Matrix effects in the analysis of biological matrices by axial view inductively coupled plasma optical emission spectrometry

We are reporting observations of positive and negative variations of emission line intensities during the determination of boron and titanium in biological matrices by axial view inductively coupled plasma optical emission spectrometry with segmented charge-coupled device detection. The study included the testing of several elements (yttrium, palladium and platinum) and analytical wavelengths for internal standardization, aiming to compensate for variations in signal recovery due to matrix interferences. Human albumin was chosen as principal matrix component to assess the effect of variable chemical and instrumental operating conditions on boron response. A parametric study was performed by considering the application of two different nebulizer–aerosol chamber systems, the effect of plasma operating conditions on analyte and internal standard signals and the influence of common blood plasma electrolytes, added as salts of alkaline or alkaline earth elements. The pneumatic injection systems tested were a standard cross-flow nebulizer with a Scott type spray chamber and a concentric Meinhard type device coupled to a glass cyclonic spray chamber. The change from standard (i.e. medium RF power and relatively high aerosol carrier gas flow rate) to robust (i.e. higher RF power and lower carrier gas flow rate) conditions contributed to large, non-correlated variations in boron intensities and in some of the analyte/internal standard ratios. Significant memory effects were observed for injection of boron solutions prepared with boric acid and containing small amounts of acid, but those effects were negligible when the boron carrier compound was boronophenylalanyne. The injection of titanium solutions did not produce analyte carry-over effects. When internal standards were employed, a less effective signal compensation was consistently observed for boron at higher albumin concentrations when the difference in energies of the lines was between 4.5 and 6 eV. This effect was enhanced for some line pairs when robust conditions are employed. Differences in the response between nebulizers were minor, with a slight advantage in sensitivity for the cross-flow/Scott system. Yttrium was found to be useful for signal compensation in the determination of boron and titanium in blood and human plasma provided that the equivalent concentration of albumin in the nebulized sample dilutions was kept below 0.2% w/v. Simultaneous measurement of a reference strontium line was found to be useful as an additional verification of the response of yttrium as internal standard.     

Analysis of 1H-NMR relaxation time distributions in L1 to L6 rat lumbar vertebrae

A better knowledge of the NMR relaxation behavior of bone tissue can improve the definition of imaging protocols to detect bone diseases like osteoporosis. The six rat lumbar vertebrae, from L1 to L6, were analyzed by means of both transverse (T(2)) and longitudinal (T(1)) relaxation of (1)H nuclei at 20 MHz and 30 degrees C. Distributions of relaxation times, computed using the multiexponential inversion software uniform penalty inversion, extend over decades for both T(2) and T(1) relaxation. In all samples, the free induction decay (FID) from an inversion-recovery (IR) T(1) measurement shows an approximately Gaussian (solid-like) component, exp[-1/2(t/T(GC))2], with T(GC) approximately 12 micros (GC for Gaussian component) and a liquid-like component (LLC) with initially simple-exponential decay. Averaging and smoothing procedures are adopted to obtain the ratio alpha between GC and LLC signals and to get separate T(1) distributions for GC and LLC. Distributions of T(1) for LLC show peaks centered at 300-500 ms and shoulders going down to 10 ms, whereas distributions of T(1) for GC are single broad peaks centered at roughly 100 ms. The T(2) distributions by Carr-Purcell-Meiboom-Gill at 600 micros echo spacing are very broad and extend from 1 ms to hundreds of ms. This long echo spacing does not allow one to see a peak in the region of hundreds of micros, which is better seen by single spin-echo T(2) measurements. Results of the relaxation analysis were then compared with densitometric data. From the study, a clear picture of the intratrabecular and intertrabecular (1)H signals emerges. In particular, the GC is presumed to be due to (1)H in collagen, LLC due to all the fluids in the bone including water and fat, and the very short T(2) peak due to the intratrabecular water. Overall, indications of some trends in composition and in pore-space distributions going from L1 to L6 appeared. Published results on rat vertebrae obtained by fitting the curves by discrete two-component models for both T(2) and T(1) are consistent with our results and can be better interpreted in light of the shown distributions of relaxation times.     

Optical image subtraction through speckle modulated by young fringes

A new method for subtracting images is proposed. It is based on assigning complementary Young's fringes to the speckles of the common parts of two images. In this way, carrier frequency is cancelled, and “a-posteriori” spatial filtering shows only noncommon parts. Suggestions on applications of the method are briefly commented.     

Experimental and in silico characterization of a biologically active inosose

Inositols have been recently reported to show a biological activity as inhibitors of both glycosidase and amyloid-β protein. After having harvested good crystals suitable for single crystal X-ray diffraction, we performed a comparison with the data inferred by means of a molecular dynamics simulation, based on the use of an appropriate Force Field coupled to the most performing charging scheme. This approach allowed a detailed analysis extended to ultra-fine details, such as atomic displacement parameters. It confirmed the good validity of a robust approach already tested by us in previous studies. A NMR analysis of the molecule in solution was also carried out, to compare the structural findings suggested by the X-ray analysis with the ones in solution and avoid confining them to the solid-state. In this framework, we investigated the above-mentioned inhibiting activity of a class of inososes, by means of a molecular docking investigation, which proved the suggested validity of the studied compound as inhibitor of the α-glucosidase.