Spectrophotometric Determination of Some Fluoroquinolone Derivatives in Dosage Forms and Biological Fluids Using Ion‐Pair Complex Formation

Abstract

A simple, rapid, sensitive, and reproducible procedure for assaying norfloxacin (NOR), ciprofloxacin (CIP), and ofloxacin (OFL) was investigated. The procedure is based on the reaction of selected drugs with Sudan II (I), Congo red (II), and Gentian violet (III) in universal buffer to give soluble ion‐pair complexes. The effects of various parameters have been studied. Beer's law plots were obeyed in the concentration ranges 0.5–11 µg ml^?1, whereas Ringbom optimum ranges were 0.7–9.5 µg ml^?1. The apparent molar absorptivity (6.4×10⁴ L mol^?1 cm^?1), Sandell sensitivity (4.99 ng cm^?2), detection (0.13 µg ml^?1), and quantification (0.44 µg ml^?1) limits were calculated. The relative standard deviation for ten determinations, for samples containing 4.0 µg ml^?1, was found to be 1.40%. The influence of commonly employed excipients in the determination of the studied drugs was examined. There was no interference from degradate product results from thermal and hydrolytic treatments. The results obtained by the proposed procedure were statistically validated. The developed procedure was successfully applied to the determination of the studied drugs in dosage forms and biological fluids.     

Electrochemical Determination of Citalopram by Adsorptive Stripping Voltammetry–Determination in Pharmaceutical Products

Abstract

The electrochemical behavior of citalopram was studied by square‐wave and square‐wave adsorptive‐stripping voltammetry (SWAdSV). Citalopram can be reduced and accumulated at a mercury drop electrode, with a maximum peak current intensity being obtained at a potential of approximately ?1.25 V vs. AgCl/Ag, in an aqueous electrolyte solution of pH 12. A SWAdSV method has been developed for the determination of citalopram in pharmaceutical preparations. The method shows a linear range between 1.0×10^?7 and 2.0×10^?6 mol L^?1 with a limit of detection of 5×10^?8 mol L^?1 for an accumulation time of 30 s. The precision of the method was evaluated by assessing the repeatability and intermediate precision, achieving good relative standard deviations in all cases (≤2.3%). The proposed method was applied to the determination of citalopram in five pharmaceutical products and the results obtained are in good agreement with the labeled values.     

Square‐Wave Voltammetry Determination of Aspartame in Dietary Products Using a Boron‐Doped Diamond Electrode

Abstract

The use of square‐wave voltammetry in conjunction with a cathodically pretreated boron‐doped diamond electrode for the analytical determination of aspartame in dietary products is described. In this determination, the samples were analyzed without previous treatment in a 0.5 mol l^?1 H₂SO₄ solution. A single oxidation peak at a potential of 1.6 V vs. Ag/AgCl (3.0 mol l^?1 KCl) with the characteristics of an irreversible reaction was obtained. The analytical curve was linear in the aspartame concentration range 9.9×10^?6 to 5.2×10^?5 mol l^?1 with a detection limit of 2.3×10^?7 mol l^?1. The relative standard deviation (n=5) obtained was smaller than 0.2% for the 1.0×10^?4 mol l^?1 aspartame solution. The proposed method was applied with success to the determination of aspartame in several dietary products and the results were similar to those obtained using an HPLC method at 95% confidence level.     

Simultaneous Spectrofluorimetric Determination of Paracetamol and Caffeine in Pharmaceutical Preparations in Solid‐Phase Using Partial Least Squares Multivariate Calibration

Abstract

Partial least‐squares algorithm (PLS)‐1 was used for the solid‐phase spectrofluorimetric determination of paracetamol (PA) and caffeine (CF) in pharmaceutical formulations. In despite of the closely overlapping spectral bands, the method allows the simultaneous quantification and sample preparation prior to analysis is not required. The calibration set consisted of 96 samples with 100–400 mg/g^?1 PA plus 10–65 mg/g^?1 CF; another set of 25 samples was used for external validation. Agreement between predicted and experimental concentrations was fair (r=0.993 and 0.964 for PA and CF models). Prediction performance was evaluated in terms of the coefficient of variability (CV), relative predictive determination (RPD), and ratio error range (RER). The PLS‐1 model was used for the determination of PA and CF in pharmaceutical formulations.     

