Probing Invisible,Excited Protein States by Non‐Uniformly Sampled Pseudo‐4D CEST Spectroscopy

Chemical exchange saturation transfer (CEST) NMR spectroscopy is a powerful tool for studies of slow timescale protein dynamics. Typical experiments are based on recording a large number of 2D data sets and quantifying peak intensities in each of the resulting planes. A weakness of the method is that peaks must be resolved in 2D spectra, limiting applications to relatively small proteins. Resolution is significantly improved in 3D spectra but recording uniformly sampled data is time‐prohibitive. Here we describe non‐uniformly sampled HNCO‐based pseudo‐4D CEST that provides excellent resolution in reasonable measurement times. Data analysis is done through fitting in the time domain, without the need of reconstructing the frequency dimensions, exploiting previously measured accurate peak positions in reference spectra. The methodology is demonstrated on several protein systems, including a nascent form of superoxide dismutase that is implicated in neurodegenerative disease.     

利用迭代软阈值方法抑制恒时演化类核磁共振实验中的采样截断伪峰

采样截断,即信号衰减殆尽之前结束采样,会在核磁共振(NMR)谱图中引入振荡状伪峰,进而影响谱图质量.在多维核磁共振实验中,为减少实验时间并为后续脉冲序列保留自旋相干,采样必然在信号衰减完毕之前结束,因此采样截断在所难免.变迹法(窗函数法)可以抑制采样截断造成的伪峰,但会导致谱峰增宽.线性预测也有助于减小截断伪峰.采样截断最严重的场合,是在恒时演化类实验中.这类实验的间接维演化时间固定,因此间接维采样信号强度没有表观衰减.本研究提出的迭代软阈值方法(Iterative Soft Thresholding,IST)虽然因为调节参数困难而在一般场合中应用受限,但恒时演化类(Constant time,CT)NMR实验的间接维信号缺没有表观衰减,这为IST处理参数设置提供了简化条件.本研究通过数据模拟和实验数据,证明了IST是抑制CT-NMR实验中采样截断伪峰的有效方法,并与其它相关方法进行了对比.     

Sampling Sets and Quadrature Formulae on the Rotation Group

In this paper, we construct sampling sets over the rotation group SO(3). The proposed construction is based on a parameterization, which reflects the product nature ² × ¹ of SO(3) very well, and leads to a spherical Pythagorean-like formula in the parameter domain. We prove that by using uniformly distributed points on ² and ¹, we obtain uniformly sampling nodes on the rotation group SO(3). Furthermore, quadrature formulae on ² and ¹ lead to quadratures on SO(3), as well. For scattered data on SO(3), we give a necessary condition on the mesh norm such that the sampling nodes possess nonnegative quadrature weights. We propose an algorithm for computing the quadrature weights for scattered data on SO(3) based on fast algorithms. We confirm our theoretical results with examples and numerical tests.     

光谱分析采样数据重建原始信号

用光谱分析方法分析信号的采样与恢复。用三个改进的升余弦脉冲构造对称的限带频谱F(ω),经理论推导获得时域信号f(t)。采用梳状函数δ_T(t)对f(t)采样,调节T值,获得Shannon采样。应用快速傅里叶变换,计算采样的频谱F_d(ω),比较计算频谱F_d(ω)与限带频谱F(ω)的差别,讨论由采样频谱F_d(ω)重建f(t)的方法。结果发现：计算频谱F_d(ω)与限带频谱F(ω)非常相似,由采样数据可以在时域直接重建原始信号,而由频谱数据经快速逆傅里叶变换,同样能准确重建原始信号。因此,信号存储,既可以存储其采样信号,也可以存储采样信号的数字频谱。     

ICP-AES中激光烧蚀固体进样的输运过程

利用激光烧蚀固体进样电感耦合等离子体光谱法,测量了标钢样品中元素P、V和Ti的光谱强度和信背比,以此研究样品输送过程对激光烧蚀固体进样方法的影响,获得优化的实验条件。结果表明：当样品输送管越短、直径越小时,测得的光源辐射强度越强,光谱信背比也越高;随着输送样品的载气流量的增大,光谱强度和信背比均为先逐渐增大而后减小,在流量约为0.5L/min有较好的效果。     

悬浮液进样石墨炉原子吸收法测定近海沉积物中的铜

本文研究了一种使用悬浮液进样石墨炉原子吸收光谱法快速、简便地测定近海沉积物中痕量铜。采用超声波将悬浮液分散，由磁力搅拌器保证悬浮液分散、均匀、稳定，以与样品基体相匹配的近海海洋沉积物成分分析标准物质(GBW07314)进行校正。试验了悬浮液的介质、酸度、悬浮液浓度等因素的影响。本法的检出限为0．6μg／g，加标回收率为88．7％-108％，RSD为2．42％。用于实际样品的分析。本方法准确、可靠，结果令人满意。     

Reconstruction of Band-Limited Functions from Local Averages

In this paper, we show that every band-limited function can be reconstructed by its local averages near certain points. We give the optimal upper bounds for the support length of averaging functions with respect to both regular and irregular sampling points. Our results improve an earlier result by Gröchenig.     

On sampling theory associated with the resolvents of singular Sturm-Liouville problems

This paper is concerned with the sampling theory associated with resolvents of eigenvalue problems. We introduce sampling representations for integral transforms whose kernels are Green's functions of singular Sturm-Liouville problems provided that the singular points are in the limit-circle situation, extending the results obtained in the regular problems.

     

Structure analysis using acoustically levitated droplets

Synchrotron diffraction with a micrometer-sized X-ray beam permits the efficient characterization of micrometer-sized samples, even in time-resolved experiments, which is important because often the amount of sample available is small and/or the sample is expensive. In this context, we will present acoustic levitation as a useful sample handling method for small solid and liquid samples, which are suspended in a gaseous environment (air) by means of a stationary ultrasonic field. A study of agglomeration and crystallization processes in situ was performed by continuously increasing the concentration of the samples by evaporating the solvent. Absorption and contamination processes on the sample container walls were suppressed strongly by this procedure, and parasitic scattering such as that observed when using glass capillaries was also absent. The samples investigated were either dissolved or dispersed in water droplets with diameters in the range of 1 micrometer to 2 millimeters. Initial results from time-resolved synchrotron small- and wide-angle X-ray scattering measurements of ascorbic acid, acetylsalicylic acid, apoferritin, and colloidal gold are presented.     

Global status of trace elements in the ocean

Trace elements in seawater can be limiting factors of biological productivity, tracers of ocean circulation and biogeochemical processes, and proxies for paleoceanography. The global status of trace elements and their isotopes (TEIs) in the ocean is being explored this decade through an international study of the global marine biogeochemical cycles of TEIs (GEOTRACES). Such an international study has become possible due to recent methodological developments in sampling, preconcentration, and measurement of TEIs. Here, we present an overview of recent methodological developments and initial GEOTRACES intercalibration activities for obtaining data about TEIs that are accurate, precise, and intercomparable.