International Journal of Advances in Pharmaceutical Analysis
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Validated gradient Stability-Indicating UPLC Method for the Determination of Lidocaine and its Degradation Impurities in Pharmaceutical Dosage Form
Get PDFObjective: Aim of the present work was to develop a stability indicating ultra performance liquid chromatography (UPLC) method to determine Lidocaine and its degradation impurities in pharmaceutical dosage forms. Method: Chromatographic separation was achieved by gradient elution on Agilent eclipse plus C18 (100x4.6) mm, and 1.8m column with potassium dihydrogen phosphate buffer (pH 4.50) and acetonitrile within a short runtime of 14.0 min. The eluted compounds were monitored at 230 nm using photodiode array (PDA) detector, the flow rate was 1.0 mL/min, and the column oven temperature was maintained at 40 ?C. Result: The resolution of Lidocaine and six (potential, bi-products and degradation) impurities was greater than 2.0 for all pairs of components. The repeatability and intermediate precision, expressed by the RSD, were less than 1.0%. The accuracy and validity of the method were further ascertained by performing recovery studies. The specificity of the method was investigated under different stress conditions including hydrolytic, oxidative, photolytic and thermal as recommended by ICH guidelines. Relevant degradation was found to take place under oxidative condition. Conclusion: Method was Robustness against small modification in pH, column oven temperature, flow rate and percentage of the mobile phase composition was ascertained. All these results provide that the method has stability indicating properties being fit for its intended purpose; it may find application for the routine analysis of the related substances of Lidocaine formulations
Stability-indicating RP-HPLC method for determination of Eprosartan in pure and pharmaceutical formulation
Get PDFA simple, sensitive and specific RP-HPLC method was developed for the determination of Eprosartan in pure and tablet forms. The method showed a linear response for concentrations in the range of 20-120 ?g/mL using Methanol: Acetonitrile: Buffer solution (Dissolve 0.02 M potassium di-hydrogen orthophosphate in water. Adjust pH of solution to 6.85 with orthophosphoric acid) in the ratio (45:35:20) as the mobile phase with detection at 232 nm using photodiode array (PDA) detector and a flow rate of 1 mL/min and retention time 7.1 min. The value of correlation coefficient, slope and intercept were, 0.9998, 1661.8 and 114.82, respectively. The method was validated as per ICH guidelines for precision, recovery, ruggedness and robustness. The specificity of the method was investigated under different stress conditions including acidic, basic, photochemical and thermal as recommended by ICH guidelines. The drug undergoes degradation under acidic, basic, photochemical and thermal degradation conditions. All the peaks of degraded product were resolved from the active pharmaceutical ingredient with significantly different retention time. As the method could effectively separate the drug from its degradation product, it can be employed as a stability-indicating one
New Colorimetric Method Development And Validation Of Sulfacetamide In Bulk And Formulation By Different Analytical Reagents
Get PDFFour simple, sensitive and reproducible spectrophotometric methods (Method A, Method B, Method C and Method D) were developed for the determination of sulfacetamide (SA) and its pharmaceutical formulation. Method A was developed based on diaziatation of the SA by sodium nitrite in acidic medium followed by coupling with B.M reagent having absorption maximum at 530 nm. Method B was developed based on reaction of NQS with primary amine in SA in presence of alkaline medium having maximum absorption at 466nm. Method C was based on reaction of primary amine with MBTH in presence of FeCl3 having maximum absorption at 562nm. Method D was developed based on reduction of phosphomolybdotungstic acid in presence of alkali medium having an absorption maximum at 760 nm. Beers law was obeyed in the range of 1 to 3 g/ml for Method A, 5 to 30 g/ml for Method B, 10 to 50 g/ml for Method C, and 100 to 300 g/ml for Method D. These methods were successfully validated and estimated in bulk and pharmaceutical formulations
A simple reversed phase High Performance Liquid Chromatography method development and validation for determination of Carvedilol in pharmaceutical dosage forms
Get PDFA simple, sensitive and precise reverse phase high performance liquid chromatographic method has been developed for the estimation of Carvedilol in pharmaceutical preparations. Chromatographic determination was performed on a reversed phase C 18 column (4.5 mm x 250 mm; 5 m particle size) using a mixture of Phosphate buffer: Acetonitrile (65:35) as mobile phase at a flow rate of 1ml/min with UV detection at 240 nm. The method was validated for linearity, accuracy, repeatability, precision, reproducibility, and specificity as per International ICH guidelines. The method was also used in determination Carvedilol content in five commercial brands available in Bangladeshi market. The method was linear in the range between 5 35 g/ml, exhibited good correlation coefficient (R 2 = 0.998) and good Accuracy study (98.08 %-99.91%). The method was found to specific for Carvedilol in presence of common excipients. Statistical analysis performed with proposed method proved it to be precise, accurate and reproducible. Hence it can be employed for routine analysis of Carvedilol both in bulk and commercial formulations
Development and Validation of RP HPLC method for the estimation of Etoricoxib in bulk and tablets.
