A survey of metabolic changes in potato leaves by NMR‐based metabolic profiling in relation to resistance to late blight disease under field conditions

Non‐targeted nuclear magnetic resonance (NMR)‐based metabolic profiling was applied to potato leaves to survey metabolic changes associated with late blight resistance under field conditions. Potato plants were grown in an experimental field, and the compound leaves with no visible symptoms were collected from 20 cultivars/lines at two sampling time points: (i) the time of initial presentation of symptoms in susceptible cultivars and (ii) 12 days before this initiation. ¹H NMR spectra of the foliar metabolites soluble in deuterium oxide‐ or methanol‐d₄‐based buffers were measured and used for multivariate analysis. Principal component analysis for six cultivars at symptom initiation showed a class separation corresponding to their levels of late blight resistance. This separation was primarily explained by higher levels of malic acid, methanol, and rutin and a lower level of sucrose in the resistant cultivars than in the susceptible ones. Partial least squares regression revealed that the levels of these metabolites were strongly associated with the disease severity measured in this study under field conditions. These associations were observed only for the leaves harvested at the symptom initiation stage, but not for those collected 12 days beforehand. Subsequently, a simple, alternative enzymatic assay for l ‐malic acid was used to estimate late blight resistance, as a model for applying the potential metabolic marker obtained. This study demonstrated the potential of metabolomics for field‐grown plants in combination with targeted methods for quantifying marker levels, moving towards marker‐assisted screening of new cultivars with durable late blight resistance. Copyright © 2016 John Wiley & Sons, Ltd.     

Metallic conductivity and ferromagnetic interaction of iron(III) d spins in the needle crystals of (ethylenedithiotetrathiafulvalenoquinone-1,3-dithiolemethide)(2).FeBr(4) salt

The 2:1 charge-transfer (CT) salts (1(2).FeBr(4) and 1(2).GaBr(4)) of ethylenedithiotetrathiafulvalenoquinone-1,3-dithiolemethide (1) with FeBr(4)(-) and GaBr(4)(-) counteranions were obtained as needle crystals, whose structures are almost the same as each other. The 1 molecules form a one dimensionally stacked column with alternation of their molecular axis direction, while the counteranions are aligned in parallel with the 1-stacked columns with the direction of their distorted-tetrahedral geometry maintained. The room-temperature electrical conductivities measured on the single crystals of 1(2).FeBr(4) and 1(2).GaBr(4) were 4.6 and 2.1 S cm(-1), respectively. From the temperature dependences of their electrical conductivities in both cases the electrical conducting properties were metallic between ca. 170 and 300 K, but below ca. 170 K converted to be semiconducting and continued till 5 K, although the activation energies are very small (4-10 meV). For 1(2).FeBr(4) very weak and antiferromagnetic interaction occurred between the d spins of FeBr(4)(-) ions in the temperature range of ca. 1-300 K. However, below ca. 15 K the ferromagnetic interaction was reversely preferential possibly by participation of the pi spin of 1.     

Matrix effect and correction by standard addition in quantitative liquid chromatographic-mass spectrometric analysis of diarrhetic shellfish poisoning toxins

An evaluation of the feasibility of liquid chromatography-mass spectrometry (LC-MS) with atmospheric pressure ionization was made for quantitation of four diarrhetic shellfish poisoning toxins, okadaic acid, dinophysistoxin-1, pectenotoxin-6 and yessotoxin in scallops. When LC-MS was applied to the analysis of scallop extracts, large signal suppressions were observed due to coeluting substances from the column. To compensate for these matrix signal suppressions, the standard addition method was applied. First, the sample was analyzed and then the sample involving the addition of calibration standards is analyzed. Although this method requires two LC-MS runs per analysis, effective correction of quantitative errors was found.     

Self-written waveguides in photopolymerizable resins

We study the optically induced growth and interaction of self-written waveguides in a photopolymerizable resin. We investigate experimentally how the interaction depends on the mutual coherence and the relative power of the input beams and suggest an improved analytical model that describes the growth of single waveguides and the main features of their interaction in photosensitive materials.     

Observation of the transient rotator phase of n-hexadecane in emulsified droplets with time-resolved two-dimensional small- and wide-angle X-ray scattering

Crystallization of n-hexadecane in emulsion droplets was studied using time-resolved two-dimensional small- and wide-angle x-ray scattering with differential scanning calorimetry (2D-SAXS-WAXS-in situ DSC) which provides information about both nano- and subnanoscale structural change. n-hexadecane in droplets reproducibly crystallized into the stable triclinic phase via a transient-rotator phase. This is in contrast with previous results that the rotator phase of n-hexadecane was observed only occasionally for bulk samples. Thus we confirmed the existence of rotator phase in n-hexadecane, which is important for the study of crystallization of soft materials. We suggest that the rotator phase at the interface of oil and water plays a precursor role for bulk crystallization. This study demonstrates that 2D-SAXS-WAXS-in situ DSC is a powerful tool for the study of a transient phase.     

Two-dimensional diffraction study of ice crystallisation in polymer gels

Ice crystallisation in crosslinked dextran (Sephadex) gels was studied by the method of two-dimensional X-ray diffraction (XRD) in combination with the simultaneous measurement of differential scanning calorimetry (DSC). With a Sephadex G25 gel where an exotherm due to ice crystallisation is observed in the DSC rewarming trace, it was indicated by the XRD pattern that small ice crystals less than approximately 10 microns in diameter are readily formed during freezing, and that the endothermic trend prior to the exotherm is not due to the glass transition but due to the melting of the small ice crystals. Moreover, the diffraction pattern observed with frozen Sephadex gels depended on the density of crosslink indicating that ice crystals of different size and dimension are formed in the gels.     

Self-ordering of nanofacets on vicinal SiC surfaces

Vicinal 4H and 6H-SiC(0001) surfaces have been investigated using atomic force microscopy and cross-sectional high-resolution transmission electron microscopy. We observed the characteristic self-ordering of nanofacets on any surface, regardless of polytypes and vicinal angles, after gas etching at high temperature. Two facet planes are typically revealed: (0001) and high index (112;n) that are induced by equilibrium surface phase separation. A (112;n) plane may have a free energy minimum due to attractive step-step interactions. The differing ordering distances in 4H and 6H polytypes imply the existence of SiC polytypic dependence on nanofaceting. Thus, it should be possible to control SiC surface nanostructures by selecting a polytype, a vicinal angle, and an etching temperature.     

Magnetic penetration depth measurements of Pr2-xCexCuO4-delta films on buffered substrates: evidence for a nodeless gap

We report measurements of the inverse squared magnetic penetration depth, lambda(-2)(T), in Pr(2-x)Ce(x)CuO(4-delta) (0.115< or =x < or =0.152) superconducting films grown on SrTiO3 (001) substrates coated with a buffer layer of insulating Pr2CuO4. lambda(-2)(0), T(c), and normal-state resistivities of these films indicate that they are clean and homogeneous. Over a wide range of Ce doping, 0.124< or =x < or =0.144, lambda(-2)(T) at low T is flat: it changes by less than 0.15% over a factor of 3 change in T, indicating a gap in the superconducting density of states. Fits to the first 5% decrease in lambda(-2)(T) produce values of the minimum superconducting gap in the range of 0.29< or =Delta(min)/k(B)T(c)< or =1.01.