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The current work suggests a new, ultrasensitive green functionalized sensor for the determination of anti-inflammatory medication diclofenac sodium (DCF). Alumina (Al2O3) and cerium oxide (CeO2) nanoparticles (NPs) have attracted great interest for their use as outstanding and electroactive nanocomposite in potentiometric and sensory research due to their ultrafunctional potential. The formed nanoparticles have been confirmed using various spectroscopic and microscopic techniques. The fennel extract-mediated Al2O3/CeO2 nanocomposite (Al2O3/CeO2 NCS) modified coated wire membrane sensor developed in this study was used to quantify DCF in bulk and commercial products. Diclofenac sodium was coupled with phosphomolybdic acid (PMA) to generate diclofenac phosphomolybdate (DCF-PM) as an active ion-pair in the existence of polyvinyl chloride (PVC) and o-nitrophenyl octyl ether (o-NPOE). Clear peaks at 270, and 303 nm with band gaps of 4.59 eV and 4.09 eV were measured using UV–vis spectroscopy of Al2O3 and CeO2, respectively. The crystallite sizes of the formed nanoparticles were XRD-determined to be 30.13 ± 8, 17.72 ± 3, and 35.8 ± 0.5 nm for Al2O3, CeO2, and Al2O3/CeO2 NCS, respectively. The developed sensor showed excellent response for the measurement and assay of DCF, with a linearity between 1.0 × 10−9 and 1.0 × 10−2 mol L−1. EmV = (57.76) log [DCF] +622.69 was derived. On the other hand, the typical type DCF-PM presented a potentiometric response range of 1.0 × 10−5-1.0 × 10−2 mol L−1 and a regression equation of EmV = (56.97) log [DCF]+367.16. The functionalized sensor that was proposed was successful in determining DCF in its commercial tablets with percent recovery 99.95 ± 0.3. Method validation has been used to improve the suitability of the suggested potentiometric technique, by studying various parameters with respect to the international council harmonization requirements for analytical methodologies.

The new research presents highly conductive polymeric membranes with a large surface area to volume ratio of metal oxide nanoparticles that were used to determine atropine sulfate (AT) in commercial dosage forms. In sensing and biosensing applications, the nanomaterials zinc oxide (ZnONPs) and magnesium oxide (MgONPs) were employed as boosting potential electroactive materials. The electroactive atropine phosphotungstate (AT-PT) was created by combining atropine sulfate and phosphotungstic acid (PTA) and mixing it with polymeric polyvinyl chloride (PVC) with the plasticizer o-nitrophenyl octyl ether (o-NPOE). The modified sensors AT-PT-ZnONPs or AT-PT-MgONPs showed excellent selectivity and sensitivity for the measurements of atropine with a linear concentration range of 6.0 × 10−8 − 1.0 × 10−3 and 8.0 × 10−8 − 1.0 × 10−3 mol L−1 with regression equations of E(mV) = (56 ± 0.5) log [AT] − 294 and E(mV) = (54 ± 0.5) log [AT] − 422 for AT-PT-NPs or AT-PT-MgONPs sensors, respectively. The AT-PT coated wire sensor, on the other hand, showed a Nernstian response at 4.0 × 10−6 − 1.0 × 10−3 mol L−1 and a regression equation E(mV) = (52.1 ± 0.2) log [AT] + 198. The methodology-recommended guidelines were used to validate the suggested modified potentiometric systems against various criteria. [ABSTRACT FROM AUTHOR]

In this study, a new high performance liquid chromatography (HPLC) analysis method was developed for the simultaneous determination of flurbiprofen (F) and thiocolchicoside (T) in pharmaceutical products. A C18 column (Agilent Poroshell 120 EC-C18) was used as the stationary phase. Elution of the analytes was achieved by using gradient elution system. Mobile phase A was an acetate buffer (100 mM, pH 4.8) and mobile phase B was acetonitrile. The flow rate for the method developed was 0.5 ml/min. The temperature of the column compartment was set at 40°C and the injection volume was 5 µl. Monitoring of the analytes was carried out at 248 nm. The method was found linear in the concentration range between 5-100 ppm. The correlation coefficient value was calculated as 0.999 for F and 0.999 for T. The method was found suitable in terms of accuracy, precision, specificity, linearity, and robustness ruggedness. Furthermore, it was applied successfully for the analysis of commercial tablets and gel samples that contains F and T without any time-consuming pre-procedure. The recovery values for Fand T were found as 99.5% and 97.0% in tablet formulations and 98.6% and 99.3% in gel formulations, respectively. All results were acceptable and this confirmed that the method is suitable for its intended use in routine quality control and an assay of drugs. [ABSTRACT FROM AUTHOR]