Flexible Potentiometric Minisensor Based on Manganese Dioxide‐Composite for the Determination of Hydrogen Peroxide in Bleach and Pharmaceutical Products

Abstract

A new flexible minisensor based on MnO₂/graphite/epoxy resin composite for the potentiometric determination of hydrogen peroxide was developed in this work. Under optimum experimental conditions, such as 25°C, 4 h of conditioning time in 0.1 mol L^?1 NH₃‐NH₄ ⁺ buffer solution (pH 8.5) and a composition of 10/60/30% w/w MnO₂/graphite/epoxy resin, respectively, the minisensor presented a Nernstian response for H₂O₂ in the concentration range from 6.0×10^?7 to 1.0×10^?3 mol L^?1, with a slope of ?58.5±0.2 mV/pH₂O₂ with a detection limit of 1.6×10^?8 mol L^?1 H₂O₂. The useful lifetime of the proposed minisensor was at least 6 months (over 670 determinations for each composite), the response time was smaller than 1.5 min, and it was successfully applied in the determination of hydrogen peroxide in bleach and pharmaceutical products.     

Post‐chemiluminescence Method of the Determination of Loperamide Hydrochloride in Human Plasma and Pharmaceutical by Using Dichlorofluorescein as Chemiluminescence Reagent

Abstract

A post‐chemiluminescence (PCL) was observed when loperamide hydrochloride solution was injected into the reaction mixture after the finish of CL reaction of alkaline N‐Chlorosuccinimide (NCS) and dichlorofluorescein. Based on this phenomenon, a simple, sensitive and fast flow injection PCL method was established for the determination of loperamide hydrochloride. The possible mechanism for the PCL reaction was discussed via the investigation of the CL kinetic characteristics, the CL spectra, the fluorescence spectra. The PCL intensity responded linearly to the concentration of loperamide hydrochloride in the range 8.0×10^?10 to 6.0×10^?7 g · ml^?1 with a linear correlation of 0.9995. The detection limit was 4×10^?10 g · ml^?1. The relative standard deviation was 2.4% for 4.0×10^?8 g · ml^?1 loperamide hydrochloride (n=11). This method has been applied to the determination of loperamide hydrochloride in human plasma and pharmaceutical samples with satisfactory results.     

High‐Performance Liquid Chromatographic Determination of Parecoxib in Human Plasma and Pharmaceutical Formulations

Abstract

A simple and sensitive RP‐HPLC method for the determination of parecoxib (PXB) in human plasma and pharmaceutical formulations has been developed and validated. The separation of PXB and the internal standard, ibuprofen (IBF) was achieved on a CLC C₁₈ (5 μ, 25 cm×4.6 mm i.d.) column using UV detector at 200 nm. The mobile phase consisted of acetonitrile‐water (92:8 v/v). The linear range of detection was found to be 0.9–18.4 µg/ml (r=0.9985). Intra‐ and inter‐day assay relative standard deviations were observed to be less than 0.3%. The method has been applied successfully for the determination of PXB in spiked human plasma and pharmaceutical preparations. Analytical parameters were calculated and complete statistical evaluation is incorporated.     

Determination of Chromate Ion in Water Using High Performance Capillary Electrophoresis

ThereisarapidIyincreasingdemandforfastandreliableanalyticaImethodsforthedeterminationofchemicaIformsofelementSinenvironmentalsamples.IthaslongbeenknownthatCrfIII)isessentialformammals,however,CrfVI)isconsideredtobeatoxicagent[l].Theanalysisofchromateion(Vl)inenvironmentwaterisusuallyperformedbyusingspephotometryandatomicabsorption,p..tr...ny[2].TheformerneedsfairIylargeamountofsample,pretreatmenLandlonganalysistime.Thelaterequipmentismuchmoreexpensive.InpreviousreportS,chromateisnormaI1…     

Micro‐ and Nanoemulsions in Cosmetic and Pharmaceutical Products

This article presents a model of droplet disruption in an ultrasonic field. It describes the experiments with preparing fine emulsions in the ultrasonic field.     

RP‐HPLC Method for the Determination of Tenofovir in Pharmaceutical Formulations and Spiked Human Plasma

Abstract

A simple reverse‐phase high‐performance liquid chromatographic method for the determination of tenofovir disoproxil fumarate (TDF) in pharmaceutical formulations and human plasma samples has been developed and validated. Piroxicam (PRX) was used as an internal standard. The assay of the drug was performed on a CLC C₁₈ (5 μ, 25 cm×4.6 mm i.d.) with UV detection at 259 nm. The mobile phase consisted of acetonitrile–water mixture in the ratio of 75∶25, and a flow rate of 1 ml/min was maintained. The standard curve was linear over the range of 0.2–10 µg/ml (r ²=0.9966). Analytic parameters have been evaluated. Within‐day and between‐day precision as expressed by relative standard deviation was found to be less than 2%. The method has been applied successfully for the determination of TDF in spiked human plasma samples and pharmaceutical formulations.     

