Hybrid Nanocomposite Based Graphene Sensor for Ultrasensitive Clomipramine HCl Detection

A potentiometric sensor modified with a nanocomposite of montmorillonite sheets decorated with polyaniline nanofibers (MT-PANI-NFs) as an efficient electroactive material and tricresyl phosphate (TCP) as a solvent mediator has been developed for the estimation of clomipramine HCl (CLP.HCl). The optimum potentiometric performance of the sensor was achieved by mixing of MT-PANI-NFs : TCP : graphene with a ratio of 2.69 : 30.11 : 67.20 (% wt/wt). The sensor exhibited a Nernstian slope of 59.0±0.1 mV decade⁻¹ over the concentration range of 1.0×10⁻⁵−1.0×10⁻² mol L⁻¹ with a theoretically calculated detection limit of 5.0×10⁻⁶ mol L⁻¹. The sensor performance was scrutinized in terms of several factors including thermal stability, pH effect, response time and selectivity. As, it displayed a high thermal stability at various temperature degrees (10–60 °C) with pH independency in the range of 3.5–8.5. Additionally, the developed sensor exhibited a very rapid performance for CLP.HCl detection with a fast response time of 4 s and reflecting a superior selectivity towards CLP.HCl over the other interfering species. SEM (scanning electron microscope) was used as a characteristic tool for the investigation of the proposed graphene sensor surface. Furthermore, the graphene sensor has been efficiently used for CLP.HCl estimation in its pharmaceutical formulations.     

Development and validation of gas chromatography-mass spectroscopy method for determination of prilocaine HCl in human plasma using internal standard methodology

The accurate determination of prilocaine HCl levels in plasma is important in both clinical and pharmacological/toxicological studies. Prilocaine HCl is quickly hydrolyzed to o-toluidine, causing methemoglobinemia. For this, the present work describes the methodology and validation of a GC-MS assay for determination of prilocaine HCl with lidocaine HCl as internal standard in plasma. The validation parameters of linearity, precision, accuracy, recovery, specificity, limit of detection and limit of quantification were studied. The range of quantification for the GC-MS was 20-250 ng/mL in plasma. Within-day and between-day precision, expressed as the relative standard deviation (RSD) were less than 6.0%, and accuracy (relative error) was better than 9.0% (n = 6). The analytical recovery of prilocaine HCl and IS from plasma has averaged 94.79 and 96.8%, respectively. LOQ and LOD values for plasma were found to be 20 and 10 ng/mL, respectively. The GC-MS method can be used for determination from plasma of prilocaine HCl in routine measurement as well as in pharmacokinetic studies for clinical use.     

Rapid colorimetric sensing of tetracycline antibiotics with in situ growth of gold nanoparticles

A colorimetric assay utilizing the formation of gold nanoparticles was developed to detect tetracycline antibiotics in fluidic samples. Tetracycline antibiotics showed the capability of directly reducing aurate salts into atomic gold which form gold nanoparticles spontaneously under proper conditions. The resulted gold nanoparticles showed characteristic plasmon absorbance at 526 nm, which can be visualized by naked eyes or with a spectrophotometer. UV–vis absorbance of the resulted gold nanoparticles is correlated directly with the concentrations of tetracycline antibiotics in the solution, allowing for quantitative colorimetric detection of tetracycline antibiotics. Reaction conditions, such as pH, temperature, reaction time, and ionic strength were optimized. Sensitivity of the colorimetric assay can be enhanced by the addition of gold nanoparticle seeds, a LOD as low as 20 ng mL⁻¹ can be achieved with the help of seed particles. The colorimetric assay showed minimum interference from ethanol, methanol, urea, glucose, and other antibiotics such as sulfonamides, amino glycosides etc. Validity of the method was also evaluated on urine samples spiked with tetracycline antibiotics. The method provides a broad spectrum detection method for rapid and sensitive detection of reductive substances such as tetracycline antibiotics in liquid and biological samples.     

