Stability indicating spectrofluorimetric method for determination ofduloxetine hydrochloride in bulk and in dosage form (original) (raw)
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Indian Journal of Pharmaceutical Education and Research, 2014
The object of current work was to study the degradation behavior of duloxetine under different ICH recommended stress condition under reverse phase high performance liquid chromatographic (HPLC) method and to establish a novel, validated stability-indicating reverse phase high performance liquid chromatographic method for the determination of duloxetine in presence of its impurities and forced degradation products in pharmaceutical formulation. The chromatographic separation was achieved on Hypersil, BDS-C8 , (250 mm × 4.6 mm, 5 µM) column with a mobile phase containing a mixture of Acetonitrile : Phosphate buffer pH 3.0 (50:50 v/v). Detection was carried out with UV detector. The retention time was about 3.99 min; the method was validated for linearity, accuracy, precision, specificity, robustness and ruggedness. The described method shows excellent linearity over a range of 8-56 µg/mL for duloxetine. To establish stability indicating capability of the method, drug product was subjected to the stress condition of acid, base, oxidative, hydrolytic, thermal and photolytic degradation. The degradation products were well resolved from duloxetine. The developed method was validated as per ICH guidelines with respect to specificity, linearity, LOD, LOQ, accuracy, precision and robustness.
Journal of Planar Chromatography – Modern TLC, 2009
A simple, selective, precise, and stability-indicating high-performance thin-layer chromatographic (HPTLC) method has been established and validated for analysis of duloxetine hydrochloride in formulations. The compound was resolved on aluminum-backed silica gel 60 F 254 plates with toluene-methanol-10% (v/v) ammonia 3:1.3:0.05 (v/v) as mobile phase. This system was found to give compact spots for duloxetine hydrochloride (R F 0.39 ± 0.02). Densitometric analysis of duloxetine hydrochloride was performed at 231 nm. Regression analysis data for the calibration plots were indicative of good linear relationships between response and concentration over the range 60-480 ng per band. The correlation coefficient was 0.9981. The slope and intercept of the calibration plot were 8.2229 ± 0.22 and 458.93 ± 7.21 respectively. The method was validated for precision and recovery. The limits of detection and quantification were 20 ± 0.51 and 60 ± 1.05 ng per spot, respectively. Duloxetine hydrochloride was subjected to acid, base, peroxide, dry heat, wet heat, and photodegradation (sunlight). In stability tests the drug was susceptible to acidic and basic hydrolysis, oxidation, and photodegradation. Statistical analysis proved the method is repeatable, selective, and accurate for estimation of duloxetine hydrochloride. Because the method could effectively separate the drug from its degradation products, it can be used as a stability-indicating method. For separation and analysis of duloxetine hydrochloride and olanzapine in a synthetic mixture, acetone-methanol-triethylamine 5:3:0.5 (v/v) was used as mobile phase. Spot detection was performed at 240 nm. The R F values were 0.63 ± 0.02 and 0.77 ± 0.02, respectively. The method was validated for linearity, accuracy, and precision. Calibration plots were linear over the ranges 100-800 and 50-400 ng per band, respectively. The method was successfully used for separation and analysis of duloxetine hydrochloride and olanzapine in a synthetic mixture.
2023
A fast, precise, and simple Reverse Phase High-Performance Liquid Chromatographic method (RP-HPLC) has been developed for the determination of Duloxetine Hydrochloride in the pharmaceutical dosage form. The chromatographic separation was done using Eclipse Plus C18 column (250 mm X 4.6 mm, 5 µm particle size) as a stationary phase with a mobile phase comprising of Phosphate Buffer:Acetonitrile: Methanol (50:30:20 v/v/v) adjust pH to 4.9 with dilute acetic acid at a flow rate of 1.0 mL/min., column temperature of 25 ± 1 o C and UV detection at 231nm. The retention time of Duloxetine Hydrochloride was 11.03 minutes. The linearity was found to be in the range of 12-60 µg/mL with a correlation coefficient of 0.9997. The stated method was validated as per ICH Q2 (R1) guidelines and can be effectively applied for the determination of Duloxetine Hydrochloride in marketed formulations.
Advanced Analytical and Bioanalytical Estimation of Duloxetine Hydrochloride – An Overview
2020
Duloxetine HCl is a drug for the treatment of neuropathic pain associated with peripheral neuropathy especially diabetic polyneuropathy for which it is first line, and as an add-on treatment in stress urinary incontinence instead of surgery also indicated for the management of fibromyalgia. The review describes different procedures for the analysis of Duloxetine HCL as a single drug or in combinations available in the currently available literature in analytical and bioanalytical techniques. The analytical methods described here are explained in Spectroscopic and Chromatographic methods. Advance analytical techniques like HPLC, HPTLC, UFLC, UPLC and LC MS/MS were used to estimate Duloxetine HCl in pure, dosage forms and in rat/human plasma. This paper certainly helpful for the researchers engaged in method development and validation of Duloxetine HCl.