A Sensitive and Specific High-Performance Thin-Layer Chromatography—Densitometry Method for Determination of Rebamipide in the Bulk Material and in Pharmaceutical Formulation

JPC – Journal of Planar Chromatography – Modern TLC -     

LC–UV Method with Pre-Column Derivatization for the Determination of Ciclopirox Olamine in Raw Material and Topical Solution

A rapid, simple and sensitive liquid chromatographic method has been developed to assay ciclopirox olamine in raw material and topical solution. The analysis used a reversed-phase C₁₈ end-capped column, with UV detection at 305 nm and pre-column derivatization with dimethyl sulphate. A linear response (r ² > 0.999) was observed in the range of 0.4–200 μg mL^?1. The method showed good recoveries for the raw material and topical solution and the relative standard deviation intra and inter-day were ≤2.00%. Validation parameters such as specificity and robustness were also determined. The proposed method provided an accurate and precise analysis of ciclopirox olamine in raw material and topical solution.     

High‐Performance Liquid Chromatography Determination of Latanoprost in Pharmaceutical Formulations using UV Detection

Abstract

A simple, fast, and accurate high‐performance liquid chromatography (HPLC) method was developed to determine latanoprost in pharmaceutical formulations. The drug was chromatographed on a C₁₈ column. Eluents were monitored at a wavelength of 210 nm using a mixture of acetonitrile and 0.05 M potassium phosphate buffer pH 3.0 (70:30, (v/v). A linear response (r>0.9998) was observed in the range of 10.0–90.0 µg mL^?1. The method showed good recoveries (average 100.4%) and the relative standard deviations intra‐ and inter‐day were ≤1.0%. The method can be used for quality control assay of latanoprost in raw materials as well as in pharmaceutical formulations.     

Highly Sensitive Determination of Traces of Co(II) in Pharmaceutical and Urine Samples Using Kinetic–Spectrophotometric Method

Abstract

A high sensitive, accurate and simple kinetic method has been developed for determination of trace of Co(II) ions, based on its strongly catalytic effect in the reaction oxidation of disodium-6-hydroxy-5-[(4-sulfophenyl)azo]-2-naphtalenesulfonic acid (artificial color, Sunset Yellow FCF, E110 in text selected as SY) by hydrogen peroxide in borate buffer at pH of 9.5, by monitoring the rate of disappearance of SY. Reaction rate was monitored spectrophotometrically, at λ_max of the SY at 478.4 nm. The optimum operating conditions regarding reagents concentration and temperature were established. The tangent method was adopted for constructing the calibration curve, which was found to be linear over the concentration range 1.18–17.67 ng ml^?1 and 17.67–58.90 ng ml^?1 of Co(II). The limit of detection (3σ) is 0.15 ng ml^?1, and limit of quantification (10σ) is 0.5 ng ml^?1. The effects of the other ions on the reaction rate were determined for an assessment of the selectivity of the method. The developed kinetic procedure was successfully applied for the determination of Co(II) in pharmaceutical and urine samples. The unique features of this procedure are that the determination can be performed at room temperature, and the analysis time is short. The newly developed method is high sensitive, simple, inexpensive and efficient for use in the analysis of a large number of samples.     

PLS Regression in the Spectrophotometric Data for the Simultaneous Determination of Levodopa and Carbidopa in Pharmaceutical Preparations by Using an Enzymatic Stopped‐Flow FIA Technique

Abstract

An enzymatic stopped‐flow‐injection analysis is proposed for simultaneous determination of levodopa and carbidopa in pharmaceutical preparations. The dopaquinones obtained after the oxidation catalized by the enzyme were measured by spectrophotometric method. A reduced calibration matrix based on a central composite experimental design was built and Partial Least Squares (PLS) was applied on the spectral data after reaction with the enzyme. The LOD was 0.015 and 0.0028 mg ml^?1, respectively and the sample throughput was 22.5 h^?1. The proposed method was applied to pharmaceutical preparations and the results are in close agreement with pharmacopeial method. The recovery study and results were satisfactory.     

