Stability-Indicating Spectrofluorimetric Method for Determination of Itopride Hydrochloride in Raw Material and Pharmaceutical Formulations

A simple, sensitive and rapid spectrofluorimetric method for determination of itopride hydrochloride in raw material and tablets has been developed. The proposed method is based on the measurement of the native fluorescence of the drug in water at 363 nm after excitation at 255 nm. The relative fluorescence intensity-concentration plot was rectilinear over the range of 0.1–2 μg/mL (2.5?×?10^?7–5.06?×?10^?6 mole/L), with good correlation (r?=?0.9999), limit of detection of 0.015 μg/mL and a lower limit of quantification of 0.045 μg/mL. The described method was successfully applied for the determination of itopride hydrochloride in its commercial tablets with average percentage recovery of 100.11?±?0.32 without interference from common excipients. Additionally, the proposed method can be applied for determination of itopride in combined tablets with rabeprazole or pantoprazole without prior separation. The method was extended to stability study of itopride. The drug was exposed to acidic, alkaline, oxidative and photolytic degradation according to ICH guidelines. Moreover, the method was utilized to investigate the kinetics of the alkaline, acidic and oxidative degradation of the drug. A proposal for the degradation pathways was postulated.     

Flip-back, an old trick to face highly contrasted relaxation times: application in the characterization of pharmaceutical mixtures by CPMAS NMR

The ¹³C–¹H CPMAS with flip-back pulse NMR experiment is revisited in view of applications to pharmaceutical mixtures. The analysis of the kinetics of relaxation and CP transfer with and without the flip-back pulse shows that a significant gain in ¹³C signal can be expected (thus in experimental time) from the flip-back pulse for protons with long T₁. The gain is of the order of T₁ of the protons expressed in seconds. The experiment is applied on samples with highly contrasted spin-lattice relaxation times T₁ for protons, situation encountered in pharmaceutical mixtures. The application of the flip-back increases significantly the relative signal intensity of the component with the longer T₁, making this component detectable even after using short recycle delays. Therefore, this CPMAS with flip-back experiment could be used routinely to get ¹³C CPMAS NMR spectra of mixtures in constant experimental time and signal-to-noise ratio without the need for optimization of the recycle delays, and for whatever may be the degree of crystallinity of the active principal ingredient (API) and/or excipients.     

Spectrophotometric and Spectrofluorimetric Determination of Certain Diuretics Through Ternary Complex Formation with Eosin and Lead (II)

Simple and sensitive spectrophotometric and spectrofluorimetric methods have been developed for the determination of hydrochlorothiazide (I), indapamide (II) and xipamide(III) based on ternary complex formation with eosin and lead (II) in the presence of methylcellulose as surfactant. The methods do not involve solvent extraction. For spectrophotometric method, the ternary complex showed an absorption maximum at 543 nm. The factors affecting the formation of ternary complex were studied and optimized. The method obeys Beer’s law over concentration range of 8–40 μg mL⁻¹. A fluorescence quenching method for the determination of the cited drugs by forming this ternary complex was also investigated for the purpose of enhancing the sensitivity of the determination. The analytical performance of both methods was fully validated, and the results were satisfactory. The methods have been successfully applied for the determination of the studied drugs in their pharmaceutical tablets and the results obtained ware in good agreement with those obtained by the reference method. Common excipients used as additives in tablets do not interfere with the proposed methods.     

DERIVATIVE RATIO SPECTROPHOTOMETRY AND DIFFERENTIAL DERIVATIVE SPECTROPHOTOMETRIC DETERMINATION OF ISONIAZID AND PYRIDOXINE HYDROCHLORIDE IN DOSAGE FORMS

Derivative ratio spectrophotometric and differential derivative spectrophotometric methods, for the determination of isoniazid and pyridoxine hydrochloride in pharmaceutical dosage forms (tablets) is described. The first method depends on ratio derivative spectra spectrophotometry where isoniazid and pyridoxine hydrochloride were determined by the measurement of the first derivative ratio spectra of amplitudes (Abs.) at 250.7 and 305.8 nm, respectively. The other method, is based on differential derivative spectrophotometry for the simultaneous determination of isoniazid and pyridoxine hydrochloride in binary mixture without any pre-treatment by measuring the ΔD₁ values.

Both methods showed good linearity, precision and reproducibility. The proposed methods were successfully applied to the pharmaceutical dosage forms containing the above-mentioned drug combination without any interference by the excipients.     

