Spectrophotometric Determination of Isoxsuprine Hydrochloride as Base Form in Pharmaceutical Formulation through Charge Transfer Complexation

Two simple and selective spectrophotometric methods are described for the determination of isoxsuprine hydrochloride (ISX·HCl) as base form in bulk drug and in injections and tablets. The methods are based on the molecular charge-transfer complexation of ISX base (ISX) with either p-chloranilic acid (PCA) or 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ). The intense colored radical anions formed on dissociation, are quantitated at 520 nm (PCA method) or 600 nm (DDQ method). The optimum assay conditions were optimized. Beer\u27s law is obeyed in the concentration ranges 5.28 × 10–5 to 42.2 × 10–5 mol dm–3 in PCA method and 0.79 × 10–5 to 10.6 × 10–5 mol dm–3 in DDQ method, with respective molar absorptivity values of 1.32 × 103 and 6.55 × 103 dm3 mol–1 cm–1. The reaction stoichiometry in both methods was evaluated by either Job’s method or limiting logarithmic method and was found to be 1:1 (ISX: PCA, ISX: DDQ). Developed methods were validated according to ICH guidelines and found to be accurate and precise

Spectrophotometric Determination of Isoxsuprine Hydrochloride as Base Form in Pharmaceutical Formulation through Charge Transfer Complexation

Two simple and selective spectrophotometric methods are described for the determination of isoxsuprine hydrochloride (ISX·HCl) as base form in bulk drug and in injections and tablets. The methods are based on the molecular charge-transfer complexation of ISX base (ISX) with either p-chloranilic acid (PCA) or 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ). The intense colored radical anions formed on dissociation, are quantitated at 520 nm (PCA method) or 600 nm (DDQ method). The optimum assay conditions were optimized. Beer\u27s law is obeyed in the concentration ranges 5.28 × 10–5 to 42.2 × 10–5 mol dm–3 in PCA method and 0.79 × 10–5 to 10.6 × 10–5 mol dm–3 in DDQ method, with respective molar absorptivity values of 1.32 × 103 and 6.55 × 103 dm3 mol–1 cm–1. The reaction stoichiometry in both methods was evaluated by either Job’s method or limiting logarithmic method and was found to be 1:1 (ISX: PCA, ISX: DDQ). Developed methods were validated according to ICH guidelines and found to be accurate and precise

Extractive Spectrophotometric Determination of Quetiapine Fumarate in Pharmaceuticals and Spiked Human Urine

A simple, sensitive and selective extractive spectrophotometric method for the determination of quetiapine fumarate (QTF) in bulk drug, tablets and spiked human urine sample is described. The method is based on the formation of a chloroform extractable yellow ion-pair complex between basic nitrogen of the drug (QTF) and the dye quinoline yellow (QY) in acetate-hydrochloride buffer (pH 2.56) medium. The formed ion-pair complex exhibited an absorption maximum at 420 nm. Beer’s law is obeyed over the concentration range 2.5–25 µg mL–1 with an apparent molar absorptivity value of 2.02 × 104 L mol–1 cm–1. The Sandell sensitivity, limits of detection (LOD) and quantification values are also reported. The composition of the ion-pair was established by Job’s continuous variations method and it was found to be 1:1 (QTF:QY). The proposed method was successfully applied for the determination of QTF in bulk drug, tablets and spiked human urine without any interference. (doi: 10.5562/cca1770

Optimized and validated spectrophotometric methods for the determination of hydroxyzine hydrochloride in pharmaceuticals and urine using iodine and picric acid

Two simple, rapid, cost-effective and sensitive spectrophotometric procedures are proposed for the determination of hydroxyzine dihydrochloride (HDH) in pharmaceuticals and in spiked human urine. The methods are based on the charge transfer complexation reaction of the drug with either iodine (I2) as a σ-acceptor (method A) in dichloromethane or picric acid (PA) as a π-acceptor (method B) in chloroform. The coloured products exhibit absorption maxima at 380 and 400 nm for I2 and PA, respectively. The Beer Law was obeyed over the concentration ranges of 1.25-15 and 3.75-45 μg mL-1 for method A and method B, respectively. The molar absorptivity values, Sandell sensitivities, limits of detection (LOD) and quantification (LOQ) are reported. The accuracy and precision of the methods were evaluated on intra-day and inter-day basis. The proposed methods were successfully applied for the determination of HDH in tablets and spiked human urine

