Stability-Indicating Methods for the Determination of Cimetidine Using Derivative and Fourier-Transform Infrared Spectrophotometry

Abstract

Two different techniques, that is, second (D₂) and third (D₃) derivative spectrophotometry and fourier transform infrared (FTIR) Spectrophotometry, are investigated for the selective determination of the intact cimetidine in presence of up to 25% and 75% of its degradates, respectively. The procedures determine 2–10 jag ml^?1 at 224 nm and 217.5 nm by D₂ and D₃, respectively, and 1–6 mg per 250 mg in K Br by the FTIR with mean accuracies of 100.0 ± 1.07%, 100.5 ± 0.87% and 100.3 ± 1.16%, respectively. The drug is successfully analysed in its pharmaceutical formulations.

     

Sensitive Synchronous Spectrofluorimetric Study of Certain Sunscreens Using Fluorescence Enhancers in Cosmeceutical Formulations

Synchronous spectrofluorimetric methods could be successfully adopted for simultaneous determination of Octinoxate (OMC), Avobenzone (AVO), Octyltriazone (OT), and Phenyl benzimidazole sulfonic acid (PBSA) in moisturizing sunscreen lotion, utilizing β-CD as fluorescence enhancer, and determination of Avobenzone (AVO), Homosalate, Tinosorb M and Phenyl benzimidazole sulfonic acid (PBSA) in presence of Octocrylene (OCR) in whitening sunscreen cream, using micellar medium of Sodium Dodecyl Sulfate (SDS) to enhance fluorescence intensity. For first product, zero order synchronous spectrofluorimetric method was used for determination of OMC and AVO, and derivative synchronous spectrofluorimetric technique was utilized for OT and PBSA in quaternary mixture. Linear calibration curves were obtained in a concentration range of 0.5–8 μg mL^??1 for OMC and AVO, and in range of 0.05–3 μg mL^??1 for OT and 0.001–5 μg mL^??1 for PBSA, by measuring the fluorescence at 370, 405, 333.2 and 340.6 nm, respectively. For second product, first derivative synchronous fluorescence method was used for each UV-filter. A linear calibration curves were obtained in a concentration range of 0.5–8 μg mL^??1 for AVO, in range of 0.1–8 μg mL^??1 for Homosalate, 2–10 μg mL^??1 for Tinosorb M and 0.001–5 μg mL^??1 for PBSA, by measuring the fluorescence at 409.8, 373, 307.2 and 316.8 nm, respectively. The detection limits are well below the maximum admissible concentration. The proposed methods were validated according to ICH guidelines and successfully applied to determine sunscreens in pure form and in Cosmeceutical formulations. All the results obtained were compared with those of published methods, where no significant difference was observed.     

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.     

UV-Spectroscopic Determination of Mixtures of Tetramethrin and Piperonyl Butoxide in Pharmaceutical Formulations

Abstract

A simple rapid and accurate UV-spectroscopic method have been developed for determination of tetramethrin in presence of piperonyl butoxide, which are present in Licid^R, a newly introduced pharmaceutical drug in Egypt used as antilice, and antiscopis. The method is applicable in the concentration range of 1–12 μg.ml^?1 and 1–50 μg.ml^?1 for tetramethrin and piperonylbutoxide respectively. Average recoveries for tetramethrin and piperonyl butoxide in Licid^R spray and Licid^R lotion are 98.14 ± 0.3 – 103.88 ± 1.88 (Tetra), 103.78 ± 1.23 (piperonyl) and 100.62 ± 0.89 – 100.94 ± 1.10 (Tetra), 102.38 ± 1.02 (piperonyl) for the spray and lotion, respectively.     

Comparative Study of the Ratio Spectra Derivative Spectrophotometry,Derivative Spectrophotometry and Vierordt's Method Appued to the Analysis of Lisinopril and Hydrochlorothiazide in Tablets

Abstract

Three new spectrophotometric methods are described for the determination of lisinopril and hydrochlorothiazide in their binary mixturer: First derivative spectrophotometry ratio spectra derivative and Vierordt's method. The procedures do not require any prior separation. In the derivative spectrophotometry, the dA/dλ values in the first derivative spectra of the mixture were measured at 269.6 nm for lisinopril and at 279.8 nm for hydrochlorothiazide. The calibration graphs were linear in the range 25.56–129.50 μg.ml^?1 for lisinopril and 10.60–139.80 μg.ml^?1 for hydrochlorothiazide. In ratio spectra derivative spectrophotometry, the calibration graphs for 15.68–129.50 μg.ml^?1 lisinopril and for 5.98–139.80 μg.ml^?1 hydrochlorothiazide were obtained by measuring the signals at 253.7 nm and 243.6 nm for lisinopril and at 280.1 nm and 270.8 nm for hydrochlorothiazide. In Vierordt's method, A¹ ₁ (1 %, 1 cm) values of lisinopril and hydrochlorothiazide were determined at 259.8 nm and 272.7 nm in the zero-order spectra. The quantity of both compounds were calculated by using the A¹ ₁ (1 %, 1cm) values. The methods were successfully applied to a pharmaceutical formulation for determination of both active compounds.     

