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.     

Applying green analytical chemistry for development and validation of RP-HPLC stability indicating assay method for estimation of fenoverine in bulk and dosage form using quality by design approach

A green and robust reverse-phase liquid chromatographic method has been developed for the determination of fenoverine (FEN), by applying combined principles of green analytical chemistry and quality by design approaches on a Spherisorb C18 column (150?×?4.6?mm, 3?µm) with UV detection at 262?nm. A two level fractional factorial design (2^^7-3) Res IV was used for screening of influential chromatographic factors. The critical method parameters actively affecting critical quality attributes (CQAs) were identified and further optimized using Box–Behnken design. The predicted optimum assay conditions comprised of methanol and ammonium acetate buffer 20?mM, in an extent of 81:19% v/v individually having a flow rate of 1.0?mL/min with a column oven temperature of 33°C. The drug was stressed in hydrolytic, oxidative, reductive, thermal, and photolytic conditions. The developed method was validated successfully. The detector response was linear in the concentration of 0.5–160?µg/mL with a limit of detection (LOD) and limit of quantitation (LOQ) as 0.1 and 0.3?µg/mL, respectively. The % recovery was found to be 99.7%. The analytical method volume intensity value for developed method was 45?mL and the environment assessment tool (EAT) score was 41.07. The method is simple, environmentally benign, rapid, and robust for the determination of FEN in bulk and in its dosage form.     

井下巷道围岩变形的散斑分析法

通过对散斑计量法原理分析、数学描述及观测实例的论述，证明激光散斑法是研究煤矿地下结构物相似模型变形状态的一种新的无损检测技术，若采用白光作为光源，该项技术可用于二维变形场的实地测试。     

Analytical issues in monitoring drinking-water contamination related to short-term, heavy rainfall events

Heavy rainfall events, increasing in frequency and intensity with climate change, impact on the quality of the water resource used for drinking-water production. Small-scale water suppliers are particularly sensitive because of their management and the related difficulties of adapting treatment to variations. Decision-support systems, based on monitoring and analytical tools, need to be developed to improve crisis-management procedures related to such events. After presenting the issues related to heavy rainfall events, the article summarizes the tools currently used for quality control of drinking water within this framework, the need for developments and other requirements.     

Curriculum, Classroom Practices, and Tool Design in the Learning of Functions Through Technology-Aided Experimental Approaches

The paper starts from classroom situations about the study of a functional relationship with help of technological tools as a ‘transposition’ of experimental approaches from research mathematical practices. It considers the limitation of this transposition in existing curricula and practices based on the use of non-symbolic software like dynamic geometry and spreadsheets. The paper focuses then on the potentialities of classroom use of computer algebra packages that could help to go beyond this shortcoming. It looks at a contradiction: while symbolic calculation is a basic tool for mathematicians, curricula and teachers are very cautious regarding their use by students. The rest of the paper considers the design and experiment of a computer environment Casyopée as means to contribute to an evolution of curricula and classroom practices to achieve the transposition in the domain of algebraic activities linked to functions.     

Metrology in Iceland: a status report

 The metrology system in Iceland has been reviewed and developed in the light of the increased needs of industry and other users of the system, in some cases to comply with the requirements of the agreement between the European Union and the European Economic Area which the Icelandic government signed in 1992. After a short historical review, the current legislation is explained, the metrological infrastructure is described, and the plans for the coming years are discussed. Received: 27 November 1995 Accepted: 18 December 1995     

Effective radiating area and beam non-uniformity ratio of ultrasound transducers at 5 MHz, according to IEC 61689:2007

This paper discloses results of measuring the effective radiating area (A_ER) and the beam non-uniformity ratio (R_BN) for US transducers at 5.0 MHz. Measurements were carried out at Laboratory of Ultrasound of the Brazilian National Institute of Metrology, Standardization, and Industrial Quality. As reliability proof of system’s adequacy, uncertainties were assessed. The calculation protocol was developed based on standard IEC 61689:2007. Type A uncertainty was estimated after four repetitions of the full procedure for the determination of A_ER and R_BN, and Type B uncertainty was estimated from the mathematical model for both calculations, obtained from IEC 61689:2007 and the guide to the expression of uncertainty in measurement. The procedure presented herein represents the state of the art regarding metrology for testing therapeutic ultrasound devices, and its application results in fundamental aspects to support their evaluation regarding quality assurance, for instance, for a certification process due safety and performance.     

Real-Time Tool Detection for Workflow Identification in Open Cranial Vault Remodeling

Deep learning is a recent technology that has shown excellent capabilities for recognition and identification tasks. This study applies these techniques in open cranial vault remodeling surgeries performed to correct craniosynostosis. The objective was to automatically recognize surgical tools in real-time and estimate the surgical phase based on those predictions. For this purpose, we implemented, trained, and tested three algorithms based on previously proposed Convolutional Neural Network architectures (VGG16, MobileNetV2, and InceptionV3) and one new architecture with fewer parameters (CranioNet). A novel 3D Slicer module was specifically developed to implement these networks and recognize surgical tools in real time via video streaming. The training and test data were acquired during a surgical simulation using a 3D printed patient-based realistic phantom of an infant’s head. The results showed that CranioNet presents the lowest accuracy for tool recognition (93.4%), while the highest accuracy is achieved by the MobileNetV2 model (99.6%), followed by VGG16 and InceptionV3 (98.8% and 97.2%, respectively). Regarding phase detection, InceptionV3 and VGG16 obtained the best results (94.5% and 94.4%), whereas MobileNetV2 and CranioNet presented worse values (91.1% and 89.8%). Our results prove the feasibility of applying deep learning architectures for real-time tool detection and phase estimation in craniosynostosis surgeries.     

Note on fundamental operations

A new type of generalization of fundamental calculating operations is attempted. Instead of generalizing the nature of the elements upon which operations are acting, the nature of the operations themselves is changed. By iterating the step which leads from addition to multiplication, new types of operations are generated. Some of these operations are discussed briefly.     

基于机器视觉的刀具轮廓在线检测方法的研究

超精密单点金刚石车削过程中需要对刀具参数进行检测。基于机器视觉原理,采用新型的机械结构设计了新型刀具在线检测系统。通过垂直放置的两组由同轴远心镜头和CMOS相机组成的光学系统来获取车刀刀尖正面及侧面的图像,再经图像处理系统来获取刀具的轮廓及位置信息,完成对刀具轮廓及位置的在线检测,实验验证可实现测量的重复性定位精度达1μm。在线检测的方式借助了超精密车床自身的高精度和运动机构,可以保证相机焦点和机床主轴之间的相对位置关系,弥补了目前刀具检测系统稳定性差和重复性精度低的不足,提高了加工的整体效率。