A Spectrophotometric Method for the Determination of Buclizine Hydrochloride Using the Charge-Transfer Spectrum of Buclizine-Iodine Complex

Abstract

A simple and sensitive spectrophotometric method is described for the determination of buclizine hydrochloride in bulk and tablets form. The method is based on the formation of charge-transfer complex between buclizine, as n-donor, and iodine, as Δ acceptor, which measured spectrophotometrically at 295 and 355 nm. A Job's plot indicated a 1:1 complex between the drug and iodine and Beer's law was obeyed in a concentration range of 4–30 μg ml^?1. A more detailed investigation of the complex was made with respect to its association constant and the free energy change. The method is simple and sensitive and has been applied successfully to the analysis of laboratory-made tablets without any interference from the tablet excipients. To validate the method, the results obtained were compared statistically with a newly developed uv-derivative spectrophotometric method. The charge-transfer method was favored due to its higher sensitivity, cheap coast and available equipments.     

A Validated Spectrofluorimetric Method for the Determination of Citalopram in Bulk and Pharmaceutical Preparations Based on the Measurement of the Silver Nanoparticles-Enhanced Fluorescence of Citalopram/Terbium Complexes

A simple, sensitive, and accurate spectrofluorimetric method was developed for the determination of citalopram in bulk and pharmaceutical preparations. The method is based on the enhancement of the weak fluorescence signal (FL) of the Tb (III)-citalopram system in the presence of silver nanoparticles. Fluorescence intensities were measured at 555 nm after excitation at 281 nm. Prepared silver nanoparticles (AgNPs) were characterized by UV-Visible spectra and transmission electron microscopy (TEM). Various factors affecting the formation of citalopram-Tb (III)-AgNPs complexes were studied and optimized. The fluorescence intensity versus concentration plot was linear over the range 0.02–14 μg?mL^?1, with an excellent correlation coefficient of 0.9978. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 7.15?×?10^?6?μg?mL^?1 and 2.38?×?10^?5?μg?mL^?1 respectively. The proposed method was found to have good reproducibility with a relative standard deviation of 3.66 % (n?=?6). The interference effects of common excipients found in pharmaceutical preparations were studied. The developed method was validated statistically by performing recoveries studies and successfully applied for the assay of citalopram in bulk powder and pharmaceutical preparations. Percent recoveries were found to range from 98.98 % to 100.97 % for bulk powder and from 96.57 % to 101.77 % for pharmaceutical preparations.     

Spectrophotometric determination of sparfloxacin in pharmaceutical formulations and urine samples

A simple and sensitive spectrophotometric method has been developed for the determination of sparfloxacin in bulk and pharmaceutical formulations, and in artificial urine. Sparfloxacin was oxidized into a red colored product using ammonium monovanadate in acidic media. The proposed method was successfully applied to the determination of sparfloxacin in different pharmaceutical formulations (tablets) and in a spiked urine sample. The influence of commonly used excipients on the determination of sparfloxacin was studied. Percentage recoveries in the range of 98.0 ± 0.14 % to 100.0 ± 0.20 % were obtained. The observed data have been evaluated statistically which showed high accuracy and precision.     

Simple and Sensitive Spectrofluorimetric Method for the Determination of Oseltamivir Phosphate in Capsules Through Derivatization with Fluorescamine

A new, simple and sensitive spectrofluorimetric method has been developed for the determination of oseltamivir phosphate (OSP) in capsules. The method is based on the reaction between oseltamivir and fluorescamine in borate buffer solution of pH 8.50 to give highly fluorescent derivatives that are measured at 483 nm using an excitation wavelength of 381. The different experimental parameters effecting the development and stability of the reaction product were carefully studied and optimized. The fluorescence intensity concentration plot is rectilinear over the range 50–450 ng mL⁻¹ with a lower detection limit (LOD) of 1.219 ng mL⁻¹ and limit of quantitation (LOQ) of 4.064 ng mL⁻¹. Selectivity was validated by subjecting stock solution of OSP to acidic, basic, oxidative, and thermal degradation. No interference was observed from excipients present in formulations. The developed method was successfully applied to determination of the drug in capsules. The mean % recovery (n = 6) was 100.08. The results obtained were in good agreement with those obtained using a reported spectrophotometric method.     

