Accurate,sensitive determination of omega-6 and omega-3 polyunsaturated fatty acids in human plasma,urine samples

Quantitative determination of omega-6 and omega-3 polyunsaturated fatty acids in human plasma and urine with high accuracy and precision provides significant information to monitor the underlying etiology of several diseases. In this regard, liquid chromatography-mass spectrometry is a good choice owing to its great selectivity and sensitivity. Additionally, the hybrid quadrupole–time of flight–mass spectrometer systems provides easy identification of target compounds with superior mass measurements. In this study, an analytical method has been developed for simple, accurate and simultaneous determination of linoleic acid, arachidonic acid, docosahexaenoic acid and eicosapentaenoic acid in a short chromatographic analysis period. The developed method is suitable for the quantitative detection of these four compounds with detection limits ranging between 1.1–3.0 ng ml⁻¹ and its applicability was assessed in human urine and plasma samples. As a result, acceptable accuracy (between 83 and 111%) and good precision (<6%) were obtained for target compounds using matrix matching calibration strategy.     

The High Energy X-ray telescope (HE) onboard the Insight-HXMT astronomy satellite

The Insight-Hard X-ray Modulation Telescope(Insight-HXMT) is a broadband X-ray and γ-ray(1-3000 ke V) astronomy satellite. One of its three main telescopes is the High Energy X-ray telescope(HE). The main detector plane of HE comprises 18 Na I(Tl)/Cs I(Na) phoswich detectors, where Na I(Tl) is used as the primary detector to measure ~ 20-250 ke V photons incident from the field of view(FOV) defined by collimators, and Cs I(Na) is used as the active shielding detector to Na I(Tl) by pulse shape discrimination. Additionally, Cs I(Na) is used as an omnidirectional γ-ray monitor. The HE collimators have a diverse FOV,i.e. 1.1°×5.7°(15 units), 5.7°×5.7°(2 units), and blocked(1 unit). Therefore, the combined FOV of HE is approximately5.7°×5.7°. Each HE detector has a diameter of 190 mm resulting in a total geometrical area of approximately 5100 cm2, and the energy resolution is ~15% at 60 ke V. For each recorded X-ray event by HE, the timing accuracy is less than 10 μs and the deadtime is less than 10 μs. HE is used for observing spectra and temporal variability of X-ray sources in the 20-250 ke V band either by pointing observations for known sources or scanning observations to unveil new sources. Additionally, HE is used for monitoring the γ-ray burst in 0.2-3 Me V band. This paper not only presents the design and performance of HE instruments but also reports results of the on-ground calibration experiments.     

Effective length calibration method for processing the fluorescence signal detected by charge‐coupled device in capillary electrophoresis

A novel method named effective length calibration method has been developed to process the fluorescence signal detected by charge‐coupled device during capillary electrophoresis. The new method treated each pixel as an individual point detector, and effectively binned a large number of pixels into a final electropherogram without losing the narrow detection window defined by a single pixel. Capillary electrophoresis separations of DNA were carried out and detected by charge‐coupled device and conventional detector (photomultiplier tube). Detection properties including signal‐to‐noise ratio, peak width, detection frequency, and tilt of detector were investigated. It was found that the new method achieved much higher signal‐to‐noise ratio and smaller peak width than the conventional detector did. A Detection width of 0.5 μm was easily achieved.     

硫代硫酸钠标准溶液配制中标定基准物质的优化选择

对硫代硫酸钠标准溶液配制实验中不同基准物质的标定效果进行了对比研究,结合试剂用量、反应时间、显著性检验等分析说明不同基准物质所产生的结果:重铬酸钾、碘酸钾、溴酸钾均可实现对硫代硫酸钠溶液的标定。其中溴酸钾作为标定的基准物质时,试剂用量少,反应时间短,实验费用低且终点易于观察。双侧t检验符合统计学要求,更适用于硫代硫酸钠溶液标定,有望引入学生实验。     

Calibration transfer employing univariate correction and robust regression

This paper proposes a new method for calibration transfer, which was specifically designed to work with isolated variables, rather than the full spectrum or spectral windows. For this purpose, a univariate procedure is initially employed to correct the spectral measurements of the secondary instrument, given a set of transfer samples. A robust regression technique is then used to obtain a model with low sensitivity with respect to the univariate correction residuals. The proposed method is employed in two case studies involving near infrared spectrometric determination of specific mass, research octane number and naphthenes in gasoline, and moisture and oil in corn. In both cases, better calibration transfer results were obtained in comparison with piecewise direct standardization (PDS). The proposed method should be of a particular value for use with application-targeted instruments that monitor only a small set of spectral variables.     