DULOXETINE HYDROCHLORIDE METHOD DEVELOPMENT USING OFFICIAL DISSOLUTION MEDIA
Aim/background: A simple, rapid, precise and economical spectrophotometric method has been developed for the quantitative estimation of Duloxetine Hydrochloride in pharmaceutical formulation. Materials and Methods: The simple, precise, economical and rapid method was developed and validated for the estimation of Duloxetine Hydrochloride using pH 6.8 phosphate buffer as a solvent. The stock solution of Duloxetine Hydrochloride was prepared and subsequent suitable dilution was prepared in pH 6.8 phosphate buffer to obtained standard curve. The standard solution of Duloxetine Hydrochloride shows absorption maxima at 289 nm. Results: The drug obeyed beer lambert's law in the concentration range of 10-50µg/ mL with regression 0.9998 at 289nm. The overall % recovery was found to be 100.674% which reflects that the method is free from interference of the impurities and other additives used in formulation. The low value of % RSD was indicative of accuracy and reproducibility of the method. The %RSD for interday and intraday precision was found to be 1.246 and 0.742, respectively which is <2% hence proved that method is precise. Conclusions: The results of analysis have been validated as per ICH guidelines. The developed method can be adopted in routine analysis of Duloxetine HCL in Capsule dosage form as well bulk dosage form.
E-Journal of Chemistry, 2010
A new, simple and sensitive spectrophotometric method in ultraviolet region has been developed for the determination of duloxetine hydrochloride in bulk and in pharmaceutical formulations. Duloxetine hydrochloride exhibits absorption maxima at 288 nm with apparent molar absorptivity of 0.97x10 4 L/mol.cm in 0.1 N HCL. Beer's law was found to be obeyed in the concentration range of 5-30 µg/mL. The method is accurate, precise and economical. The proposed method has been applied successfully for the analysis of the drug in pure and in its capsule dosage forms. In this method, there is no interference from any common pharmaceutical additives and diluents. Results of the analysis were validated statistically and by recovery studies.
An analytical method has been developed and validated for estimation of duloxetine hydrochlorideinpharmaceutical dosage form (tablet) by RP-HPLC.The chromatography was carried out isocraticallyby a BDS Hypersil C 18 column (250 x 4.6 mm, 5 µm) with a mixture of methanol:buffer (pentane-1sulfonic acid sodium salt) in the ratio of 65:35 v/v as mobile phase. Detection was carried out using a UV detector at 235 nm wavelength. The drug was well resolved on the stationary phase and the retention time was found to be 6.8 minutes. System suitability parameters like, tailing factor 1.79, theoretical plate 5393.002 and injection precision 0.1084% for n=6 were calculated. The developed method was found to be accurate, precise and linear. The calibration curve was found to be linear (R 2 =0.9996) in the concentration range of 20-70 µg/ml for duloxetine hydrochloride.
Luminescence, 2014
ABSTRACTA new, sensitive and selective spectrofluorimetric method has been developed for the determination of duloxetine (DLX) in capsule and spiked human plasma. DLX, as a secondary amine compound, reacts with 7‐chloro‐4‐nitrobenzofurazon (NBD‐Cl), a highly sensitive fluorogenic and chromogenic reagent used in many investigations. The method is based on the reaction between the drug and NBD‐Cl in borate buffer at pH 8.5 to yield a highly fluorescent derivative that is measured at 523 nm after excitation at 478 nm. The fluorescence intensity was directly proportional to the concentration over the range 50–250 ng/mL. The reaction product was also measured spectrophotometrically. The relation between the absorbance at 478 nm and the concentration is rectilinear over the range 1.0–12.0 µg/mL. The methods were successfully applied for the determination of this drug in pharmaceutical dosage form. The spectrofluorimetric method was also successfully applied to the determination of duloxet...
Estimation of duloxetine hydrochloride in pharmaceutical formulations by RP-HPLC method
Indian Journal of Pharmaceutical Sciences, 2008
Patel, et al.: RP-HPLC estimation of duloxetine hydrochloride Simple, specifi c, accurate and precise method, namely, reverse phase high performance liquid chromatography was developed for estimation of duloxetine HCl in pharmaceutical formulations. For the high performance liquid chromatography method, Phenomenox C-18, 5 µm column consisting of 250×4.6 mm i.d. in isocratic mode, with mobile phase containing 0.01M 5.5 pH phosphate buffer: acetonitrile (60:40 v/v) and fi nal pH adjust to 5.5±0.02 with phosphoric acid was used. The fl ow rate was 1.2 ml/min and effl uent was monitored at 231 nm. The retention time was 5.61 min. The method was validated in terms of linearity, accuracy and precision. The linearity curve was found to be linear over 0.25-4 µg/ml. The limit of detection and limit of quantifi cation were found to be 0.10 and 0.25 µg/ml respectively. The proposed method was successfully used to determine the drug content of marketed formulations.