RESUMO
Quantitative (1)H NMR (qNMR) is a widely applied technique for compound concentration and purity determinations. The NMR spectrum will display signals from all species in the sample, and this is generally a strength of the method. The key spectral determination is the full and accurate determination of one or more signal areas. Accurate peak integration can be an issue when unrelated peaks resonate in an important integral region. We describe a "hybrid" approach to signal integration that provides an accurate estimation of signal area, removing the component(s) that may arise from unrelated peaks. This is achieved by using the most accurate integration method for the region and removing unwanted contributions. The key to this performing well, and in almost all cases, is the use of areas from deconvolved peaks. We describe this process and show that it can be very successfully applied to cases where the highest precision is required and for more common cases of NMR-based quantitation.
RESUMO
Nuclear magnetic resonance (NMR) spectroscopy is a powerful analytical technique, but its low sensitivity and highly sophisticated, costly, equipment severely constrain more widespread applications. Here we show that a non-resonant planar transceiver microcoil integrated in a microfluidic chip (detection volume 25 nl) can detect different nuclides in the full broad-band range of Larmor frequencies (at 9.4 T from 61 to 400 MHz). Routine one-dimensional (1D) and two-dimensional (2D), homo- and heteronuclear experiments can be carried out using the broad-band coil set-up. Noteworthy, heteronuclear 2D experiments can be performed in a straightforward manner on virtually any combination of nuclides (from classical ¹H-¹³C to more exotic combinations like ¹9F-³¹P) both in coupled and decoupled mode. Importantly, the concept of a non-resonant system provides magnetic field-independent NMR probes; moreover, the small-volume alleviates problems related to field inhomogeneity, making the broad-band coil an attractive option for, for example, portable and table-top NMR systems.
RESUMO
We present a novel approach to the nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI) analysis of complex samples with nontrivial distribution of longitudinal relaxation rate R(1). Parametrically enabled relaxation filters with double and multiple inversion (PERFIDI) aim to separate signals arising from components with different R(1) values prior to actual data acquisition. Given any standard NMR/MRI pulse sequence, which, by itself, is insensitive to differences in R(1) values, it can be combined with a PERFIDI preamble, which functions as a preliminary R(1) filter and confers on the original technique sensitivity to the dimension R(1). This article states the principles of the approach, including the way to account for instrumental imperfections, and shows how PERFIDI with specific filter profile functions can be built. Using terms borrowed from electronics, these filters are classified as low-pass, high-pass and band-pass types. Also included are an experimental verification example and a discussion of potential applications of PERFIDI in various NMR areas.
Assuntos
Imageamento por Ressonância Magnética/métodos , Espectroscopia de Ressonância Magnética/métodos , Processamento de Sinais Assistido por ComputadorRESUMO
A quantitative analysis of NMR proton relaxation in hen egg albumen and yolk is undertaken to research the causes of quality loss during the first few days of storage and to access the feasibility of an on-line NMR sensor of internal egg quality. It is shown that the change in the transverse relaxation in thick egg albumen mainly results from an increase in proton exchange rate resulting from a pH increase attributed to loss of carbon dioxide by diffusion through the eggshell. The results suggest that the low-field T1 is the best relaxation time indicator of albumen quality.