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.     

Structural Characterization of Aniline-Bentonite Composite by FTIR,DTA/TG,and PXRD Analyses and BET Measurement

ABSTRACT

The aniline species incorporated into the acid-activated bentonite matrices leads to the decay of the skeletal stretches centered at 1041 cm^?1 and the rise of new features in the phenyl ring frequency region, 1700–1400 cm^?1, demonstrates clearly the influence of the acid activation on the Lewis sites necessary for coordination of aniline to bentonite. The exothermic DTA features at 507, 684, and 725°C indicate the release of both the clusters and the decomposed fragments of the aniline-clay composite, and the highly stable carbonaceous residue, respectively. The basal difference by ～1.0 nm and the much smaller surface area (33.8 m²/g) than that of the nonintercalated bentonite (129.2 m²/g) prove the presence of the tilted aniline species between the interlamellar grooves of the bentonite framework.     

An Innovative Measurement of Extractable Proteins from Concentrated Latex Containing Eggshell Calcium Oxide Compounds by Near-Infrared Spectroscopy

ABSTRACT

Near-infrared reflectance (NIR) spectroscopy, in the spectral range of 1100–2500 nm, was used to measure the amount of the directly extractable proteins (EP) where a small amount can cause a latex allergy to patients. The NIR spectra revealed an amino or a peptide (N-H) of the extractable proteins from the concentrated rubber latex added with sodium dodecyl sulphate (SDS) and calcium chloride, the latter being obtained from the pyrolysis of eggshells at 900°C for 2 hr and dissolving in 2 M HCl. The extractable proteins measured by NIR are equal to 5306.58 ± 1727.00 µg/g (0.53%) close to the value obtained by the modified Lowry method, which is 5566.02 ± 717.39 µg/g (0.56%). A partial least square regression model (PLSR) of the NIR spectra and the extractable protein contents yields a correlation coefficient of .72, a root mean square error of calibration (RMSEC) of 1298 µg/g, and a small bias value of ?0.0002 µg/g. The absorbance peaks at the wavelengths of 1520 nm and 1980 nm are related to the first overtone N-H (υ₁N-H) and the asymmetric combination of N-H, respectively. Furthermore, the absorbance peaks at the wavelengths of 1450 nm and 1920 nm correspond to the first overtone of O-H (υ₁O-H) of the concentrated latex compounds. The results demonstrate the NIR spectroscopy potential as a fast and noninvasive measurement technique.     

Resonance enhanced multiphoton ionisation (REMPI) detection of Cl(2Pj) atom in the photodissociation of halogenated pyrimidines at 235 nm: role of triplet states

ABSTRACT

The dynamics of chlorine atom (²P_j) formation in the photodissociation process of halogen substituted pyrimidines, namely, 2,4,6-trichloropyrimidine and 5-chloro-2,4,6-trifluoropyrimidine have been studied around 235?nm using Resonance Enhanced Multiphoton Ionisation Time-of-Flight Mass Spectrometry technique. For the chlorine atom dissociation channel, we have determined the translational energy distribution, the recoil anisotropy parameter, β, and the spin–orbit branching ratio. In both the molecules, the TOF profiles for Cl (²P_3/2) and Cl* (²P_1/2) are found to be independent of laser polarisation suggesting a zero value for β, within the experimental uncertainties. For 2,4,6-trichloropyrimidine, the average translational energies for Cl and Cl* elimination channels are determined to be 6.0?±?1.2 and 7.0?±?1.5 kcal/mol, respectively. Similarly, for 5-chloro-2,4,6-trifluoropyrimidine, the average translational energies for Cl and Cl* elimination channels are determined to be 6.5?±?1.2 and 7.9?±?1.6 kcal/mol, respectively. Computational calculations are performed to generate the potential energy curves along the dissociating C-Cl bond using equation of motion coupled cluster with single and double excitations (EOM-CCSD) method. Computational studies suggest the role of triplet states in the photodissociation process forming the Cl atom.     

