scholarly journals Development and Validation of a New RP-HPLC Analytical Method for the Simultaneous Determination of Luliconazole and Clobetasol Propionate in Synthetic Mixture

Author(s):  
Binal Solanki ◽  
Hirak Joshi

Aim: To develop new selective and sensitive reverse-phase high-performance liquid chromatography (RP-HPLC) approach for the quantification of antifungal drug Luliconazole integrate with corticosteroid drug Clobetasol Propionate in a synthetic mixture. Methods: The method was validated to achieve International Conference Harmonization (ICH) requirements. Chromatographic separation was carried out by isocratic technique on a reversed-phase Inertsil C18 column (5 µm, 250mm x 4.6mm i.d with the mixture of Acetonitrile: Water pH adjusted with H3PO4 (60: 40) and UV detection at 264 nm. The compounds were eluted at a flow rate of 1.0 mL/min with an injection volume of 20μL. Results: The calibration curves were linear (r2 > 0.999) over the concentration range 10-200 μg/mLfor Luliconazole and 5-100 μg/mL for Clobetasol Propionate. The average retention times for Luliconazole and Clobetasol Propionate were 3.16 and 6.94 min, respectively. The % RSD   for the proposed method was found to be less than %2. The % recovery was found to between 99.22-99.48% for the developed method. Conclusion: The developed method is simple, rapid, precise, and accurate and hence was successfully applied for the determination of Luliconazole and Clobetasol Propionate in a synthetic mixture.

Author(s):  
Bijithra Cholaraja ◽  
Shanmugasundaram P ◽  
Ragan G ◽  
Sankar Ask ◽  
Sumithra M

ABSTRACTObjective: To development and validation of a reversed-phase high-performance liquid chromatography (RP-HPLC) for the determination of modafinilin bulk and pharmaceutical dosage forms.Methods: A simple, precise, rapid, and accurate RP-HPLC method was developed for the estimation of modafinil in bulk and pharmaceutical dosageforms. Xterra RP 18 (250 mm × 4.6 mm, 5 µ particle size) with a mobile phase consisting of methanol:water 70:30 V/V was used. The flow rate1.0 ml/min and the effluents were monitored at 260 nm. The retention time and recovery time was 12 minutes. The detector response was linear inthe concentration of 10-50 µg/ml. The respective linear regression equation being Y=452.1x+65237. The limit of detection and limit of quantificationwere 4.547 and 1.377 mcg, respectively. The method was validated by determining its accuracy, precision, and system suitability.Result: The objective of the present work is to develop simple, precise, and reliable HPLC method for the analysis of modafinil in bulk andpharmaceutical dosage forms. This is achieved using the most commonly employed Xterra RP 18 (250 mm × 4.6 mm, 5 μ particle size) columndetection at 260 nm. The present method was validated according to ICH guidelines.Conclusion: In this study, a simple, fast and reliable HPLC method was developed and validated for the determination of modafinil in pharmaceuticalformulations.Keywords: Modafinil, Reversed-phase high-performance liquid chromatography, Estimation, ICH guidelines, Tablets. 


Author(s):  
O. S. S. Chandana ◽  
D. Sathis Kumar ◽  
R. Ravichandra Babu

Objective: Our main objective is to develop an accurate and precise RP-HPLC method for the determination of Eprosartan Mesylate and its impurities. Methods: A Develosil ODS UG-5; (150 × 4.6) mm; 5 µm column was used for the Separation of drugs by a mobile phase consisting of Buffer and Acetonitrile mixture in the gradient proportion. The flow rate maintained was 0.8 ml/min and the wavelength used for detection was 235 nm.Results: The linearity was observed in the range of 0.025-50µg/ml of spiked impurities in Eprosartan Mesylate, impurity 1 and impurity 2 with a correlation coefficient of 0.99927, 0.99910 and 0.99934 respectively. The mean percentage recoveries for LOQ, 50%, 80%, 100%, 150% and 200% accuracy were found to be 101.5±1.51, 107.0±1.7, 104.6±0.4, 102.8±0.36, 101.7±0.26 and 101.3±0.15 respectively for impurities in Eprosartan Mesylate, impurity 1 and impurity 2. Linearity, accuracy, precision and robustness parameters for the suggested method were estimated for validation.Conclusion: The developed method is uncomplicated, accurate, sensitive and precise for the determination of related substances in the Eprosartan Mesylate. The satisfying % recoveries and low % RSD Values confirmed the suitability of the developed method for the usual analysis of Eprosartan mesylate in pharmaceuticals.


