Interphases, Interfaces, and Surfaces of Active Materials in Rechargeable Batteries and Perovskite Solar Cells.

The ever-increasing demand for clean sustainable energy has driven tremendous worldwide investment in the design and exploration of new active materials for energy conversion and energy-storage devices. Tailoring the surfaces of and interfaces between different materials is one of the surest and best studied paths to enable high-energy-density batteries and high-efficiency solar cells. Metal-halide perovskite solar cells (PSCs) are one of the most promising photovoltaic materials due to their unprecedented development, with their record power conversion efficiency (PCE) rocketing beyond 25% in less than 10 years.

Novel Carbon-Encapsulated Porous SnO2 Anode for Lithium-Ion Batteries with Much Improved Cyclic Stability.

Porous SnO2 submicrocubes (SMCs) are synthesized by annealing and HNO3 etching of CoSn(OH)6 SMCs. Bare SnO2 SMCs, as well as bare commercial SnO2 nanoparticles (NPs), show very high initial discharge capacity when used as anode material for lithium-ion batteries. However, during the following cycles most of the Li ions previously inserted cannot be extracted, resulting in considerable irreversibility.

Formation of interfacial layer and long-term cyclability of Li-O₂ batteries.

The long-term operation of Li-O2 batteries under full discharge/charge conditions is investigated in a glyme-based electrolyte. The formation of stable interfacial layer on the electrode surface during the initial cycling stabilizes reaction products at subsequent cycling stages as demonstrated by quantitative analyses of the discharge products and the gases released during charging. There is a quick switch from the predominant formation of Li2O2 to the predominant formation of side products during the first few cycles.

Beyond successful ISR: case-by-case investigations for unmatched reassay results when ISR passed.

Incurred sample reanalysis (ISR) is now commonly practiced in regulated bioanalytical laboratories. With an average ISR success rate of 95% or higher and an increasing number of ISR tests being conducted, more and more situations deserve scientific evaluation or investigation for the unmatched reassay results revealed in ISR tests even though they meet the acceptance criteria. First, should an investigation be initiated when an ISR test is acceptable? How large a discrepancy or what situation would warrant an investigation? What would be the impact on a study? How would investigations regarding unmatched reassay results be conducted? What are the main root causes identified? Can normal random errors cause a large discrepancy in unfavorable combinations? How could the timeline and cost be affected? All these questions are addressed in this paper with five real case examples.

2010 white paper on recent issues in regulated bioanalysis & global harmonization of bioanalytical guidance.

The 4th Calibration and Validation Group Workshop on Recent Issues in Regulated Bioanalysis, a 2-day full immersion workshop, was organized by the Calibration and Validation Group. Contract research organizations, pharmaceutical companies and regulatory agencies came together to discuss several 'hot' topics concerning bioanalytical issues and regulatory challenges and to reach a consensus among panelists and attendees on many points regarding method validation of small and large molecules.

2009 White Paper on recent issues in regulated bioanalysis from the 3rd Calibration and Validation Group Workshop.

The 3rd Calibration and Validation Group Workshop on Recent Issues in Regulated Bioanalysis was organized by the Calibration and Validation Group as a 1.5-day full immersion workshop for contract research organizations, pharmaceutical companies and regulatory agencies to discuss several 'hot' topics concerning bioanalytical issues and regulatory challenges. A consensus was reached among panelists and attendees on many points regarding method validation of small molecules.

Bioanalytical method development and validation using incurred samples--simultaneous quantitation of ramipril and ramiprilat in human EDTA plasma by LC-MS/MS.

A new method development and validation approach is proposed in order to develop a reliable method for the simultaneous quantitation of ramipril and ramiprilat in the presence of numerous labile metabolites. This new approach involves the usage of a synthesized labile acyl glucuronide of ramipril as well as individual and pooled incurred (study) samples in the development and validation process. Following the method validation and prior to its application to a large clinical study, a mini pilot study was performed to evaluate the performance of the method.

Internal standard response variations during incurred sample analysis by LC-MS/MS: Case by case trouble-shooting.

Internal standard (IS) responses can directly impact the accuracy of reported concentrations in bioanalysis as the majority of LC-MS/MS methods are based on analyte/IS response ratios for quantitation. Due to the complexity of incurred sample matrices and drug formulation, variable IS responses are quite common upon applying a validated method to the analysis of incurred samples. To maintain the integrity of a study and to avoid economic losses, it is therefore extremely important to monitor IS response variations during bioanalysis and to quickly identify the root causes if variations are observed.

Mass spectrometric quantitation of C-reactive protein using labeled tryptic peptides.

Given the extensive efforts applied toward proteomics and research in biomarkers, methods for the simultaneous measurement of proteins, peptides, metabolic intermediates, hormones, etc. in a complex sample may be required in the foreseeable future. Assays based on mass spectrometric detection may be suitable for meeting the demands of such complex samples with sensitivity and specificity.

Regulation of cytochrome P450 by posttranslational modification.

Cytochrome P450s are a family of enzymes represented in all kingdoms with expression in many species. Over 3,000 enzymes have been identified in nature. Humans express 57 putatively functional enzymes with a variety of critical physiological roles.

Complete chemical and enzymatic treatment of phosphorylated and glycosylated proteins on ProteinChip arrays.

A simple and quick protocol for chemical treatment, enzymatic digestion, and subsequent identification of proteins on ProteinChip arrays is presented. Chicken ovalbumin, bovine fetuin and a heavily posttranslationally modified protein, human epidermal growth factor receptor extracellular domain, were employed as model proteins to evaluate the novel protocol. The chemical treatment includes denaturation, reduction, and alkylation, while enzymatic digestion encompasses deglycosylation, dephosphorylation, and digestion by various proteases.

Sensitive capillary chromatography mass spectrometric methods for the determination of salcatonin in human biological matrices.

New methods employing capillary liquid chromatography in combination with time-of-flight mass spectrometry (microLC-TOF/MS) were developed for the rapid determination of salcatonin in human urine and plasma. The present approaches utilize (13)C(6)-leucine (19)-labeled salcatonin as internal standard, small matrix volumes and simple sample preparation procedures. They allow TOF/MS to be used as a highly selective detector for providing accurate quantitation of salcatonin.

Substance P and neurotensin are up-regulated in the lumbar spinal cord of animals with neuropathic pain.

Many neuropeptides have been shown to be up-regulated in response to pain. The purpose of this study was to identify pain-related peptides in a rat model of neuropathic pain induced by sciatic nerve cuff implantation. Rats were tested for touch sensitivity prior to and 7 days following cuff implantation or sham surgeries.

Validation of a sensitive and automated 96-well solid-phase extraction liquid chromatography-tandem mass spectrometry method for the determination of desloratadine and 3-hydroxydesloratadine in human plasma.

To support clinical development, a liquid chromatographic-tandem mass spectrometric (LC-MS-MS) method was developed and validated for the determination of desloratadine (descarboethoxyloratadine) and 3-OH desloratadine (3-hydroxydescarboethoxyloratadine) concentrations in human plasma. The method consisted of automated 96-well solid-phase extraction for sample preparation and liquid chromatography/turbo ionspray tandem mass spectrometry for analysis. [2H(4)]Desloratadine and [2H(4)]3-OH desloratadine were used as internal standards (I.