Get PDFObjective: Objective of the present analytical research work was to develop and validate Reverse Phase High Performance Liquid Chromatographic method (RP-HPLC Method) for the Etoricoxib in bulk and tablets dosage form. Methods: A RP-HPLC method has been developed and validated for estimation of ETOR in pharmaceutical oral dosage form. Method A (RP-HPLC Method): The RP-HPLC Method for Etoricoxib was developed using Shimadzu HPLC, LC-10, temperature maintained 25 0C, phenorex Gemini C18 (250 mm 4.60 mm 5?m), as stationary particle, isocratic mode. Water: ACN: OPA: TEA (40:60:0.1:0.1, v/vv/v). Mobile phase was maintained at a flow rate of 1.0 ml/min and detection was carried out at 245 nm. Results: Etoricoxib was found to be linear in the concentration range of 8 - 12 ?g/ml for RP-HPLC method. Retention time was found to be 2.7 min for Etoricoxib. The amount of Etoricoxib in marketed formulation was found to be 99.14 %. Interpretation and Conclusion: Results of assay and validation study were found to be satisfactory. So, the method can be successfully applied for the routine analysis of Etoricoxib
Simultaneous estimation of Etodolac and Paracetamol in bulk drug dosage form by RP-HPLC
Get PDFA simple, specific, rapid, economical and accurate reverse phase high performance liquid chromatographic method was developed for simultaneous estimation of Etodolac and Paracetamol in bulk drug and tablet dosage form. Sepration was achieved by capcell pack C-18 column having 250 mm4.6 mm i.d. in isocratic mode, with mobile phase containing 25 nM potassium dihydrogen phosphate buffer(adjusted to pH 6.1 using ortho phosphoric acid) : methanol (40:60). The flow rate was 1.0 ml/min and effluents were monitored at 235 nm. The retention time of Etodolac and Paracetamol were 3.19 min and 6.08 min respectively. The linearity for Etodolac and Paracetamol were in the range of 10-100 ?g/ml. The recoveries of Etodolac and Paracetamol were found in the range of 99.27-99.78 % and 99.74-99.88 % respectively. The proposed method was validated as per ICH and USP guidelines and successfully applied to the estimation of Etodolac and Paracetamol in bulk drug and tablet dosage form
STABILITY INDICATING RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF RABEPRAZOLE SODIUM AND LEVOSULPIRIDE IN CAPSULE DOSAGE FORM
No full textA Stability indicating Reverse-Phase liquid chromatographic method for the simultaneous estimation of RPS and LSP was developed. The chromatographic assay involves the use of C 18 Column (150 4.6mm, with particle size 5?m) with a simple mobile phase composition (Phosphate Buffer pH-3.3 and Methanol 55:45 v/v) at a flow rate of 1mL/min with U.V detection at wavelength of 230 nm. The method showed good linearity in the concentration range of 90.0-210.0 ?g/mL for LSP and 24.056.0 ?g/mL for RPS. The proposed method was also successfully applied to 20 tablets of marketed formulation (Neopride). The developed method was successfully validated as per the ICH guidelines for following parameters. Accuracy, precision, repeatability, ruggedness, robustness, system suitability tests, etc. The RSD for Intra-day and Inter-day precision was found to be 1.02-1.83, 0.96-1.42 For LSP and 0.55-0.59, 0.75-0.63 for RPS. Average Percent recovery was found to be 980.2, 100.570.2, 99.800.2 for LSP and 101.380.2, 98.670.2, 99.530.2 for RPS which was a good agreement with labeled amount of pharmaceutical formulation. The stability indicating capacity was tested by accelerated degradation of marketed formulation in acidic (0.1 N HCl), basic (0.1 N NaOH), Neutral (water), Oxidative (3% H 2 O 2 ), Thermal (60 0 C), Sunlight exposure
Development and Validation of UV Spectrophotometric and RP HPLC method for the estimation of Eszopiclone bulk and tablets.
