Two validated chromatographic determinations of an antifungal drug,its toxic impurities and degradation product: A comparative study

Tolnaftate, a thionoester anti‐fungal drug, was subjected to alkaline hydrolysis to produce methyl(m‐tolyl)carbamic acid and β ‐naphthol (tolnaftate impurity A). N‐Methyl‐m‐toluidine, tolnaftate impurity D, was synthesized and structurally elucidated along with tolnaftate alkaline degradation products using IR, H¹NMR and MS. Two stability‐indicating HPTLC and RP‐HPLC methods were developed and validated, for the first time, for determination of tolnaftate, its alkaline degradation products and toxic impurities in the presence of methyl paraben, as a preservative in Tinea Cure^® cream. The proposed HPTLC method depended on separation of the studied components on TLC silica gel F₂₅₄ plates using hexane–glacial acetic acid (8:2, v/v) as a developing system and scanning wavelength of 230 nm. The proposed RP‐HPLC method was based on separation of the five components on an Eclipse plus C₁₈ column. The mobile phase used was acetonitrile–water containing 1% ammonium formate (40:60, v/v), with a flow rate of 1 mL/min and detection wavelength of 230 nm. The proposed methods allowed the assay of tolnaftate toxic impurities, β ‐naphthol and N‐methyl‐m‐toluidine, down to 2%, allowing tracing of β ‐naphthol that could be absorbed by the skin causing systemic toxic effects, unlike tolnaftate, indicating the high significance of such determination. International Conference on Harmonization guidelines were followed for validation.     

Thermal Degradation and Fire Behavior of High Performance Polymers

Abstract

High performance and high temperature polymers are a class of polymeric materials exhibiting high thermal stability and their resistance to fire makes them valuable assets for many applications. Those applications include as typical examples high temperature gas separation membranes, automotive and aerospace industry as well as the construction industry. The high performance polymers have been synthesized since the early 1960s, and have developed rapidly over the past few decades. Most high performance polymers comprise a highly aromatic backbone, linear chains, and strong inter-chain interactions. This review deals mostly with commercial polymeric materials. Studies regarding their thermal behavior, degradation mechanism and their reaction to fire have been synthetically combined in order to bring out potential insight concerning the effect of the thermal decomposition and thermal behavior on the fire properties of those polymers.     

A fast iterative method to find the matrix geometric mean of two HPD matrices

The purpose of this research is to present a novel scheme based on a quick iterative scheme for calculating the matrix geometric mean of two Hermitian positive definite (HPD) matrices. To do this, an iterative scheme with global convergence is constructed for the sign function using a novel three‐step root‐solver. It is proved that the new scheme is convergent and shown to have global convergence behavior for this target, when square matrices having no pure imaginary eigenvalues. Next, the constructed scheme is used and extended through a well‐known identity for the calculation of the matrix geometric mean of two HPD matrices. Ultimately, several experiments are collected to show its usefulness.     

Development and characterization of hydroquinone-loaded nanofiber for topical delivery: effect of chitosan

Hydroquinone (HQ) loaded polymer solution was electrospun for its topical application. Nanofibers were then investigated in terms of stability, drug release, and antifungal activity. The effect of chitosan (CS) was investigated on the viscosity, stability, drug release, and antifungal activity of the developed formulation. Results indicate a significantly stable HQ-loaded nanofiber formulation. The addition of CS caused hydration of the drug delivery system and enhanced drug release but reduced its stability. HQ-loaded nanofiber mat showed significant antifungal activity, however, there was no inhibition zone in samples containing CS.     

时间延迟扩散-波动分数阶微分方程有限差分方法

本文提出求解时间延迟扩散-波动分数阶微分方程有限差分方法，方程中对时间的一阶导函数用α阶（0 < α < 1） Caputo分数阶导数代替.文章中利用Lubich线性多步法对分数阶微分进行差分离散，且文章利用分段区间证明该方法是稳定的，且利用数值实验加以验证.     