The current work suggests a new, ultrasensitive green functionalized sensor for the determination of anti-inflammatory medication diclofenac sodium (DCF). Alumina (Al 2 O 3 ) and cerium oxide (CeO 2 ) nanoparticles (NPs) have attracted great interest for their use as outstanding and electroactive nanocomposite in potentiometric and sensory research due to their ultrafunctional potential. The formed nanoparticles have been confirmed using various spectroscopic and microscopic techniques. The fennel extract-mediated Al 2 O 3 /CeO 2 nanocomposite (Al 2 O 3 /CeO 2 NCS) modified coated wire membrane sensor developed in this study was used to quantify DCF in bulk and commercial products. Diclofenac sodium was coupled with phosphomolybdic acid (PMA) to generate diclofenac phosphomolybdate (DCF-PM) as an active ion-pair in the existence of polyvinyl chloride (PVC) and o -nitrophenyl octyl ether ( o -NPOE). Clear peaks at 270, and 303 nm with band gaps of 4.59 eV and 4.09 eV were measured using UV-vis spectroscopy of Al 2 O 3 and CeO 2 , respectively. The crystallite sizes of the formed nanoparticles were XRD-determined to be 30.13 ± 8, 17.72 ± 3, and 35.8 ± 0.5 nm for Al 2 O 3 , CeO 2 , and Al 2 O 3 /CeO 2 NCS, respectively. The developed sensor showed excellent response for the measurement and assay of DCF, with a linearity between 1.0 × 10 -9 and 1.0 × 10 -2  mol L -1 . E mV = (57.76) log [DCF] +622.69 was derived. On the other hand, the typical type DCF-PM presented a potentiometric response range of 1.0 × 10 -5 -1.0 × 10 -2  mol L -1 and a regression equation of E mV = (56.97) log [DCF]+367.16. The functionalized sensor that was proposed was successful in determining DCF in its commercial tablets with percent recovery 99.95 ± 0.3. Method validation has been used to improve the suitability of the suggested potentiometric technique, by studying various parameters with respect to the international council harmonization requirements for analytical methodologies., Competing Interests: The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (© 2024 The Authors.)

The new research presents highly conductive polymeric membranes with a large surface area to volume ratio of metal oxide nanoparticles that were used to determine atropine sulfate (AT) in commercial dosage forms. In sensing and biosensing applications, the nanomaterials zinc oxide (ZnONPs) and magnesium oxide (MgONPs) were employed as boosting potential electroactive materials. The electroactive atropine phosphotungstate (AT-PT) was created by combining atropine sulfate and phosphotungstic acid (PTA) and mixing it with polymeric polyvinyl chloride (PVC) with the plasticizer o-nitrophenyl octyl ether (o-NPOE). The modified sensors AT-PT-ZnONPs or AT-PT-MgONPs showed excellent selectivity and sensitivity for the measurements of atropine with a linear concentration range of 6.0 × 10−8 − 1.0 × 10−3 and 8.0 × 10−8 − 1.0 × 10−3 mol L−1 with regression equations of E(mV) = (56 ± 0.5) log [AT] − 294 and E(mV) = (54 ± 0.5) log [AT] − 422 for AT-PT-NPs or AT-PT-MgONPs sensors, respectively. The AT-PT coated wire sensor, on the other hand, showed a Nernstian response at 4.0 × 10−6 − 1.0 × 10−3 mol L−1 and a regression equation E(mV) = (52.1 ± 0.2) log [AT] + 198. The methodology-recommended guidelines were used to validate the suggested modified potentiometric systems against various criteria.