Effect of the particle size on the electrochemical performance of nano-Li2FeSiO4/C composites

Nano-Li₂FeSiO₄/C composites were prepared from three kinds of nano-SiO₂ (their particle sizes are 15?±?5, 30?±?5, and 50?±?5 nm, respectively) by a traditional solid-state reaction method. The as-prepared materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), elementary analyzer, Brunauer–Emmett–Teller (BET) analysis, galvanostatic charge–discharge test, and electrochemical impedance spectroscopy. XRD results reveal that nano-Li₂FeSiO₄ composites fabricated from nano-SiO₂ (smaller than 30 nm) have less impurity. SEM results indicate that the particle size of nano-Li₂FeSiO₄ composites is nearly accord with the particle size of nano-SiO₂. BET analysis indicates that the specific surface areas of LFS15, LFS30, and LFS50 are 35.10, 35.27, and 26.68 m² g, respectively, and the main pore size distribution of LFS15, LFS30, and LFS50 are 1.5, 5.5, and 10 nm, respectively. Electrochemical measurements indicate that nano-Li₂FeSiO₄ composites prepared from nano-SiO₂ of 30?±?5 nm have the best electrochemical performance among the three samples.     

Simultaneous measurements of indoor radon and thoron and inhalation dose assessment in Douala City,Cameroon

ABSTRACT

Radon, thoron and associated progeny measurements have been carried out in 71 dwellings of Douala city, Cameroon. The radon–thoron discriminative detectors (RADUET) were used to estimate the radon and thoron concentration, while thoron progeny monitors measured equilibrium equivalent thoron concentration (EETC). Radon, thoron and thoron progeny concentrations vary from 31?±?1 to 436?±?12 Bq?m^–3, 4?±?7 to 246?±?5 Bq?m^–3, and 1.5?±?0.9 to 13.1?±?9.4 Bq?m^–3. The mean value of the equilibrium factor for thoron is estimated at 0.11?±?0.16. The annual effective dose due to exposure to indoor radon and progeny ranges from 0.6 to 9?mSv?a^–1 with an average value of 2.6?±?0.1?mSv?a^–1. The effective dose due to the exposure to thoron and progeny vary from 0.3 to 2.9?mSv?a^–1 with an average value of 1.0?±?0.4?mSv?a^–1. The contribution of thoron and its progeny to the total inhalation dose ranges from 7 to 60?% with an average value of 26?%; thus their contributions should not be neglected in the inhalation dose assessment.     

Fluorimetric Determination of Some Sulfur Containing Compounds Through Complex Formation with Terbium (Tb<Superscript>+3</Superscript>) and Uranium (U<Superscript>+3</Superscript>)

Two simple, sensitive and specific fluorimetric methods have been developed for the determination of some sulphur containing compounds namely, Acetylcysteine (Ac), Carbocisteine (Cc) and Thioctic acid (Th) using terbium Tb⁺³ and uranium U⁺³ ions as fluorescent probes. The proposed methods involve the formation of a ternary complex with Tb⁺³ in presence of Tris-buffer method (I) and a binary complex with aqueous uranyl acetate solution method (II). The fluorescence quenching of Tb⁺³ at 510, 488 and 540 nm (λ_ex 250, 241 and 268 nm) and of uranyl acetate at 512 nm (λ_ex 240 nm) due to the complex formation was quantitatively measured for Ac, Cc and Th, respectively. The reaction conditions and the fluorescence spectral properties of the complexes have been investigated. Under the described conditions, the proposed methods were applicable over the concentration range (0.2–2.5 μg ml⁻¹), (1–4 μg ml⁻¹) and (0.5–3.5 μg ml⁻¹) with mean percentage recoveries 99.74±0.36, 99.70±0.52 and 99.43±0.23 for method (I) and (0.5–6 μg ml⁻¹), (0.5–5 μg ml⁻¹), and (1–6 μg ml⁻¹) with mean percentage recoveries 99.38±0.20, 99.82±0.28 and 99.93±0.32 for method (II), for the three cited drugs, respectively. The proposed methods were successfully applied for the determination of the studied compounds in bulk powders and in pharmaceutical formulations, as well as in presence of their related substances. The results obtained were found to be in agree statistically with those obtained by official and reported ones. The two methods were validated according to USP guidelines and also assessed by applying the standard addition technique.     

Selective Spectrofluorimetric Method with Enhanced Sensitivity for Determination of Silodosine in Dosage Form and Human Plasma. Application to Stability Studies and Content Uniformity Testing

A novel, sensitive and selective spectrofluorimetric method has been developed and validated for determination of silodosine (SLD) in its dosage form and human plasma. The method is based on nucleophilic substitution reaction of SLD with 5-(dimethylamino) naphthalene-1-sulfonyl chloride (dansyl chloride) in presence of 5.0 × 10^?4 M sodium carbonate (pH 10.50) to yield a highly fluorescent derivative that was measured at 435 nm after excitation at 347 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 30.0–200.0 ng ml^?1, with a correlation coefficient of 0.9979. The limits of detection (LOD) and quantification (LOQ) were found to be 5.44 and 16.47 ng ml^?1, respectively. The proposed method was validated according to ICH guidelines, and successfully applied to the assay of commercial capsules as well as content uniformity testing. The high sensitivity of the proposed method allowed its successful application to the analysis of SLD in spiked human plasma with % recovery of 92.88 ± 1.05–100.73 ± 0.75%, (n = 6). The application of the proposed method was further extended to stability studies of SLD after exposure to different forced degradation conditions, such as acidic, alkaline and oxidative conditions, according to ICH guidelines, where this work describe the first attempt for selective spectrofluorimetric determination of silodosine in plasma and in the presence of its oxidative degradation.     