Flow‐Based Fluorimetric Determination of Furosemide in Pharmaceutical Formulations and Biological Samples: Use of Micelar Media to Improve Sensitivity

Abstract

Two fast flow injection procedures with fluorimetric detection based on the furosemide emission are presented. The first configuration used a phosphate buffer solution pH 3.00, 0.2 ionic strength (μ) solution flowing at 3.0 ml min^?1 as carrier, a 80 cm sample loop (400 µl total sample injection), and a 40 cm long reactor coil, which was kept at room temperature; the second has a unique difference: the introduction of a new channel of surfactant solution with reduction of flow rate. The excitation and emission were carried out at 270 and 410 nm, respectively; both systems presented linear dynamic range from 1.0×10^?7 to 1.0×10^?5 mol l^?1. The limit of detection (3σ/slope) was 3.0×10^?8 mol l^?1, to the first system, and 10^?8 mol l^?1 for the second one. Both proposed methods were applied to three commercial samples from different suppliers, as tablets and ampoules, and a synthetic urine sample spiked with the analyte. They presented an analytical frequency of 90 and 60 measurements per hour, respectively to phosphate and micelar media. The results agreed with those from the label and determined by a UV‐Vis spectrophotometric comparative procedure. Recoveries around 101% were found in the commercial formulations and synthetic urine matrixes.     

Determination of α-tocopherol in Cosmetic Products by Chronopotentiometry

Abstract

In the present study, a rapid chronopotentiometric method was developed for the determination of α-tocopherol in various cosmetic products. Determination of α-tocopherol is based on its irreverse oxidation by constant current at the planar glassy carbon electrode. The influence of the most important experimental parameters of chronopotentiometry was investigated. After optimization, an appropriate procedure for the sample preparation was developed. Under the defined experimental conditions, a detection limit of 7.5 mg L^?1 of α-tocopherol was obtained. The accuracy of the defined method was confirmed by means of recovery assay. The developed method was successfully applied to quantitation of α-tocopherol in various cosmetic products.     

Ammonium Ion Optical Sensor Formation and Characterization of a Self‐Assembled Thiazole Containing Dibenzo‐18‐Crown‐6 Monolayer toward Developing Ammonium Ion‐Sensing Interface

Abstract

This letter demonstrates a selective NH₄ ⁺ detection using a synthesized thiazole benzo crownether ethylamine‐lipoic acid conjugate (1) monolayer. A self‐assembled monolayer (SAM) of 1 was formed on Au surface and well characterized by atomic‐force microscopy, Fourier transform infrared reflection absorption spectroscopy and cyclic voltammetry (CV). A good selectivity for NH₄ ⁺ sensing was observed in a range of 1.0×10^?1 to 1.0×10^?6 M by surface plasmon resonance.     

Determination of Some Heavy-metal-ions Using a Sulfur Ion Modified BZ Oscillating System

The oscillating reaction as one important phenomenon of nonlinear chemistry has been a focus in recent years. Among all oscillating systems, Belousov-Zhabotinskii (BZ) oscillating system was first found and studied extensively. The mechanism of BZ oscilla…     

Solid Phase Extraction of Trace Metals in Seawater Using Morpholine Dithiocarbamate‐Loaded Amberlite XAD‐4 and Determination by ICP‐AES

Abstract

Application of morpholine dithiocarbamate (MDTC) coated Amberlite XAD‐4, for preconcentration of Cu(II), Cd(II), Zn(II), Pb(II), Ni(II) and Mn(II) by solid phase extraction and determination by inductively coupled plasma (ICP) atomic emission spectrometry (AES) was studied. The optimum pH values for quantitative sorption of Cu(II), Cd(II), Zn(II), Pb(II), Ni(II), and Mn(II) were 6.5–8.0, 7.0–8.5, 6.0–8.5, 6.5–8.5, 7.5–9.0, and 8.0–8.5, respectively. The metals were desorbed with 2 mol L^?1. The t_1/2 values for sorption of metal ions were 2.6, 2.9, 2.5, 2.6, 3.0, and 3.8 min respectively for Cu(II), Cd(II), Zn(II), Pb(II), Ni(II) and Mn(II). The effect of diverse ions on the determination of the previously named metals was studied. Simultaneous enrichment of the six metals was accomplished, and the method was applied for use in the determination of trace metal ions in seawater samples.