A kinetic spectrophotometric method has been developed for the determination of perindopril erbumine in pure and commercial dosage forms. The method is based on the reaction of drug with potassium permanganate in alkaline medium at room temperature (30 ± 1 °C). The reaction was followed spectrophotometrically by measuring the increase in absorbance with time at 603 nm and the initial rate, fixed time (at 8.0 min) and equilibrium time (at 90.0 min) methods were adopted for constructing the calibration graphs. All the calibration graphs are linear in the concentration range of 5.0–50.0 μg/ml. The limits of detection for initial rate, fixed time and equilibrium time methods were 0.752, 0.882 and 1.091 μg/ml, respectively. The activation parameters such as Ea, ΔH‡, ΔS‡ and ΔG‡ were also determined for the reaction and found to be 60.93 kJ/mol, 56.45 kJ/mol, 74.16 J/K mol and −6.53 kJ/mol, respectively. The variables were optimized and the proposed methods are validated as per ICH guidelines. The method has been further applied to the determination of perindopril erbumine in commercial dosage forms. The analytical results of the proposed methods when compared with those of the reference method show no significant difference in accuracy and precision and have acceptable bias.

Two optimized and validated spectrophotometric methods have been developed for the determination of amiodarone hydrochloride in commercial dosage forms. Method A is based on the reaction of tertiary amino group of the drug with N -bromosuccinimide in methanol–acetone medium resulting in the formation of a yellow colored product, which absorbed maximally at 353 nm. Method B involves the formation of a colored chloroform extractable ion-pair complex of the drug with bromothymol blue at pH 2.32 absorbing maximally at 400 nm. Beer’s law is obeyed in the concentration ranges 50–600 and 2–55 μg mL −1 with molar absorptivity of 1.58 × 10 2 and 1.50 × 10 4 L mol −1 cm −1 for methods A and B, respectively. The regression analysis yields the calibration equations: A = 4.012 × 10 −4 + 1.16 × 10 −3 C and A = 9.612 × 10 −4 + 2.198 × 10 −2 C for methods A and B, respectively. The application of the proposed methods to commercial dosage forms is presented. [ABSTRACT FROM AUTHOR]

An accurate, selective and sensitive spectrofluorimetric method was developed for the determination of citalopram hydrobromide in commercial dosage forms. The method was based on the formation of a fluorescent ion-pair complex between citalopram hydrobromide and eosin Y in the presence of a disodiumhydrogen phosphate/citric acid buffer solution of pH3.4 that was extractable in dichloromethane. The extracted complex showed fluorescence intensity at λem = 554nm after excitation at 259 nm. The calibration curve was linear over at concentrations of 2.0-26.0 μg/mL. Under optimized experimental conditions, the proposed method was validated as per ICH guidelines. The effect of common excipients used as additives was tested and the tolerance limit calculated. The limit of detection for the proposed method was 0.121 μg/mL. The proposed method was successfully applied to the determination of citalopramhydrobromide in commercial dosage forms. The results were compared with the reference RP-HPLC method. [ABSTRACT FROM AUTHOR]

Abstract: Aim of the work: This study aimed to assess serum levels of some adipocytokines (leptin, adiponectin and resistin) and IL-6 in patients with ankylosing spondylitis (AS) to evaluate their relationship to disease activity and functional capacity. Patient and method: Twenty-five AS patients were enrolled. Body mass index (BMI), Bath AS Disease Activity Index (BASDAI), Bath AS Functional Index (BASFI) and acute phase reactants, such as erythrocyte sedimentation rate (ESR) and C-reactive protein (CRP) levels, were assessed. Serum leptin, adiponectin, resistin and interleukin (IL)-6 levels were determined using enzyme-linked immunosorbent assay (ELISA). Results: The mean levels of leptin (9.1±3.9ng/ml), resistin (2.27±1.15ng/ml) and IL-6 (9.2±5.8pg/ml); were significantly elevated in patients with AS compared to the controls (p =0.000, p =0.0028 and p =0.000, respectively). Only serum leptin levels correlated significantly with IL-6 (p =0.004), and both serum leptin and IL-6 levels correlated significantly with BASDAI (p =0.02 and p =0.005, respectively), ESR (p =0.04) and CRP (p =0.01 and p =0.006, respectively) in AS patients. Serum resistin did not correlate with any of the AS disease parameters, whereas, serum adiponectin neither significantly elevated nor correlated with any of these parameters. Conclusion: The associations of significantly increased levels of serum leptin and IL-6 with AS disease activity parameters give clues to their role in the inflammatory process of the disease. Failure to find any correlation between high serum resistin levels and AS disease activity parameters is suggestive of its role in the pathogenesis rather than disease activity. [Copyright &y& Elsevier]