Change points in heavy‐tailed multivariate time series: Methods using precision matrices

We propose two robust data‐driven techniques for detecting network structure change points between heavy‐tailed multivariate time series for situations where both the placement and number of change points are unknown. The first technique utilizes the graphical lasso method to estimate the change points, whereas the second technique utilizes the tlasso method. The techniques not only locate the change points but also estimate an undirected graph (or precision matrix) representing the relationship between the time series within each interval created by pairs of adjacent change points. An inference procedure on the edges is used in the graphs to effectively remove false‐positive edges, which are caused by the data deviating from normality. The techniques are compared using simulated multivariate t‐distributed (heavy‐tailed) time series data and the best method is applied to two financial returns data sets of stocks and indices. The results illustrate the method's ability to determine how the dependence structure of the returns changes over time. This information could potentially be used as a tool for portfolio optimization.     

管式炉中半导体激光器巴条Au80Sn20焊料封装研究

为了提高半导体激光器的封装质量和效率,引入管式炉利用夹具进行批量封装。由于封装质量的好坏直接影响半导体激光器的输出特性和使用寿命,利用MOCVD生长808 nm芯片,重点分析了管式炉温度和封装时间对半导体激光器巴条双面金锡封装质量的影响。利用X射线检测、结电压、光电特性参数和smile效应测试手段,确定了管式炉封装半导体激光器巴条的最优封装条件,为以后的产业化提供了指导意义。     

Highly sensitive and selective detect of p‐arsanilic acid with a new water‐stable europium metal–organic framework

The p‐arsanilic acid (p‐ASA), as an aromatic organoarsenic compounds, had received considerable concerns for their potential toxicity and carcinogenic properties. It was essential to detect p‐ASA with a facile method. In this paper, an europium based fluorescent metal–organic framework (MOF) [Eu₂(clhex)·2H₂O)]·H₂O ( BUC‐69 ) was successfully prepared under hydrothermal conditions with 1,2,3,4,5,6‐cyclohexanehexacarboxylic acid (H₆clhex) as organic linker. BUC‐69 displayed superior fluorescence capability to achieve selective and sensitive detection toward p‐ASA in water, which presented the first example of a MOF‐based sensor to detect p‐ASA. BUC‐69 showed excellent chemical stability in solutions under pH ranging from 4 to 12, which makes it be a potential sensor both in acidity and alkalinity condition. Significantly, BUC‐69 performed well in fluorescent sensing of p‐ASA at a low concentration (10^?6 M) in the simulated wastewater prepared with real lake water, and the results were comparable to the values detected by Inductively Coupled Plasma Optical Emission Spectrometer (ICP‐OES). The corresponding mechanism of fluorescent sensing toward p‐ASA with BUC‐69 was proposed and affirmed.     

Pharmacokinetic analysis of plasma bicyclol by liquid chromatography–tandem mass spectrometry

Bicyclol is a synthetic drug widely used to treat chronic hepatitis B. This study aimed to develop a selective, sensitive and high‐throughput liquid chromatography–tandem mass spectrometric method for the detection of bicyclol in human plasma. Bicyclol was detected using a multiple reaction monitoring mode, with ammonium adduct ions (m/z 408.2) as the precursor ion and the [M‐CH₃]⁺ ion (m/z 373.1) subjected to demethylation as the product ion. Chromatographic separation was achieved using a Zobax Eclipse XDB‐C₁₈ column with a gradient elution and a mobile phase of 2 mm ammonium formate and acetonitrile. Bicyclol was extracted from plasma matrix by precipitation. A linear detection response was obtained for bicyclol ranging from 0.500 to 240 ng/mL, and the lower limit of quantification was 0.500 ng/mL. The intra‐ and inter‐day precisions were all ≤7.4%, and the accuracies were within ±6.0%. The extraction recovery was >95.9%, and the matrix effects were between 96.0% and 108%. Bicyclol was found to be unstable in human plasma at room temperature, but the degradation was minimized by conducting sample collection and preparation in an ice bath. The validated method was successfully applied to investigate the pharmacokinetics of bicyclol tablets in six healthy Chinese volunteers.