Application of Validated RP-HPLC Method for the Determination of Armodafinil in Bulk and Formulation (original) (raw)
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The main objective of present study was to develop a RP-HPLC method for estimation of Armodafinil in pharmaceutical dosage forms and characterization of its base hydrolytic product. The method was developed for Armodafinil estimation and base hydrolytic products were characterized. The separation was carried out on C 18 column by using mobile phase as mixture of water and methanol (45:55%v/v). Eluents were detected at 220nm at 1ml/min. Stress studies were performed with milder conditions followed by stronger conditions so as to get sufficient degradation around 20%. A total of five degradation products were detected and separated from analyte. The linearity of the proposed method was investigated in the range of 20-120µg/ml for Armodafinil. The detection limit and quantification limit was found to be 0.01183µg/ml and 0.035µg/ml respectively. The precision % RSD was found to be less than 2% and the recovery was between 98-102%. Armodafinil was found to be more sensitive to the base hydrolysis and yielded its carboxylic acid as degradant. The developed method was stability indicating assay, suitable to quantify Armodafinil in presence of possible degradants. The drug was sensitive to acid, base & photolytic stress and resistant to thermal & oxidation.
A reverse phase high performance liquid chromatography (RP HPLC) method was developed and validated for the simultaneous estimation of atenolol and chlorthalidone in marketed formulation. The determination was carried out on an Xterra RP8 (150 x 4.6 mm, 5 µm) column using a mobile phase of potassium dihydrogen phosphate buffer solution: methanol (50:50v/v, pH 3.6) with flow rate 0.5ml/min (UVdetection at 240 nm). The retention time for atenolol was 3.2 min and for chlorthalidone 5.0 min. Atenolol and chlorthalidone showed a linear response in the concentration range of 50-150 µg/ml. The correlation coefficient (' r ' value) for atenolol and chlorthalidone was 0.9996. The developed method was validated with regard to linearity, accuracy, precision, selectivity and robustness and the method was found to be precise, accurate, linear and specific. The method was validated as per ICH guidelines. The RSD for intra-day and inter-day precision were found to be less than 2 %. The percentage recoveries obtained for atenolol and chlorthalidone ranges from 100.54-103.32% and 98.03-102.77% respectively which was in good agreement with the labeled amount in the pharmaceutical formulations.
E-journal of Chemistry, 2011
A simple, fast, precise, selective and accurate RP-HPLC method was developed and validated for the simultaneous determination of atenolol and indapamide from bulk and formulations. Chromatographic separation was achieved isocratically on a Waters C18 column (250×4.6 mm, 5 µ particle size) using a mobile phase, methanol and water (adjusted to pH 2.7 with 1% orthophosphoric acid) in the ratio of 80:20. The flow rate was 1 mL/min and effluent was detected at 230 nm. The retention time of atenolol and indapamide were 1.766 min and 3.407 min. respectively. Linearity was observed in the concentration range of 12.5-150 µg/mL for atenolol and 0.625-7.5 µg/mL for indapamide. Percent recoveries obtained for both the drugs were 99.74-100.06% and 98.65-99.98%, respectively. The method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method developed can be used for the routine analysis of atenolol and indapamide from their combined dosage form.
RP-HPLC method development for the determination of Atenololrelated substance in bulk drug
2010
A simple Reverse phase HPLC method has been developed for the quantitative estimation of Atenolol Related substance in pure drug. The quantification was carried out using stainless steel column C18 125 mm x 4.0 mm, 5 μm BDS Hypersil in Isocratic mode with mobile phase containing 1.0 g of Octane-1-Sulphonic acid sodium salt and 0.4 g of Tetra – n - butyl ammonium hydrogen Sulphate in a mixture of 20 volumes of Tetrahydrofuran, 180 volumes of methanol and 800 volumes of 3.4 g/L solution of Potassium dihydrogen phosphate and pH adjusted to 3 ± 0.2 using dilute ortho-phosphoric acid. The method was linear in the range of 1.6-3.2 μg /ml. The proposed method was found to be simple, precise, accurate, and reproducible for the estimation of Atenolol Related substance.
International Journal of Pharmacy and Pharmaceutical Sciences, 2011
The aim of present work was to validate the high performance liquid chromatographic method for the analysis of enalapril maleate in pharmaceutical formulation. The method valdation of enalapril maleate was performed by using Hypersil MOS, 5μ (250 mm x 4.6 mm) as stationary phase with mobile phase consists of buffer solution and Acetonitrile (40:60) at flow rate of 1.5 ml/min. The column temperature and wavelength were monitored at 65 0
INTERNATIONAL JOURNAL OF PHARMACEUTICAL QUALITY ASSURANCE, 2020
The new stability-indicating high performance liquid chromatography (HPLC) method has been developed and validated with different parameters for atenolol (ATE) and nifedipine (NIFE) in the combined dosage form. The chromatographic conditions were optimized using a mobile phase of MeOH:OPA (70:30) with a flow rate of 0.7 mL/min. Column (C18) of 4.6 × 250 mm dimension was used as a stationary phase; the particle size capacity of the column was 5 μm. The detection was carried out at 233 nm. The method was validated according to ICH guidelines for linearity, precision, repeatability, the limit of detection (LoD), and limit of quantitation (LoQ). The response was found to be linear in the concentration range of 20 to 100 mcg/mL for ATE and 1 to 5 mcg/mL for NIFE. The developed method shows the minimum quantity of drugs to be identified (LoD) and minimum drug to be quantified (LoQ). The LoD and LoQ were found to be 0.1415 and 0.4289, respectively, for ATE, and 0.1834 and 0.5558, respectiv...