Determination of Protoporphyrin IX Disodium Salt Based on Fluorescence Quenching of Glutathione-Capped Cadmium/Tellurium Quantum Dots

ABSTRACT

Aqueous glutathione-capped cadmium/tellurium quantum dots with a diameter of about 3 nm were synthesized. The fluorescence was quenched in the presence of protoporphyrin IX disodium salt, with the excitation wavelength at 320 nm. Under the optimal conditions, the quenched fluorescence intensity was linear in the range of 0.096–16 µg · mL^?1 with a concentration of protoporphyrin IX disodium salt, and the detection limit (3σ) was 2.8 × 10^?2 µg · mL^?1. The proposed method has been applied to the determination of protoporphyrin in serum samples with satisfactory results. The interaction mechanism was investigated.     

Improved characteristics for MOHOS memory with oxygen-rich GdO as charge storage layer annealed by NH3

Characteristics of metal–oxide–high-k–oxide–silicon (MOHOS) memories with oxygen-rich or oxygen-deficient GdO as charge storage layer annealed by NH₃ or N₂ are investigated. Transmission electron microscopy, X-ray photoelectron spectroscopy and X-ray diffraction are used to analyze the cross-sectional quality, composition and crystallinity, respectively, of the stacked gate dielectric with a structure of Al/Al₂O₃/GdO/SiO₂/Si. The MOHOS capacitor with oxygen-rich GdO annealed in NH₃ exhibits a good trade-off among its memory properties: large memory window (4.8 V at ±12 V, 1 s), high programming speed (2.6 V at ±12 V/100 μs), good endurance and retention properties (window degradation of 5 % after 10⁵ program/erase cycles and charge loss of 18.6 % at 85 °C after 10 years, respectively) due to passivation of oxygen vacancies, generation of deep-level traps in the grain boundaries of the GdO layer and suppression of the interlayer between GdO and SiO₂ by the NH₃ annealing.     

Characterization of an intermediate case exciton in the emission of Cd-doped and pure AgBr

Abstract

Pulsed emission data and ODMR spectra of the 580 nm band provide evidence for an intermediate case exciton in pure and Cd²⁺-doped AgBr. This interpretation is based on the observed g-factor and the absence of a wavelength shift of the emission after pulsed excitation in pure AgBr. It is supported by the response of the ODMR spectra as the microwave modulation frequency is changed. The two central ODMR lines observed in AgBr (g = 1. 78) are assigned to transitions from the m_s=±1 levels to the m_s = 0 level of an intermediate case triplet exciton, which has an exchange coupling (singlet-triplet splitting) of -1. 9 ± 0. 2 cm^?1.     

A new isotope andα-lines in the Th-Np region and their production cross-sections

In the fusion reactions of^20,22Ne with²⁰⁵Tl,²⁰⁸Pb, and²⁰⁹Bi the absolute production cross-sections of the²²⁷Np,^222–224Pa,^222–224Th, and²²¹Ac isotopes were measured and the products of the xn evaporation channels and theirα-decay properties were investigated. The identified isotope is²²⁷Np (7680±10 keV). A newα-line structure of²²⁴Pa was established (7460±10 keV (25±3 %) and 7555±10 keV (75±3 %)). Fourα-lines of²²³Th were identified (7290±10 keV (41±5 %), 7320±10 keV (29±5 %), 7350 ± 15 keV (20±5 %), and 7390±15 keV (10±4 %)). The half life of²¹⁷Fr was measured to be 16±2 μs and that of²²⁰Ra was found to be 17 ±2 ms.     

Modified Spectrophotometric Method for the Determination of Some Important Antibiotics Through Charge - Transfere Complexation Reaction with Chloranil

Abstract

A new modified Spectrophotometric procedures are presented for the determination of three pharmaceutical antibiotic compounds through charge-transfere complexation reaction with chloranil. The complex shows an absorption mAxima at 550 nm, having a molar absorptivity coefficient of 5.55×10³,7.81×10³ and 1.38×10⁴ 1. mol^?1cm^?1 for ampicillin, amoxycillin and neomycin, respectively. Optimization of the reaction conditions has been investigated Obediance to Beer's law (40μg/ml) permitted the assay of thes drugs in its dosage forms A variety of pharmaceutical dosage forms containing ampicillin, amoxycillin and neomycin are successfully analysed by the proposed procedure.