A novel spectrofluorimetric method has been developed for the determination of doxepin hydrochloride in commercial dosage forms. The method is based on the fluorescent ion pair complex formation of the drug with eosin Y in the presence of sodium acetate–acetic acid buffer solution of pH 4.52 which is extractable in dichloromethane. The extracted complex showed fluorescence intensity at λem = 567 nm after excitation at 464 nm. The calibration curve was linear over the working range of 0.1–0.8 µg ml−1. Under the optimized experimental conditions, present method is validated as per International Conference on Harmonization guidelines. The limit of detection for the developed method is 2.95 ng ml−1. The method has been successfully applied to the determination of doxepin hydrochloride in commercial dosage forms. The results are compared with the reference spectrofluorimetric method. [ABSTRACT FROM AUTHOR]

Four simple, rapid and sensitive spectrophotometric methods have been proposed for the determination of enalapril maleate in pharmaceutical formulations. The fi rst method is based on the reaction of carboxylic acid group of enalapril maleate with a mixture of potassium iodate (KIO3) and iodide (KI) to form yellow colored product in aqueous medium at 25 ± 1°C .The reaction is followed spectrophotometrically by measuring the absorbance at 352 nm. The second, third and fourth methods are based on the charge transfer complexation reaction of the drug with p-chloranilic acid (pCA) in 1, 4-dioxan-methanol medium, 2, 3-dichloro 5, 6-dicyano 1, 4-benzoquinone (DDQ) in acetonitrile-1,4 dioxane medium and iodine in acetonitrile-dichloromethane medium. Under optimized experimental conditions, Beer's law is obeyed in the concentration ranges of 2.5-50, 20-560, 5-75 and 10-200 μg mL-1, respectively. All the methods have been applied to the determination of enalapril maleate in pharmaceutical dosage forms. Results of analysis are validated statistically. [ABSTRACT FROM AUTHOR]

A kinetic spectrophotometric method has been developed for the determination of perindopril erbumine in pure and commercial dosage forms. The method is based on the reaction of drug with potassium permanganate in alkaline medium at room temperature (30 ± 1 °C). The reaction was followed spectrophotometrically by measuring the increase in absorbance with time at 603 nm and the initial rate, fixed time (at 8.0 min) and equilibrium time (at 90.0 min) methods were adopted for constructing the calibration graphs. All the calibration graphs are linear in the concentration range of 5.0–50.0 μg/ml. The limits of detection for initial rate, fixed time and equilibrium time methods were 0.752, 0.882 and 1.091 μg/ml, respectively. The activation parameters such as E a , ΔH ‡ , ΔS ‡ and ΔG ‡ were also determined for the reaction and found to be 60.93 kJ/mol, 56.45 kJ/mol, 74.16 J/K mol and −6.53 kJ/mol, respectively. The variables were optimized and the proposed methods are validated as per ICH guidelines. The method has been further applied to the determination of perindopril erbumine in commercial dosage forms. The analytical results of the proposed methods when compared with those of the reference method show no significant difference in accuracy and precision and have acceptable bias. [ABSTRACT FROM AUTHOR]

An accurate, selective and sensitive spectrofluorimetric method was developed for the determination of citalopram hydrobromide in commercial dosage forms. The method was based on the formation of a fluorescent ion-pair complex between citalopram hydrobromide and eosin Y in the presence of a disodium hydrogen phosphate/citric acid buffer solution of pH 3.4 that was extractable in dichloromethane. The extracted complex showed fluorescence intensity at λem = 554 nm after excitation at 259 nm. The calibration curve was linear over at concentrations of 2.0-26.0 µg/mL. Under optimized experimental conditions, the proposed method was validated as per ICH guidelines. The effect of common excipients used as additives was tested and the tolerance limit calculated. The limit of detection for the proposed method was 0.121 μg/mL. The proposed method was successfully applied to the determination of citalopram hydrobromide in commercial dosage forms. The results were compared with the reference RP-HPLC method., (Copyright © 2015 John Wiley & Sons, Ltd.)