Study of blood collection and sample preparation for analysis of vitamin D and its metabolites by liquid chromatography–tandem mass spectrometry

The analysis of vitamin D status, with special emphasis on 25-hydroxyvitamin D and 1,25-dihydroxyvitamin D, is gaining interest in clinical studies due to the classical and non-classical effects attributed to this prohormone. In this research, the influence of the two steps preceding determination (viz. sample collection and preparation) on the quantitative analysis of vitamin D and its more important metabolites has been studied. Two preparation approaches, deproteination and solid-phase extraction (SPE), have been evaluated in terms of sensitivity to delimit their application, thus establishing that detection of 1,25-dihydroxyvitamin D cannot be addressed by protein precipitation. Concerning sample collection, serum and plasma reported high accuracy (above 83.3%) for vitamin D and metabolites, while precision, expressed as relative standard deviation, was below 12.9% for all analytes in both samples. Statistical analysis revealed that serum and plasma provided similar physiological levels for vitamin D₃, 24,25-dihydroxyvitamin D₃ and 25-hydroxyvitamin D₃, while significantly different levels were obtained for 1,25-dihydroxyvitamin D₃, always higher in plasma than in serum. Sample collection and treatment have proved to be significant in the analysis of vitamin D and its relevant metabolites.     

HyperFLOW软件非结构网格亚跨声速湍流模拟的验证与确认

计算流体力学(computational fluid dynamics,CFD)数值模拟在航空航天等领域发挥越来越重要的作用,然而CFD数值模拟结果的可信度仍然需要通过不断地验证与确认来提高.本文给出了从制造解精度测试、简单到复杂外形湍流模拟网格收敛性研究等三个方面开展CFD软件验证与确认的方法,并对自主研发的CFD软件平台HyperFLOW在非结构网格上模拟亚跨声速湍流问题的能力进行了验证与确认.首先通过基于Euler方程和标量扩散方程的制造解精度测试,分别验证了HyperFLOW在非结构网格上对Euler方程和黏性项的求解精度,结果表明其能够在任意非结构网格上达到设计的二阶精度. 其次,通过NASATurbulence Modeling Resource中的湍流平板、二维翼型近尾迹流动、二维Bump等几个典型的亚声速湍流算例的网格收敛性研究,量化考察了数值结果的观测精度阶和网格收敛性指数,并与国外知名CFD解算器CFL3D,FUN3D的计算结果进行了对比,验证了HyperFLOW对简单湍流问题的模拟能力,且具有良好的网格收敛性和计算精度(阶). 最后,通过NASA CommonResearchModel标模定升力系数的网格收敛性研究和升阻极曲线预测,验证了软件在复杂外形亚跨声速湍流流动数值模拟中也具有良好的可信度.      

Bounded invariant verification for time-delayed nonlinear networked dynamical systems

We present a technique for bounded invariant verification of nonlinear networked dynamical systems with delayed interconnections. The underlying problem in precise bounded-time verification lies with computing bounds on the sensitivity of trajectories (or solutions) to changes in initial states and inputs of the system. For large networks, computing this sensitivity with precision guarantees is challenging. We introduce the notion of input-to-state (IS) discrepancy of each module or subsystem in a larger nonlinear networked dynamical system. The IS discrepancy bounds the distance between two solutions or trajectories of a module in terms of their initial states and their inputs. Given the IS discrepancy functions of the modules, we show that it is possible to effectively construct a reduced (low dimensional) time-delayed dynamical system, such that the trajectory of this reduced model precisely bounds the distance between the trajectories of the complete network with changed initial states. Using the above results we develop a sound and relatively complete algorithm for bounded invariant verification of networked dynamical systems consisting of nonlinear modules interacting through possibly delayed signals. Finally, we introduce a local version of IS discrepancy and show that it is possible to compute them using only the Lipschitz constant and the Jacobian of the dynamic function of the modules.     

Assessing the Calibration of High-Dimensional Ensemble Forecasts Using Rank Histograms

Any decision-making process that relies on a probabilistic forecast of future events necessarily requires a calibrated forecast. This article proposes new methods for empirically assessing forecast calibration in a multivariate setting where the probabilistic forecast is given by an ensemble of equally probable forecast scenarios. Multivariate properties are mapped to a single dimension through a prerank function and the calibration is subsequently assessed visually through a histogram of the ranks of the observation’s preranks. Average ranking assigns a prerank based on the average univariate rank while band depth ranking employs the concept of functional band depth where the centrality of the observation within the forecast ensemble is assessed. Several simulation examples and a case study of temperature forecast trajectories at Berlin Tegel Airport in Germany demonstrate that both multivariate ranking methods can successfully detect various sources of miscalibration and scale efficiently to high-dimensional settings. Supplemental material in form of computer code is available online.     