Titrimetric and Spectrophotometric Assay of Oxcarbazepine in Pharmaceuticals Using N-Bromosuccinimide and Bromopyrogallol Red

Titrimetric and spectrophotometric methods are described for the determination of oxcarbazepine (OXC) in bulk drug and in tablets. The methods use N-bromosuccinimide (NBS) and bromopyrogallol red (BPR) as reagents. In titrimetry (method A), an acidified solution of OXC is titrated directly with NBS using methyl orange as indicator. Spectrophotometry (method B) involves the addition of known excess of NBS to an acidified solution of OXC followed by the determination of the unreacted NBS by reacting with BPR and measuring the absorbance of the unreacted dye at 460 nm. Titrimetry allows the determination of 6–18 mg of OXC and follows a reaction stoichiometry of 1 : 1 (OXC : NBS), whereas spectrophotometry is applicable over the concentration range of 0.8–8.0 μg mL−1. Method B with a calculated molar absorptivity of 2.52 × 104 L mol−1 cm−1 is the most sensitive spectrophotometric method ever developed for OXC. The optical characteristics such as limits of detection (LOD), quantification (LOQ), and Sandell's sensitivity values are also reported for the spectrophotometric method. The accuracy and precision of the methods were studied on intraday and interday basis. The methods described could usefully be applied to routine quality control of tablets containing OXC. No interference was observed from common pharmaceutical adjuvants. Statistical comparison of the results with a reference method shows an excellent agreement and indicates no significant difference in accuracy and precision. The reliability of the methods was further ascertained by recovery studies in standard addition procedure

Sensitive and selective spectrophotometric determination of pantoprazole sodium in pharmaceuticals using permanganate

A simple visible spectrophotometric method is described for the determination of pantoprazole sodium sesquihydrate (PSS). The method is based on the formation of a brown colored product on treating PSS with permanganate in neutral medium, the absorbance being measured at 350 nm. The experimental conditions for the assay were optimized. The absorbance is found to increase linearly with the concentration of PSS and the calibration graph is linear in the range of 2.5-40.0 μg ml-1 with a linear regression coefficient of 0.998. The calculated molar absorptivity value is 1.27x104 l mol-1 cm-1 and the corresponding Sandel sensitivity is 0.0341 µg cm-2. The limits of detection (LOD) and quantification (LOQ) are calculated to be 0.49 and 1.47 µg ml-1, respectively. Intra-day and inter-day accuracy expressed as relative error were better than 2.0% and the corresponding precision (RSD) was less than 2.5 %. The developed and validated method was applied to the determination of the active ingredient in a tablet dosage form and the results obtained agreed well with those of the reference method. The accuracy and reliability of the method were ascertained by performing recovery experiments via standard-addition procedure

SIMPLE AND SENSITIVE SPECTROPHOTO¬METRIC ASSAY OF OFLOXACIN IN PHARMACEUTICALS BASED ON ION-PAIR REACTION

Two simple, sensitive, economical and extraction-free spectrophotometric methods have been developed for the determination of ofloxacin (OFX) in pure form and in tablets. The methods are based on the interaction of OFX with two sulphonphthalein dyes, namely, bromothymol blue (method A) and bromophenol blue (method B) in dichloromethane medium to form stable, yellow-colored ion–pair complexes peaking at 410 nm. Under the optimum conditions, OFX could be assayed in the concentration ranges 1.25-20 and 1.0-16 µg mL-1 OFX by methods A and B, respectively, with correlation coefficient of 0.999 in both methods. The apparent molar absorptivity values are calculated to be 1.74104 and 2.18104, L moL-1 cm-1, for method A and B, respectively, with corres¬pond¬ing Sandell sensitivity values of 0.021 and 0.017 µg cm-2. The limits of detec¬tion (LOD) and quantification (LOQ) are also reported. The stoichiometry of the reaction was found to be 1:1 in both cases and the conditional stability cons¬tants (Kf) of the complexes have also been reported. The intra-day and inter-day variation was assessed. The methods were applied to determine OFX from marked tablet formulations. Statistical analysis proved that the proposed methods were both accurate and precise

