effects of agricultural management on soil structure and water movement.     

Isolation and structural characterization of new acylated anthocyanin-vinyl-flavanol pigments occurring in aging red wines

Three newly formed pigments were detected and isolated from a 2-year-old Port wine through TSK Toyopearl HW-40(S) gel column chromatography and characterized by UV-visible spectrophotometry, NMR, and mass spectrometry (ESI/MS). (1)H NMR and (13)C NMR data for these pigments obtained using 1D and 2D NMR techniques (COSY, NOESY, gHSQC, and gHMBC) are reported for the first time. The structure of the pigments was found to correspond to the vinyl cycloadducts of malvidin 3-coumaroylglucoside bearing either a procyanidin dimer or a flavanol monomer ((+)-catechin or (-)-epicatechin). Additionally, conformational analysis was performed for one of these newly formed pigment using computer-assisted model building and molecular mechanics. A chemical nomenclature is proposed to unambiguously name this new family of anthocyanin-derived pigments.     

Stabilized municipal sewage sludge addition to improve properties of an acid mine soil for plant growth

Purpose

Degraded soils, such as those encountered in areas of mine activities, need to be ameliorated by liming to correct soil acidity and by addition of organic inputs to improve soil properties and fertility.

Materials and methods

Non-amended mine soil and soil amended with stabilized sewage sludge were incubated for 45 days. Soil physicochemical and biological indicators were periodically measured along incubation and other enzyme activities at the end of incubation. In improved soils, a study of plant development in 250-g pots was carried out with three vegetal species: tomato, rye grass and ahipa. Germination and mortality rates, biomass production and photosynthetic pigments were measured.

Results and discussion

Soil incubation with sewage sludge slightly increased soil pH and led to an enhancement of soil electrical conductivity, organic carbon and dehydrogenase activity, especially for the higher doses (5 and 10%). However soil respiration was more promoted with the 2% dose, pointing to a possible toxic effect of the sludge. At the end of incubation, physicochemical and biological properties were in general enhanced. Biomass production was improved in tomato and rye grass by sewage sludge addition (more at the 2% dose), whilst ahipa growth was not affected by sewage sludge treatments. Tomato mortality reached 73% with high sludge doses (10%).

Conclusions

According to this set of parameters, amendment with sewage sludge of a limed acid mine soil would be considered as a good strategy for soil amelioration in view of plant establishment and development.     

Variations in mercury and other trace elements contents in soil and in vine leaves from the Almadén Hg-mining district

Purpose

Vines (Vitis vinifera, L.) are a very important agricultural resource for Spain in general and for the Castilla-La Mancha region in particular, providing important productions of wines. Grapes and raisins are used for direct consumption too. In this work, we study analytical constraints regarding metallic trace elements uptake, focusing on Hg, from vines growing in the Almadén mercury mining district, the world's largest producer of this element, inactive nowadays.

Materials and methods

The study started with the analysis of these metals in soils and sets of vines leaves from seven sites located at different distances from the Almadén Hg mine. The samples of soils were dried at ambient temperature for 1 week. They were then sifted (<2 mm) and were stored for subsequent analysis. The leaves were dried and the leaf blade and petiole were separated. About 2 g of each sample were hand milled and analyzed using the same fluorescence spectrometer. Total mercury in soils and vine leaves were determined using a Lumex RA-915+ device, an atomic absorption spectrometer with a pyrolysis unit (RP-91c).

Results and discussion

Results show significant correlations between soil and leaves contents for total and organic mercury (R?=?0.934 and 0.984, respectively). Hg contents range in soil from 2,376 to 0.04 mg/kg in non-polluted places. For the organic fraction, the range varies between 197.49 and 3.15 mg/kg. Total Hg contents measured in leaves were from 5.14 mg/kg (close to dump zone of the mine) to 0.03 mg/kg in the proximity of Carrión de Calatrava, located some 100 km away from Almadén. Mercury reaches maximum in the proximity of known sources of the element: the mining and/or metallurgical areas of Almadén and Almadenejos.

Conclusions

Soils from the study area contain normal contents in trace metals, and these are conditioned by the local geology or urban locations of the area. Trace metals contents in leaves do not show a relationship with soil contents, possibly due to the low bioavailability of these elements in the soils investigated. Mercury is, as expected for this area, an exception to this trend, with very high concentrations that reach maximum values in the proximity of the known sources of the element: the proximity of mining and/or metallurgical areas in Almadén and Almadenejos.     

水源涵养基本功能区水力侵蚀现状分析简

针对全国水土保持区划中确定的22个具有水源涵养功能的基本功能区,利用第1次全国水利普查获取的水力侵蚀数据,分析这些区域的水力侵蚀现状.结果表明：1）水源涵养基本功能区水力侵蚀以轻中度侵蚀为主,超过80％,强烈、极强烈、剧烈面积分布较少,与全国基本状况相似;2）与第2次全国土壤侵蚀遥感调查成果相比,水源涵养基本功能区水力侵蚀整体上有所好转,水力侵蚀总面积减少3.75％,轻中度侵蚀面积大幅减少,减幅超过20％;3）水源涵养基本功能区局部地区水力侵蚀形势严峻,极强烈和剧烈侵蚀面积虽然不大,但是与第2次遥感调查成果相比,面积均有所增加,相对增幅较大,说明局部地区存在水力侵蚀恶化的现象.     

Bacterial ghost technology for pesticide delivery

Bacterial ghosts are nondenaturated empty cell envelopes of Gram-negative bacteria produced by E-mediated lysis. Such envelopes from the plant-adhering bacterium Pectobacterium cypripedii were tested for their ability to adhere to plant material and to be used as carriers for pesticide delivery. We show, using fluorescence-labeled P. cypripedii ghosts, that depending on the target plants 55 or 10% (rice or soya, respectively) of the applied bacterial ghosts was retained on the leaves after heavy simulated rain (84 mm). Furthermore, the bacterial ghosts could be loaded with the lipophilic triazole fungicide tebuconazole. In subsequent plant experiments in the glass house, the efficacy of the loaded bacterial ghost for resistance to rainfall and the protective and curative effects against the pathogens Erysiphe graminis, Leptosphaeria nodorum, and Pyrenophora teres on barley and wheat and against Sphaerotheca fuliginea on cucumber were tested. The bacterial ghosts were compared primarily with a commercial tebuconazole formulation, a wettable powder, as it has similar physical characteristics. The comparison revealed similar effects and showed consistently higher or comparable efficacy against the pathogens. The standard operational comparison with the most protective, cereal specific emulsion of oil in water displayed that the bacterial ghosts had equal to or lower efficacy than the emulsion. This study confirmed the potential of bacterial ghost platform technology as a new alternative carrier system for pesticides.