Relativistic dynamics of interacting point particles: Central position of the Wheeler-Feynman scheme

The Wheeler-Feynman (WF) relativistic theory of interacting point particles, generalized by acceptance of an arbitrary spacelike interaction, is shown to possess a privileged status, reminiscent of the central force interactions occurring in Newtonian mechanics. This scheme is shown to be isomorphic to the classical one of the statics of interacting flexible current-carrying wires obeying the Ampère-Laplace (AL) formulas: to the tensionT (T ² =const) of the wire corresponds the momentum-energy pⁱ (p_ipⁱ=–c²m²) of the particle; to the Laplace linear force density –iH×dr corresponds the Lorentz force QH^ij dr_j; to the Laplace potential ir^–1 dr corresponds the WF potential Q(r²) drⁱ, etc. Among the differences, there is self-action in the AL scheme and no self-action in the WF scheme. A stationary energy principle in the AL scheme is isomorphic to Fokker's stationary action principle in the WF scheme.     

Validated Spectrofluorimetric Method for the Determination of Lamotrigine in Tablets and Human Plasma Through Derivatization with <Emphasis Type="BoldItalic">o</Emphasis>-phthalaldehyde

A sensitive, simple and selective spectrofluorimetric method was developed for the determination of Lamotrigine (LMT) in pharmaceutical formulations and biological fluids. The method is based on reaction of LMT with o-phthalaldehyde in presence of 2-mercaptoethanol in borate buffer of pH 9.8 to yield a highly fluorescent derivative that is measured at 448 nm after excitation at 337 nm. The different experimental parameters affecting the development and stability of the reaction product were carefully studied and optimized. The fluorescence-concentration plot was rectilinear over the range of 0.1–1.0 μg ml⁻¹ with lower limit of detection (LOD) 0.02 μg ml⁻¹ and limit of quantification (LOQ) 0.06 μg ml⁻¹ respectively. The proposed method was successfully applied to the the analysis of commercial tablets. Statistical comparison of the results obtained by the proposed and reference method revealed no significant difference in the performance of the two methods regarding the accuracy and precision respectively. The proposed method was further extended to the in-vitro and in-vivo determination of the drug in spiked and real human plasma. The mean percentage recoveries in spiked and real human plasma (n = 3) were 95.78 ± 1.37 and 90.93 ± 2.34 respectively. Interference arising from co-administered drugs was also studied. A proposal for the reaction pathway with o-phthalaldehyde was postulated.     

Stability - Indicating Method For The Determination of Bromazepam And Delorazepam Via Proton Magnetic Resonance Spectroscopy

A new, simple proton magnetic resonance method (¹HNMR) for the rapid and direct quantitation of intact bromazepam and delorazepm in presence of their acid - induced degradation products is presented. DMSO - d₆ is used as a solvent and maleic acid as internal reference standard. The resonance peak of the two hydrogens of the methylene group of each drug near 4.2 ppm is integrated as a measure for the drug in comparison to the sharp singlet of maleic acid at about 6.25 ppm.

The proposed procedure gives accurate and reproducibe results when applied for the anlaysis of both drugs either per se, in mixtures with their degradation products or in their tablets.     

Spectrophotometric Determination of Metformin via Charge-Transfer Complex with Iodine

Abstract

A spectroscopic method is described for the determination of Metformin based on its formation of molecular complex with iodine in dichloroethane. Quantitative measurements are made at the maximum absorption of 295nm. The molar ratio of the formed metformin-iodine complex is 1:1 as revealed by Job's method. Beers' law is obeyed in the range 2–12 ug.ml^?1 base solution. The proposed method is statistically comparable with the official B. P. method. When applied to pharmaceutical preparation, tablets, average percentage recovery of 99.97 ± 0.81 was obtained.     

VCSEL-based oxygen spectroscopy for structural analysis of pharmaceutical solids

We present a minimalistic and flexible single-beam instrumentation based on sensitive tunable diode laser absorption spectroscopy (TDLAS) and its use in structural analysis of highly scattering pharmaceutical solids. By utilising a vertical cavity surface emitting laser (VCSEL) for sensing of molecular oxygen dispersed in tablets, we address structural properties such as porosity. Experiments involve working with unknown path lengths, severe backscattering and diffuse light. These unusual experimental conditions has led to the use of the term gas in scattering media absorption spectroscopy (GASMAS). By employing fully digital wavelength modulation spectroscopy and coherent sampling, system sensitivity in ambient air experiments reaches the 10^-7 range. Oxygen absorption exhibited by our tablets, being influenced by both sample porosity and scattering, was in the range 8×10^-5 to 2×10^-3, and corresponds to 2–50 mm of path length through ambient air (L_eq). The day-to-day reproducibility was on average 1.8% (0.3 mm L_eq), being limited by mechanical positioning. This is the first time sub-millimetre sensitivity is reached in GASMAS. We also demonstrate measurements on gas transport on a 1-s time scale. By employing pulsed illumination and time-correlated single-photon counting, we reveal that GASMAS exhibits excellent correlation with time-domain photon migration. In addition, we introduce an optical measure of porosity by relating oxygen absorption to average photon time-of-flight. Finally, the simplicity, robustness and low cost of this novel TDLAS instrumentation provide industrial potential. PACS 42.62.Fi; 39.30.+w; 78.55.Mb; 42.62.Cf; 87.64.Cc     