Sensitive and Selective Extractive Spectrophotometric Method for the Determination of Hydroxyzine Dihydrochloride in Pharmaceuticals 233 Sensitive and Selective Extractive Spectrophotometric Method for the Determination of Hydroxyzine Dihydrochloride in P

Abstract. Hydroxyzine dihydrochloride (HDH), a piperazine H 1 -receptor antagonist and antihistamine, is a rapid acting anxiolytic used principally as an anti-emetic. A sensitive, selective, and precise and accurate spectrophotometric method based on the formation of an ion-pair with orange II (ORG II) as ion-pair complexing agent was developed and validated for the determination of HDH in pharmaceuticals. The chloroform-extractable ion-pair complex exhibited an absorption maximum at 480 nm. Optimization of different experimental conditions is described. Beer's law is obeyed in the range of 1.5-15 µg mL -1 with an apparent molar absorptivity value of 2.07 × 10 4 L mol -1 cm -1 and Sandell's sensitivity value of 0.0216 µg cm -2 . The limit of detection (LOD) and limit of quantification (LOQ) are 0.14 and 0.41 µg mL -1 , respectively. A Job's plot of absorbance versus molar ratio of HDH to ORG II indicated (1:2) stoichiometric ratio. Within-and between-day relative standard deviations at three different concentration levels were < 3%. The developed method was successfully applied to commercial tablets. The results obtained were in good agreement with those obtained using the official method. No interference was encountered from co-formulated substances. Recoveries were 96-109 %. Keywords: Spectrophotometry, hydroxyzine, orange II, pharmaceuticals. Resumen. El dihidrocloruro de hidroxicina (HDH), una piperazina antagonista del receptor H 1 y un antihistamínico, es un ansiolítico de acción rápida usado principalmente como anti-emético. Se desarrolló y validó un método espectrofotométrico sensible, selectivo, preciso y exacto basado en la formación de un par iónico con naranja II (ORG II) como un agente complejante para la determinación de HDH en productos farmacéuticos. El par iónico extraído en cloroformo exhibió un máximo de absorción a 480 nm. Se describió la optimización de las diferentes condiciones experimentales. La ley de Beer se obedeció en el intervalo de 1.5-15 µg mL -1 con un valor de absortividad molar aparente de 2.07 × 10 4 L mol -1 cm -1 y un valor de sensibilidad de Sandell de 0.0216 µg cm -2 . El límite de detección (LD) y el límite de cuantificación (LC) son 0.14 y 0.41 µg mL -1 , respectivamente. Una gráfica de Job de absorbancia versus relación molar de HDH y ORG II indicó una relación estequiométrica (1:2). Las desviaciones estándar relativas dentro y entre días, a tres diferentes niveles de concentración, fueron < 3%. El método desarrollado fue aplicado exitosamente a tabletas comerciales. Los resultados obtenidos estuvieron en buena concordancia con los obtenidos con el método oficial. No se encontró ninguna interferencia de parte de las sustancias de la formulación. Las recuperaciones fueron de 96-109 %

Titrimetric and spectrophotometric determination of doxycycline hyclate using bromate-bromide, methyl orange and indigo carmine

One titrimetric and two indirect spectrophotometric methods are described for the determination of doxycycline hyclate (DCH) in bulk drug and in its formulations. The methods use bromate-bromide, methyl orange and indigo carmine as reagents. In titrimetry (method A), DCH is treated with a known excess of bromate- -bromide mixture in acid medium and the residual bromine is back titrated iodometrically after the reaction between DCH and in situ bromine is ensured to be complete. In spectrophotometric methods, the excess of bromine is estimated by treating with a fixed amount of either methyl orange (method B) or indigo carmine (method C) and measuring the change in absorbance either at 520 or 610 nm. Titrimetric method is applicable over 1-8 mg range and the calculations are based on a 1:2 (DCH:bromate) stoichiometric ratio. In spectrophotometry, the calibration graphs were found to be linear over 0.25-1.25 and 1.0-5.0 μg mL-1 for method B and C, respectively, with corresponding molar absorptivity values of 2.62×105 and 6.97×104 L mol-1 cm-1. The accuracy and precision of the assays were determined by computing the intra-day and inter-day variations at three different levels of DCH