On the uncertainty of CFD in sail aerodynamics

A verification and validation procedure for yacht sail aerodynamics is presented. Guidelines and an example of application are provided. The grid uncertainty for the aerodynamic lift, drag and pressure distributions for the sails is computed. The pressures are validated against experimental measurements, showing that the validation procedure may allow the identification of modelling errors. Lift, drag and L₂ norm of the pressures were computed with uncertainties of the order of 1%. Convergence uncertainty and round‐off uncertainty are several orders of magnitude smaller than the grid uncertainty. The uncertainty due to the dimension of the computational domain is computed for a flat plate at incidence and is found to be significant compared with the other uncertainties. Finally, it is shown how the probability that the ranking between different geometries is correct can be estimated knowing the uncertainty in the computation of the value used to rank. Copyright © 2013 John Wiley & Sons, Ltd.     

Concurrent combined verification: reducing false positives in automated NMR structure verification through the evaluation of multiple challenge control structures

Automated structure verification using ¹H NMR data or a combination of ¹H and heteronuclear single‐quantum correlation (HSQC) data is gaining more interest as a routine application for qualitative evaluation of large compound libraries produced by synthetic chemistry. The goal of this automated software method is to identify a manageable subset of compounds and data that require human review. In practice, the automated method will flag structure and data combinations that exhibit some inconsistency (i.e. strange chemical shifts, conflicts in multiplicity, or overestimated and underestimated integration values) and validate those that appear consistent. One drawback of this approach is that no automated system can guarantee that all passing structures are indeed correct structures. The major reason for this is that approaches using only ¹H or even ¹H and HSQC spectra often do not provide sufficient information to properly distinguish between similar structures. Therefore, current implementations of automated structure verification systems allow, in principle, false positive results. Presented in this work is a method that greatly reduces the probability of an automated validation system passing incorrect structures (i.e. false positives). This novel method was applied to automatically validate 127 non‐proprietary compounds from several commercial sources. Presented also is the impact of this approach on false positive and false negative results. Copyright © 2012 John Wiley & Sons, Ltd.     

基于CAN总线的某型数字化战车自动测试系统设计

针对现代数字化战车电气与电子系统技术复杂、各分系统关联程度高、维修保障困难等问题,设计了一种基于CAN总线的数字化战车自动测试系统;整体设计基于模块化思想,充分利用车载备用总线,综合运用了DSP+FPGA控制处理技术、AFPN智能故障诊断技术,能够对车载电气与电子系统进行分系统独立测试和全系统联合检测,具有快速故障定位能力和拓扑适应能力;采用适配器与上位机测试软件的分体式设计,实现了平台物理资源复用。应用表明,该系统能够较好的适用于现代数字化战车的维修保障,使用方便,故障诊断快速有效。     

基于LabVIEW的砝码自动检定系统设计与实现

针对目前砝码检定工作操作过程复杂、检定效率低等问题,设计了一种基于LabVIEW的砝码自动检定系统。在符合砝码检定规程的情况下,系统实现了检定数据实时采集、数据处理、生成原始记录、管理标准器、查询历史数据和衡器控制等功能。相对现有的砝码检定方法有操作简单、高效、程序移植性好等优点。系统由主控计算机、串口转无线扩展卡、多台衡器设备及相应的标准砝码装置组成。通过使用串口转Wi-Fi模块,系统可实现控制多台衡器设备的需求。实验结果证明,系统运行稳定可靠,采集数据准确,容易扩展,且大幅度减轻了检定人员的劳动强度,在计量检定工作中具有一定的实用和推广价值。     

基于云环境的分布式软件接口自动化测试

软件测试是保证软件质量,提供可靠服务的重要技术手段。目前基于Web Service的分布式软件越来越多,其测试技术手段也越来越受到关注。Web Service的分布性和多样性使手工测试变得非常低效,因而需要不断提高Web Service测试的自动化程度。另外,云计算因其计算成本低、可伸缩性强的特点为自动化测试提供了新的支持环境。本文结合Web Service的测试需求,首次提出了基于云环境的Web Service接口自动化测试的技术框架,分析了框架内原子Web Service、组合Web Service测试的关键技术,并研发了基于CloudStack云平台的自动化测试的原型系统。实验结果表明,本文所提出的基于云平台的WebService自动化测试方案可行且提高了测试效率。     

火试金法配料过程自动化的探索和应用

火试金法中配料方式采用的是传统的人工配料,针对人工配料方式的不足,设计了一款自动化程度较高的自动配料机,通过对配料机的准确性、效率及可靠性实验,结果表明配料机检测称量误差在±0.2 g以内,效率为人工配料的2~3倍,检测结果与人工配料的相一致。与此同时,应用此设备改善了工作环境,避免了人为失误造成的检测质量问题,降低了复检率,为企业降低了成本,提高了效益,在业内具有广泛应用前景。