Reference database of Raman spectra of pharmaceutical excipients

Raman spectroscopy has evolved into an important fast, direct and nondestructive technique in pharmaceutical analysis. Usually, the focus in this field is mainly on the active ingredients and not on the excipients present in the drugs. A collection of Raman spectra of widely used pharmaceutical excipients is presented in this article, which can serve as a reference for the interpretation of Raman spectra during drug analysis (including classical qualitative and quantitative pharmaceutical analysis, counterfeit tracing and process analytical technology (PAT) applications). The 43 analyzed excipients can be classified into seven categories: mono‐ and disaccharides (dextrose, lactitol, maltitol, lactose and sucrose), polysaccharides (microcrystalline cellulose, methylcellulose (MC), carboxymethylcellulose (CMC), hydroxypropyl cellulose (HPC), hydroxypropyl methylcellulose (HPMC), wheat starch, maltodextrin, primojel, tragacanth and pectin), polyalcohols (propylene glycol, erythritol, xylitol, mannitol and sorbitol), carboxylic acids and salts (alginic acid, glycine, magnesium stearate, sodium acetate and sodium benzoate), esters (arachis oil, lubritab, dibutyl sebacate, triacetin, Eudragit E100 and Eudragit RL100), inorganic compounds (calcium phosphate, talc, anatase and rutile (TiO₂), calcium carbonate, magnesium carbonate, sodium bicarbonate and calcium sulfate) and some unclassified products [gelatin, macrogol 4000 (polyethylene glycol (PEG), polyvinyl pyrrolidone and sodium lauryl sulfate]. Copyright © 2008 John Wiley & Sons, Ltd.     

Micelle-Enhanced Spectrofluorimetric Method for Determination of Cholesterol-Reducing Drug Ezetimibe in Dosage Forms

A simple and sensitive spectrofluorimetric method was developed for the determination of ezetimibe in its pharmaceutical formulations. The proposed method is based on investigation of the fluorescence spectral behavior of ezetimibe in sodium dodecyl sulfate (SDS) micellar system. In aqueous solution of acetate buffer pH 5.0, the fluorescence intensity of ezetimibe was greatly enhanced, 200% enhancement, in the presence of SDS. The fluorescence intensity of ezetimibe was measured at 380 nm after excitation at 268 nm. The fluorescence-concentration plot was rectilinear over the range of 0.03–3.0 μg/mL with lower detection limit of 3.08 × 10⁻³ μg/mL. The method was successfully applied to the analysis of ezetimibe in its commercial tablets; the results were in good agreement with those obtained with the reported method. The application of the proposed method was extended to the stability studies of ezetimibe after exposure to different forced degradation conditions, such as acidic, alkaline, photo and oxidative conditions, according to ICH guidelines.     

Fluctuation-induced magnetotransport of superconductors in the quasiballistic regime

We study the fluctuation-induced magnetotransport of a two-dimensional superconductor in the quasiballistic regime, where ξ _GL(T) ≪ ℓ (ℓ is the electron mean free path and ξ _GL(T) is the Ginzburg-Landau coherence length). The magnetoconductivity is evaluated in the nonlocal fluctuation regime thereby extending the existing theory valid in the local limit. We show that the Maki-Thompson (MT) and density-of-states (DOS) contributions strongly compensate each other and their sum is negligible in comparison with the Aslamazov-Larkin (AL) term. The hierarchy of the fluctuation contributions to the magnetoconductivity in the high-field limit is also qualitatively discussed. Received 10 July 2002 / Received in final form 21 November 2002 Published online 7 May 2003     

Vibrational spectroscopic study of budesonide

The Raman spectrum of budesonide is reported for the first time, and molecular assignments are proposed on the basis of ab initio BLYP DFT calculations with a 6‐31 G* basis set and vibrational wavenumbers predicted on a quasi‐harmonic approximation. Comparison with previously published infrared data has explained several spectral features, and the relative band intensities in the CO and CC stretching regions are interpreted. The results from this study provide data that can be used for the preparative process monitoring of budesonide, an important steroidal pharmaceutical in various dosage forms, and its interaction with excipients and other components. Copyright © 2007 John Wiley & Sons, Ltd.     

