19 research outputs found

    Estimation of Delafloxacin Using Derivative Spectrophotometry and Area Under Curve in Bulk Material and in Laboratory Mixture

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    Simple, specific, rapid and accurate UV-spectrophotometric methods have been developed using a solvent acetonitrile (50 %) to determine delafloxacin in bulk material and in laboratory mixture. “Method A” is zero order derivative UV- spectrophotometry using absorbance, “Method B” is zero order derivative UV-spectrophotometry using Area Under Curve (AUC) technique, “Method C” is first order derivative UV-spectrophotometry using amplitude, “Method D” is First Order Derivative UV-spectrophotometry- AUC,“Method E” is Second Order Derivative UV-spectrophotometry using amplitude and “Method F” is second order derivative UV- spectrophotometry using (AUC) technique. The developed methods have shown excellent results in terms of linearity and range, accuracy, precision and Limit of Detection (LOD) and Limit of Quantification (LOQ). In all Methods, delafloxacin obeyed linearity in the concentration range of 2 - 12 μg/mL with (r2 > 0.999). All these methods were applied for estimation of delafloxacin in laboratory mixture. All the above mentioned methods were validated considering linearity and range, accuracy, precision, ruggedness and sensitivity

    Pharmaceutical Analysis of Eptifibatide via Simple, Rapid, Economical UV-Spectrophotometric Methods

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    Eptifibatide is an antiplatelet drug of the glycoprotein IIb/IIIa inhibitor class. Pharmaceutically it is applied to reduce the risk of acute cardiac ischemic events. The present work reveals two simple, rapid and economical UuV-Spectrophotometric methods for pharmaceutical analysis of Eeptifibatide bulk and in parenteral formulation. The ‘Method I’ is based on the Zero Order Spectrophotometric determination of drug at its wavelength maximum 218.20 nm and ‘Method II’ employed First Order Derivative - Aarea Uunder Curve (AUauC) technique in which the area has been integrated between two wavelengths 220.20 to 237.20 nm. The drug obeyed linearity in the concentration range of 3 - 18 μg/mLl with coefficient of correlation; greater than 0.999 in both methods. The amounts of drug determined by both methods are in conformity with label claim. These methods are validated for accuracy, precision and ruggedness with % RSD value less than 2.0

    Analytical Review on Raloxifene -An Estrogen Receptor Modulator in Different Pharmaceutical Formulations and Biological Fluids

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    Raloxifene (RLX) is an oral selective estrogen receptor modulator (SERM). It is showing estrogenic action on bone and anti-estrogenic action on uterus and breast. An extensive literature has been published for analysis of RLX in different pharmaceutical formulations. This review article endeavor to provide the detail account on analytical methods for RLX and also validation details for its readers. It further helps to avoid costly chemicals and time consuming exercises for further investigation of RLX

    Development and Validation of UV Spectrophotometric Method for Simultaneous Estimation of Quinfamide and Mebendazole in in-house Pharmaceutical Formulation

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    The present work described the development of two simple, accurate, rapid, cost effective and reproducible UV-Spectrophotometric methods for the simultaneous estimation of Quinfamide and Mebendazole in bulk and in laboratory mixture using 0.01M methanolic HCl as a solvent. The absorption maximum for Quinfamide and Mebendazole were found to be at 260.00 nm and 232.40 nm respectively. Beer’s - lamberts was followed in concentration ranges of 1 - 6 μg/mL for Quinfamide and 2- 12 μg/mL for Mebendazole. The percentage recovery of Quinfamide and mebendazole ranged from 98.48 to 99.08 and 98.83 to 99.62 (Method I); from 98.14 to 98.93 and 99.16 to 99.35 (Method II) for Quinfamide and Mebendazole. The established methods were sensible for simultaneous quantitative determination of both these drugs in fixed dose combinations. Validation of both these methods was performed as per ICH guidelines. The developed methods can routinely be used for estimation of both these drugs in their combined dosage form