Patients diagnosed with hypertension are prescribed an large number of medications for appropriate therapy, increasing risk of side effects or drug interactions. Enalapril, ACE inhibitor is commonly used as a drug of choice for the treatment of hypertension. On the other hand, NSAIDs are generally used for the treatment of pain, fever and inflammation, particularly in arthritis. A simple, efficient, economical and least time consuming isocratic method for the simultaneous determination of enalapril (ENP) and non-steroidal anti-inflammatory drugs (flurbiprofen, diclofenac sodium, ibuprofen and mefanamic) in bulk, pharmaceutical formulations and human serum using high performance liquid chromatography (HPLC) has been developed and validated. ENP was separated from NSAIDs using a Purospher STAR C18 column (250×4.6 mm, 5 μm) and a mobile phase consisting of methanol, water (80:20, v/v, pH was adjusted by ortho phosphoric acid to 2.8 at a flow rate of 1.8 mL min -1 and at ambient temperature. Effluents from the column were monitored at 225 nm. The retention time of ENP was 4.1 minute and that for flurbiprofen, diclofenac sodium, ibuprofen and mefanamic acid was 5.4, 5.9, 6.4 and 8.7 mins respectively. LLOD and LLOQ of enalapril were 0.7 and 2.2 ng ml -1 respectively and that of flurbiprofen, diclofenac sodium, ibuprofen and mefanamic were 0.24, 0.07, 0.1, 0.1 and 0.7, 0.2, 0.3 and 0.4 ng ml -1 respectively. The method was validated according to ICH guidelines. Linearity of the method was studied in the concentration range 2.5-100 µg mL -1 for ENP and 0.625-25 µg mL -1 for (NSAIDs) where it demonstrated good linearity with r=0.9995, 0.9979, 0.9995, 0.9967, 0.9967 and 0.9995 (n=6), respectively, recovery was >97.8%. The developed method may successfully be applied for the quantitative analysis of ENP and NSAIDs alone or in combination from raw materials, in bulk drugs, dosage formulations and in serum.
Development and validation of HPLC-UV method for the estimation of fulvestrant in bulk drug
Aim: The present work is aimed to develop a simple, rapid, selective, sensitive and validated HPLC method for the determination of fulvestrant in bulk drug. Method: Fulvestrant was measured using a validated HPLC method with UV detector at 225nm chromatographic peaks were separated on Phenomix, C18 column (250 mm x 4.6 mm x3.5µ) using 50% aetonitrile in channel A and acetonitlile in channel B as mobile phase with gradient elution at a flow rate of 1 ml/min. Results & Discussions: The chromatograms showed good peak shapes and no interference of solvent peaks. The retention time of fulvestrant was found to be 13.6 min. LOD and LOQ were found to be 0.0226µg/ml (0.001%) and 0.0712µg/ml,(0.004%) respectively. The percentage recovery of fulvestrant was found to be 99.1% - 100.75% which are within the limit. The method was linear over the concentration range of 0.08to 2ìg/ml with coefficient of correlation (r2) 0.99997. Both intraday and inter day accuracy and precision data showed good reproducibility. Conclusions: The low % RSD values (= 2) indicated that the method was precise and accurate. this method was successfully applied to forced degradation studies and can be adopted for routine estimation of fulvestrant in quality control laboratories.
HPLC-UV Method for the Determination of Enalapril in Bulk, Pharmaceutical Formulations and Serum
Journal of Analytical & Bioanalytical Techniques, 2012
A simple reversed phase HPLC method have been successfully developed and validated for the quantitative determination of enalapril maleate (ENP) in bulk material, pharmaceutical formulation and serum. Purospher Start C 18 (250 cm x 4.6 mm, 5 µm) and Hypersil, ODS columns were used. The mobile phase, methanol-acetonitrile-water (70:30v/v pH 3.5 adjusted by phosphoric acid), was delivered at a flow rate of 1 mLmin-1 , eluent was monitored using UV detector at 215 nm. The proposed method is specific, accurate (99-102%), precise (intra-day and inter-day variation 0.07-1.25%) and linearity (R 2 >0.999) within the desired range 2.5-100 µgmL-1 concentration. The detection limit and quantification 3.9 ngmL-1 and 12 ngmL-1 respectively. The anticipated method is applicable to routine analysis of ENP in pharmaceutical formulations as well as in human serum samples.