Get PDFObjective: Objective of the present analytical research work was to develop and validate Spectrophotometric method and Reverse Phase High Performance Liquid Chromatographic method (RP-HPLC Method) for the Eszopiclone bulk and tablets dosage form. Methods: A spectrophotometric method and a RP-HPLC method have been developed and validated for estimation of ESZ in pharmaceutical oral dosage form. Method A (RP-HPLC Method): The RP-HPLC Method for Eszopiclone was developed using Shimadzu HPLC, LC-10, temperature maintained 25 0C, phenorex Gemini C18 (250 mm 4.60 mm 5?m), as stationary particle, isocratic mode. MeOH: Water (80:20v/v) as mobile phase. Mobile phase was maintained at a flow rate of 1.0 ml/min and detection was carried out at 305 nm. Method B (UV SPECTROMETRY Method): The stock and working standard solutions of the drugs were prepared in methanol. Standard solutions were scanned over the range of 400-200 nm in spectrum mode of spectrophotometer at medium scanning speed using UV spectrophotometer 2450, SHIMADZU. The maximum absorbance for Eszopiclone was found at 305 nm. Both the methods were validated in accordance with ICH guidelines Results: Eszopiclone was found to be linear in the concentration range of 4 - 24 ?g/ml for spectrophotometric method and 5-30 ?g/ml for RP-HPLC method. Retention time was found to be 5.38 min for Eszopiclone. The amount of Eszopiclone in marketed formulation by spectrophotometric method was found to be 100.02 %, the amount of Eszopiclone in marketed formulation by RP-HPLC method was found to be 100.03 %. Interpretation and Conclusion: Results of assay and validation study were found to be satisfactory. So, the methods can be successfully applied for the routine analysis of Eszopiclone
Estimation of Pazopanib Hydrochloride in Tablet Dosage Forms By RP-HPLC
Get PDFA simple, precise, rapid and accurate RP- HPLC method was developed for the Estimation of Pazopanib HCl (PZP) in tablet dosage forms. An XTerra RP C 18 , (250X4.6 with 5 microns particle size) and the mobile phase, consisting of 0.03M KH 2 PO 4 in water adjusting the pH-3.2 with O-Phosphoric Acid: Acetonitrile in ratio of 70:30 v/v and water: Acetonitrile (50:50 v/v) was used as diluent in the gradient mode. The flow rate was 1.0 ml/min and the effluents were monitored at 267 nm. The retention time was 7.392 for Pazopanib HCl. The detector response was linear in the concentration of 20-240 g/mL for PZP. The respective linear regression equation being Y (528142.1276 = 172694.049x + 428066.7611 for PZP. The Limit of Detection (LOD) is 0.10 and The Limit of Quantification (LOQ) is 0.30 for PZP respectively. The % assay of PZP was found out to be 99.49%. The method was validated by determining its accuracy, precision and system suitability. The results of the study showed that the proposed RP-HPLC method is simple, rapid, precise and accurate, which is useful for the routine determination of PZP in bulk drug and in its pharmaceutical dosage forms
Extractive method development and validation of tulobuterol in api and its pharmaceutical dosage forms by spectrophotometry
Get PDFA simple, accurate, sensitive and reproducible visible spectrophotometric method has been developed for the determination of Tulobuterol (TLB) in bulk and also in its pharmaceutical dosage formulations. The proposed method was based on complexation of the drug with Bromo Cresol Green (BCG) extracted with chloroform showing absorbance maxima at 624 nm respectively. Beer's law is obeyed over a concentration range of 0.1-0.8g/mL. The respective linear regression equation being Y (0.0309) =1.065x +0.0396 for TLB. Results of analysis for the method established, was validated statistically and also by recovery studies. The color was stable for about 1 hour. The apparent molar absorptivity and Sandells Sensitivity values are 0.43x10 4 L mol-1 cm -1 and 0.7674gcm -2 respectively. The assay and recovery studies were found to be 101.43% and coefficient correlation(r) was found to be0.994.The different experimental parameters effecting the development and stability were studied carefully and optimized. No interference was observed in the presence of common pharmaceutical excipients. The validity of the methods was tested by analyzing the drug in its pharmaceutical preparations. Good recoveries were also obtained. The developed method employed was successful for the determination of TLB in various pharmaceutical preparations