    An Insight on Analytical Profile on Bisoprolol Fumarate – A Selective Beta-1 Adrenoreceptor Blocker

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    BF is Beta-adreno receptor antagonist and used as an AntiHypertensive Drug. BF gives the blocking action on β1-adrenergic receptors in the heart and vascular smooth muscle. The present review compiles the various approaches implemented for quantification of BF in bulk drug, pharmaceutical matrix and biological fluid. This review represents more than 50 analytical methods which include capillary electrophoresis, HPLC, HPTLC, UV-Spectroscopy, UPLC, impurity profiling and electrochemical methods implemented for estimation of BF as a single component as well as in multicomponent

    Design of experiment avenue for development and validation of RP-HPLC-PDA method for determination of apremilast in bulk and in in-house tablet formulation

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    Abstract Background Apremilast is phosphodiesterase-4 and an immunomodulating agent used for treatment of refractory psoriatic arthritis. Methods The reversed-phase high-performance liquid-chromatography method for analysis of apremilast was developed and validated as per ICH guidelines. The separation of apremilast was performed on PrincetonSPHERE Ultima C18 column (250 mm × 4.6 mm, i.d., 5 μm particle size) with photodiode array detection carried out at 231 nm. A Box–Behnken design with response surface methodology was executed out for optimization of chromatographic conditions of reversed-phase high-performance liquid-chromatography for finished desired chromatographic separation of apremilast from its formulation with less number of experimental trials. Three independent factors, namely methanol composition in the mobile phase, pH of an aqueous phase, and flow rate, were used to construct a mathematical model and study the effects of these independent factors on responses such as retention time, theoretical plates, and tailing factor. Results Optimized experimental conditions for proposed work consists of methanol and water, pH 3.50 adjusted with ortho-phosphoric acid (70:30 % v/v) as a mobile phase at a flow rate 1 ml/min with a retention time was found to be 5.15 min. Accuracy study was completed at three different levels and was found in the range of 99.44–101.49%. Conclusion The 3D response surface graphs revealed that the methanol composition and pH of an aqueous phase were both most stringent factors affecting the responses. Thus, a new, precise, and accurate HPLC method was developed and validated and can be used for regular analysis of apremilast

    Novel HPTLC and UV-AUC analyses: For simple, economical, and rapid determination of Zileuton racemate

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    Novel, simple, rapid and reliable High-Performance Thin-Layer Chromatographic (HPTLC) and UV-spectroscopic area under curve (UV-AUC) methods were developed and validated for the analysis of zileuton racemate in bulk and in in-house tablet formulation. HPTLC quantitation of zileuton was done by UV detection at 260 nm and analysis was performed on (20 × 10 cm) aluminium sheets precoated with silica gel 60-F254 (E. Merck) as stationary phase and toluene–methanol–glacial acetic acid (3.5:1.5:0.1 v/v) as mobile phase. Quantitation by HPTLC method was performed over the concentration range of 200–1200 ng/band. The HPTLC method resulted into a compact and well resolved band for zileuton at retention factor (Rf) of 0.51 ± 0.02. Linear regression analysis data for calibration of HPTLC method represented a good linear relationship with regression coefficient; r2 = 0.997. UV-AUC method was developed using sodium lauryl sulphate (0.05 M) as a hydrotropic agent to enhance water solubility and area was determined at a wavelength range in between 248.40 and 271.0 nm. Correlation coefficient for UV-AUC analysis was found to be r2 = 0.999. The developed UV-AUC method depicted a fine linear relationship for zileuton racemate in a concentration range of 2–12 μg/mL. Both the developed methods were validated for precision, robustness, ruggedness, accuracy, sensitivity as per guidelines laid by the International Conference on Harmonisation (ICH). Statistical analysis proved that the developed methods were precise, robust, sensitive and accurate and can be used effectively for the analysis of zileuton in bulk and pharmaceutical formulations

    Development and validation of simple RP-HPLC-PDA analytical protocol for zileuton assisted with Design of Experiments for robustness determination