2012 ◽  
Vol 1 (11) ◽  
pp. 366-369 ◽  
Author(s):  
Kalakonda Sri Nataraj ◽  
Mohammad Badrud Duza ◽  
Kalyani Pragallapati ◽  
Dussa Kiran Kumar

A method for the determination of omeprazole in bulk and capsule dosage form by reverse phase high performance liquid chromatography has been developed. This is a simple, rapid, precise and an accurate method. The method was developed on a Novapak C18, (250 x 4.6 mm, 5µ) column using phosphate buffer (pH 7.4) and acetonitrile in the ratio of 60:40, v/v as a mobile phase which was pumped at a flow rate of 1.0 ml/min and detection was done at 302 nm. The retention time of the drug was found to be 7.71 min. The method was validated for accuracy, precision, linearity, specificity, robustness. The linearity was observed in the range of 20-60 ppm. The results of recovery studies indicated that the method was accurate. Hence the developed method was found to be suitable for the estimation of omeprazole in bulk and capsule dosage forms.DOI: http://dx.doi.org/10.3329/icpj.v1i11.12062 International Current Pharmaceutical Journal 2012, 1(11): 366-369


2020 ◽  
Vol 16 ◽  
Author(s):  
Kemal Hussien Seid ◽  
Tarekegn Berhanu ◽  
Kaleab Asres ◽  
Ayenew Ashenef

Introduction: A reverse-phase high performance liquid chromatography (RP-HPLC) method was developed and validated for the simultaneous analysis of two drugs, levamisole hydrochloride(LH) and oxyclozanide(OX), in co-formulations for veterinary use. Materials and Methods: The new HPLC method was validated per ICH and other guidelines. A C18 column was used with agradient program; eluent A was an equal mixture of methanol and acetonitrile, and eluent B a 25 mM phosphate buffer at pH 7.0 containing 30 mM sodium decanesulfonate andtriethylamine(50:50:1 v/v)then pH adjusted to 7.0 with H3PO4 [51:49 v/v] .The detection wavelength was set at 220 nm.For the final gradient program, the retention times were 8.2(for LH)and 13.6(for OX) minutes respectively at flow rate of 1 ml/min over 20 minute run time. Results: The method wasprecise, specific and robust.The correlation coefficients, R2 were 0.9998 and 0.9999 for LH and OX respectively in the ranges of 5 – 280 µg / mL.The percent y-intercepts and percent residual standard deviations were 1.6%/0.4% and 1.4%/1.0% for LH and OX, respectively. The LOD and LOQ of the method were 0.21 µg / mL and 0.62 µg / mL for LHand 0.06 µg / mL and 0.18 µg / mL for OX. The method has average accuracy of 100.5% for LH and 101.1% for OX when tested on veterinary bolus formulations, and the samples couldbe stored under typical lab conditions for about 7 days without significant degradation. Conclusion: This HPLC method is suitable forassayinglevamisole hydrochloride and oxyclozanide simultaneously from veterinary formulations.


2014 ◽  
Vol 2014 ◽  
pp. 1-7
Author(s):  
Harshal Ashok Pawar ◽  
Pooja Rasiklal Joshi

Satranidazole is a new nitroimidazole derivative with potent antiamoebic action and is available in market in the form of tablet and dry syrup either alone or in combination with Ofloxacin. The present study involves the development of simple, accurate, precise, and reproducible reversed phase high performance liquid chromatography (RP-HPLC) method for determination of Satranidazole from its granular dosage form. Isocratic elution at a flow rate of 1.0 mL/min was employed on BDS Hypersil C18 (250 mm × 4.6 mm, 5 μm) column at 25°C temperature. The mobile phase consists of 0.16% v/v orthophosphoric acid solution, pH 3: acetonitrile in the ratio of 60 : 40 v/v. The UV detection wavelength was 320 nm, and 20 μL sample was injected. The retention time for Satranidazole was about 4.3 minutes. The method was validated for various parameters such as system suitability, precision, recovery, robustness, and ruggedness as per ICH guidelines. The validated RP-HPLC method was found to be specific, linear, precise, and accurate and can be successfully employed for the assay of Satranidazole taste masked granules coated with Eudragit E100 and marketed tablets.


2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.


2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Katso Binang ◽  
David T. Takuwa

Abstract The aim of the study was to develop a rapid, efficient, and cheap chromatographic method for determining four selected antihypertensive active flavonoid compounds in medicinal plants in Botswana. The determination of rutin, quercetin, and kaempferol in selected medicinal plants was conducted in less than 6 min using the developed reverse phase-high performance liquid chromatography (RP-HPLC) method with a 2.7 µm Ascentis C18 express column (150 × 4.60 mm i.d) at 340, 360, and 368 nm detection wavelengths and mobile phase of methanol and 0.068% of formic acid solution in isocratic elution. Validation results showed good selectivity, linearity (r 2 > 0.99), high percentage recoveries (90.2–104.7%), and precision (% RSD < 2) for n = 3, confirming suitability of the method for determination of the investigated flavonoids in Zingiber officinale (ginger). Application of the developed RP-HPLC method was performed in selected medicinal plants (Lippia javanica ) (mosukujane), Myrothanmus flabellious (galalatshwene), and Elephantorrhiza elephantina (mositsana) used to manage hypertension by herbalists in Botswana. M. flabellious a very commonly used plant for managing hypertension was found to contain highest amounts of rutin and myricetin, whereas nothing was detected for E. elephantina.


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