Spectrofluorimetric Determination of Chlorpromazine Hydrochloride and Thioridazine Hydrochloride

Abstract

Fluorescence spectroscopy was applied to the development of a sensitive and simple method for the determination of chlorpromazine HCl and thioridazine-HCl. The method is based upon development of an intense fluorescence using N-bromosuccinimide as the fluorogenic reagent. The produced fluorescence has very characteristic excitation and emission spectra and was stable for at least one hour. The results were reproducible and as little as 5 ng/ml chloropromazine HCl and 1 ng/ml thioridazine-HCl could be determined. The method was applied successfully to the analysis of various commercially available dosage forms. The obtained results were in good agreement with those of the official BP 93 procedures.     

Effect of leaching concentration and time on the morphology of pores in porous glasses

Herein, porous glass was prepared by the acid leaching of phase-separated sodium borosilicate glass. The effects of hydrochloric acid (HCl) leaching concentrations varying from 0.1 to 3 M and of leaching times varying from 2 to 48 h on pore size and shape are reported here. The porous structure evolution was investigated through small angle X-rays scattering measurements and were compared to the classical nitrogen adsorption technique. We argue that the composition of these samples is not significantly modified with the acidic concentrations of the solution or with the leaching times tested. However, as expected a priori, we clearly show strong differences in porous structure. The investigation of different HCl leaching concentrations (from 0.1 to 3 M), with a small variation between each concentration, has enabled the observation of an interesting result. That is, we clearly show a non-linear effect of acidic concentration on the porous structure of these materials. At low acid concentrations, the specific area of these materials is relatively low. Increasing the HCl concentration to approximately 0.7 M leads to a strong increase in a specific BET area and total pore volume. However, further increasing of the acid concentration of the leaching solution leads to a decrease of both the specific surface area and the total pore volume. All of these results due to the presence of colloidal silica inside the pore structure can be explained by the well-known Zhdanov's model. These nanoparticles formed at an intermediate acid concentration seem to cluster when the acidity increases. The effect of the leaching time is less significant than the HCl concentration; however, this same assumption can be explained by the experimental results.     

Synthesis and growth mechanism of zirconia nanotubes by anodization in electrolyte containing Cl−

The formation and growth of a self-organized zirconia porous layer can be achieved directly by anodization of Zr in chloride containing electrolytes. The morphology of the porous layers is affected by electrochemical conditions such as Cl⁻ concentration. Zirconia nanotubes with diameters ranging from 250 to 300 nm and a length of 33 μm were formed under proper conditions. The nanotubes have smooth and straight walls. The composition of the nanotubes was characterized by using an energy dispersive spectrometer. Selected area electron diffraction investigation reveals that the as-anodized zirconia nanotubes have an amorphous structure. Crystal phase transition and structural stability of the ZrO₂ nanotubes after heat treatment were characterized. A possible growth mechanism is presented.     

The use of hot‐stage microscopy and thermal micro‐Raman spectroscopy in the study of phase transformation of metoclopramide HCl monohydrate

The aim of this work was to investigate the transformation behavior of metoclopramide HCl with monohydrate (MCP HCl H₂O) using differential scanning calorimetry (DSC), thermogravimetric analysis, hot‐stage microscopy (HSM), and thermal micro‐Raman spectroscopy. The results of the present study indicate that the three‐step phase transformation of MCP HCl H₂O was clearly determined via the thermal‐dependant Raman spectral changes. These three steps of phase transformation were dehydration, recrystallization, and new crystal formation, which were markedly correlated with the endothermic and exothermic results of DSC study and the observations of HSM. The results generally evidence that MCP HCl H₂O crystals were first dehydrated to form an anhydrous sample, then recrystallized and transformed to a new crystal form of MCP HCl. Copyright © 2011 John Wiley & Sons, Ltd.     

A Visible‐Light‐Induced α‐H Chlorination of Alkylarenes with Inorganic Chloride under NanoAg@AgCl

An efficient, photocatalytic chlorination of alkylarene α‐H groups using NaCl/HCl as a chlorine source has been developed, which involves a radical mechanism under visible‐light (including sunlight) conditions. A chlorine radical is proposed to be formed by an electron transfer from chloride ion to O₂ in air through the bandgap hole of the semiconductor AgCl. The chlorination protocol is characterized by its use of natural sunlight or other visible light, mild conditions, cheap source of chlorine, green solvent, and high selectivity. The yield of benzylchloride is 95 % with a toluene conversion as high as 40 %, which rivals traditional chlorination methods.