Tutorial review on validation of liquid chromatography–mass spectrometry methods: Part I

This is the part I of a tutorial review intending to give an overview of the state of the art of method validation in liquid chromatography mass spectrometry (LC–MS) and discuss specific issues that arise with MS (and MS/MS) detection in LC (as opposed to the “conventional” detectors). The Part I briefly introduces the principles of operation of LC–MS (emphasizing the aspects important from the validation point of view, in particular the ionization process and ionization suppression/enhancement); reviews the main validation guideline documents and discusses in detail the following performance parameters: selectivity/specificity/identity, ruggedness/robustness, limit of detection, limit of quantification, decision limit and detection capability. With every method performance characteristic its essence and terminology are addressed, the current status of treating it is reviewed and recommendations are given, how to determine it, specifically in the case of LC–MS methods.     

Revisiting the extrapolation of correlation energies to complete basis set limit

The extrapolation scheme of correlation energy is revisited to evaluate the complete basis set limit from double‐zeta (DZ) and triple‐zeta levels of calculations. The DZ level results are adjusted to the standard asymptotic behavior with respect to the cardinal number, observed at the higher levels of basis sets. Two types of adjusting schemes with effective scaling factors, which recover errors in extrapolations with the DZ level basis set, are examined. The first scheme scales the cardinal number for the DZ level energy, while the second scheme scales the prefactor of the extrapolation function. Systematic assessments on the Gaussian‐3X and Gaussian‐2 test sets reveal that these calibration schemes successfully and drastically reduce errors without additional computational efforts. © 2015 Wiley Periodicals, Inc.     

Simultaneous determination of naphazoline and pyridoxine in eye drops using excitation–emission matrix fluorescence coupled with second-order calibration method based on alternating trilinear decomposition algorithm

A novel method is developed for the direct determination of naphazoline hydrochloride(NAP) and pyridoxine hydrochloride(VB6) in commercial eye drops. By using excitation–emission matrix(EEM)fluorescence coupled with second-order calibration method based on the alternating trilinear decomposition(ATLD) algorithm, the proposed approach can achieve quantitative analysis successfully even in the presence of unknown and uncalibrated interferences. The method shows good linearity for NAP and VB6 with correlation coefficients greater than 0.99. The results were in good agreement with the labeled contents. To further confirm the feasibility and reliability of the proposed method, the same batch samples were analyzed by multiple reaction monitoring(MRM) based on LC–MS/MS method.T-test demonstrated that there are no significant differences between the prediction results of the two methods. The satisfactory results obtained in this work indicate that the use of the second-order calibration method coupled with the EEM is a promising tool for industrial quality control and pharmaceutical analysis due to its advantages of high sensitivity, low-cost and simple implementation.     

箔式高阻值低压锰铜压阻应力计的设计及动态标定

设计了低压锰铜压阻传感器 ,并通过平板撞击实验标定了该传感器在 0 .3～ 9.4GPa范围内的压阻关系。标定曲线在 0 .3～ 1.5GPa范围内是线性的 ,对应的是传感器的弹性状态 ,而在 1.5～ 9.4GPa范围内是二次曲线。标定曲线的拐点在 1.5GPa附近 ,这与理论分析和他人的实验结果相接近。     

光纤陀螺捷联系统标定测试软件的设计与开发

基于 windows 平台,采用 VC 6.0 开发了光纤陀螺捷联惯组标定测试软件,着重阐述了该软件的设计思想和关键技术的实现。该软件实现了对光纤陀螺捷联组合误差系数的标定与测试,为光纤陀螺捷联系统标定测试提供了方便,具有很强的工程实用价值。