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    A simple, rapid, sensitive, robust, stability-indicating RP-HPLC-PDA analytical protocol was developed and validated for the analysis of zileuton racemate in bulk and in tablet formulation. Development of method and resolution of degradation products from forced; hydrolytic (acidic, basic, neutral), oxidative, photolytic (acidic, basic, neutral, solid state) and thermal (dry heat) degradation was achieved on a LC – GC Qualisil BDS C18 column (250 mm × 4.6 mm × 5 μm) by isocratic mode at ambient temperature, employing a mobile phase methanol and (0.2%, v/v) orthophosphoric acid in ratio of (80:20, v/v) at a flow rate of 1.0 mL min−1 and detection at 260 nm. ‘Design of Experiments’ (DOE) employing ‘Central Composite Design’ (CCD) and ‘Response Surface Methodology’ (RSM) were applied as an advancement to traditional ‘One Variable at Time’ (OVAT) approach to evaluate the effects of variations in selected factors (methanol content, flow rate, concentration of orthophosphoric acid) as graphical interpretation for robustness and statistical interpretation was achieved with Multiple Linear Regression (MLR) and ANOVA. The method succeeded over the validation parameters: linearity, precision, accuracy, limit of detection and limit of quantitation, and robustness. The method was applied effectively for analysis of in-house zileuton tablets

    RP-HPTLC method for determination of Voriconazole in bulk and in cream formulation

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    Voriconazole is used as an antifungal agent. A new rapid, simple, economical and environmental friendly Reversed -Phase High-Performance Thin-Layer Chromatography (RP-HPTLC) has been developed and validated for quantitative determination of voriconazole in bulk and in cream formulation. RP-HPTLC separation was performed on aluminium plates precoated with silica gel 60RP-18F-254S as the stationary phase using Acetonitrile: Water (60:40% v/v) as mobile phase. Quantification was achieved by densitometric analysis at 257 nm over the concentration range of 200–1200 ng/band. The method was found to give compact and well resolved band for Voriconazole at Retention factor (Rf) 0.48 ± 0.02. The linear regression analysis data for calibration graph showed good linear relationship with r2 = 0.999. The method was validated for precision, recovery, robustness, ruggedness and sensitivity as per International conference on Harmonization (ICH) guidelines. The Limit of Detection (LOD) and Limit of Quantification (LOQ) were found to be 19.99 ng and 60.60 ng, respectively. The proposed developed RP-HPTLC method can be applied for identification and quantitative determination of Voriconazole in bulk and in cream formulation

    Development and validation of a stability indicating RP-TLC/densitometric method for determination of Loratadine in bulk and in tablets

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    A new rapid, economical and environmentally friendly Reversed-Phase Thin-Layer chromatography (RP-TLC)/densitometry has been developed and validated for quantitative determination of Loratadine (LOR) in bulk and in tablets. RP-TLC separation was achieved on aluminium plates precoated with silica gel 60RP-18F 254S as the stationary phase using methanol:acetonitrile (90:10% v/v) as mobile phase. Quantitation was performed at 247 nm over the concentration range of 200–1200 ng/band. The method was found to give compact and well resolved band for LOR at retention factor (Rf) 0.58 ± 0.02. The linear regression analysis data for calibration graph showed good linear relationship with r2 = 0.998. The method was validated for recovery, precision, robustness, ruggedness and sensitivity as per International conference on Harmonisation (ICH) guidelines. The minimum detectable amount and limit of quantitation were found to be 19.40 ng and 61.51 ng, respectively. LOR was subjected to hydrolysis in acid, alkali, oxidation, photo-degradation and neutral condition. The drug demonstrated degradation under acid and alkali conditions. Statistical analysis proves that the method is sensitive, selective, precise and accurate for the estimation of LOR. The proposed developed RP-TLC/densitometry method can be applied for identification and quantitative determination of LOR in bulk drug and pharmaceutical dosage forms
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