Spectrofluorimetric Protocol for Ceftriaxone in Commercial Formulation and Human Plasma After Condensation with Formaldehyde and Ethyl Acetoacetate

A new spectrofluorimetric method has been developed and validated for the quantification of ceftriaxone in bulk powder, pharmaceutical formulations and spiked human plasma. The developed method is reproducible, accurate, sensitive and cost effective. In this method, ceftriaxone was converted into a fluorescent compound by reacting with 0.8 M ethyl acetoacetate and 25% formaldehyde in a buffered medium (pH = 4.2) at 90 °C. The excitation and emission wavelengths of the fluorescent reaction product are 316 nm and 388 nm respectively. Optimization of the experimental conditions affecting the condensation reaction were carefully carried out and the optimum experimental conditions were incorporated in the procedure. The developed method has a broad linear range (0.2–20 μg mL⁻¹) with a correlation coefficient of 0.9992. The limit of detection (LOD) and limit of quantification (LOQ) was found to be 1.94 × 10⁻² μg mL⁻¹ and 6.47 × 10⁻² μg mL⁻¹ respectively. The common excipients and co-administered drugs were investigated for their interferences effect in the assay. The developed method was validated statistically through recovery studies and successfully applied to ceftriaxone determination in bulk powder, pharmaceutical formulations and spiked human plasma samples. The percent recoveries were found to be in the range of 99.04–100.26% for bulk powder, 98.88–99.92% for pharmaceutical formulations and 94.22–98.48% for spiked human plasma. The results were verified by comparing with reference literature HPLC method and were found in good agreement.     

Flow Injection Analysis of Pharmaceutical Compounds. VI. Determination of Some Central Nervous System Acting Drugs by UV-Spectrophotometric Detection

Abstract

The Present work describes a direct flow injection analysis (FIA) of five commonly used central nervous system (CNS) acting drugs namely amitriptyline hydrochloride, carbamazepine, clomipramine hydrochloride, fluphenazine hydrochloride and imipramine hydrochloride. The characteristics of the system and the conditions of the speatrophotometric determination are evaluated. The proposed technique can be applied for pharmaceutical quality control of the pure material and pharmaceutical dosage forms containing the drug. Amount ranging from 16 to 80 μg. ml^?1 of amitriptyline hydrochloride.

The Present work describes a direct flow injection analysis (FIA) of five commonly used central nervous system (CNS) acting drugs namely amitriptyline hydrochloride, carbamazepine, clomipramine hydrochloride, fluphenazine hydrochloride and imipramine hydrochlorode. The characteristics of the system and the conditions of the spectrophotometric determination are evaluated. The proposed technique can be applied for pharmaceutical quality control of the pure material and pharmaceutical dosage forms containing the drug. Amount ranging from 16 to 80 μ.ml^?1 of amitriptyline hydrochloride, carbamazepine and fluphenazine hydrochloride and from 32 to 160 μ. ml^?1 of clomipramine hydrochloride and imipramine hydrochloride dissolved and/or extracted in ethanol could be accurately analyzed. Standard addition (0.5 to 3 times of the claimed amounts) of authentic samples to powdered tablets gave good mean percent recoveries with low standard deviations. Samples can be introduced at rates of about 180 per hour or even more. The results obtained by applying the proposed FIA method are statistically analyzed and compared with those obtained from applying pharmacopoeial procedures.     

100 keV质子辐照对空间GaAs/Ge太阳电池光电效应的影响

利用空间环境模拟设备,用固定能量为100keV、注量为1×10⁹—3×10¹²cm^-2的质子,对空间实用GaAs/Ge太阳电池进行了辐照试验.利用伏安(I-V)特性、光谱响应和光致发光(PL)光谱测试,研究分析了电池的光电效应.试验表明,电池的各种电性能参数如短路电流(I_sc)、开路电压(V_oc)、最大输出功率(P_{m< 关键词： GaAs/Ge太阳电池 质子辐照 光电效应}