scholarly journals Determination of Carbamazepine and Its Impurities Iminostilbene and Iminodibenzyl in Solid Dosage Form by Column High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (4) ◽  
pp. 1059-1068 ◽  
Author(s):  
Predrag Lj Džodić ◽  
Ljiljana J ivanovi ◽  
Ana D Proti ◽  
Mira L Zeevi ◽  
Biljana M Joci
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Solid Dosage ◽  
Rp Hplc ◽  
Good Repeatability ◽  
Chemometric Approach

Abstract An accurate and precise RP-HPLC method was developed and validated for the determination of carbamazepine and its impurities iminostilbene and iminodibenzyl in a tablet formulation with fluphenazine as an internal standard. Buffermethanol (50 + 50, v/v) was used as the mobile phase. During validation, specificity, linearity, precision, accuracy, LOD, LOQ, and robustness of the method were tested. The method was proven to be specific against placebo interference. Linearity was evaluated over the concentration range of 100500, 0.050.25, and 0.10.5 g/mL, and the r values were 0.9994, 0.9997, and 0.9979 for carbamazepine, iminostilbene, and iminodibenzyl, respectively. Intraday precision of the method was good, and RSD was below 2 for all analytes. The accuracy of the method ranged from 100.69 to 102.10, 99.76 to 102.66, and 99.26 to 100.08 for carbamazepine, iminostilbene, and iminodibenzyl, respectively. LOD was 0.0125, 0.025, and 0.05 g/mL and LOQ was 0.05, 0.05, and 0.1 g/mL for carbamazepine, iminostilbene, and iminodibenzyl, respectively. Robustness of the method was proven by using a chemometric approach. The method was successfully applied to the analysis of commercially available carbamazepine tablets and showed good repeatability, with RSD below 2.

scholarly journals Validation of an HPLC method for the simultaneous determination of eletriptan and UK 120.413

2006 ◽  
Vol 71 (11) ◽  
pp. 1195-1205 ◽  
Author(s):  
Mira Zecevic ◽  
Biljana Jocic ◽  
Snezana Agatonovic-Kustrin ◽  
Ljiljana Zivanovic
Keyword(s):  
Mobile Phase ◽  
Analytical Procedure ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Control Analysis ◽  
Internal Standard Method ◽  
Rp Hplc ◽  
Good Repeatability

Arapid and sensitive RPHPLCmethod was developed for the routine control analysis of eletriptan hydrobromide and its organic impurity UK 120.413 in Relpax? tablets. The chromatography was performed at 20?C using a C18 XTerra ? (5 ?m, 150 x 4,6 mm) column at a flow rate 1.0 ml/min. The drug and its impurity were detected at 225 nm. The mobile phase consisted of TEA (1 %) - methanol (67.2:32.8 v/v), the pH of which was adjusted to 6.8 with 85 % orthophosphoric acid. Quantification was accomplished by the internal standard method. The developed RP HPLC method was validated by testing: accuracy, precision, repeatability, specificity, detection limit, quantification limit, linearity, robustness and sensitivity. High linearity of the analytical procedure was confirmed over the concentration range of 0.05 - 1.00 mg/ml for eletriptan hydrobromide and from 0.10 - 1.50 ?g/ml for UK 120.413, with correlation coefficients greater than r = 0.995. The low value of the RSD expressed the good repeatability and precision of the method. Experimental design and a response surface method were used to test robustness of the analytical procedure and to evaluate the effect of variation of the method parameters, namely the mobile phase composition, pH and temperature. They showed small deviations from the method setting. The good recovery and low RSD confirm the suitability of the proposed RP HPLC method for the routine determination of eletriptan hydrobromide and its impurity UK 120.413 in Relpax? tables.

scholarly journals Analysis of Nabumetone in Bulk and Tablet Formulation by a New and Validated Reverse Phase High Performance Liquid Chromatography

2009 ◽  
Vol 6 (s1) ◽  
pp. S59-S64 ◽  
Author(s):  
Prafulla Kumar Sahu ◽  
M. Mathrusri Annapurna
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Internal Standard ◽  
Dosage Forms ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

RP-HPLC analytical method for the estimation of nabumetone in pharmaceutical dosage forms was developed and validated. A Hypersil ODS C18, 4.6 mm x 250 mm, 5 μm column from Supelco (India), with mobile phase comprised of acetonitrile: triple distilled water (50:50) with a total run time of 18 min was used and the wavelength of the detector was set at 230 nm. Stavudin is used as internal standard. The retention times were 14.167 min and 1.967 min for nabumetone and stavudin (IS) respectively. The extraction recovery of nabumetone from pharmaceutical dosage form (tablets) was >101% and the calibration curve was linear (r2= 0.995) over nabumetone concentrations ranging from 1 to 200 µg/mL. The method had an accuracy of >99% and LOD and LOQ of 0.17482 µg/mL and 0.5827 µg/mL respectively. The method reported is simple, reliable, precise and accurate and has the capability of being used for determination of nabumetone in bulk and pharmaceutical dosage forms.

scholarly journals Method Development and Validation of Polmacoxib in Capsule Dosage Form by RP-HPLC

2021 ◽  
Vol 11 (4-S) ◽  
pp. 59-63
Author(s):  
Anjali Chaudhary ◽  
Meenakshi Dhaiya ◽  
Shaily Tyagi ◽  
Swati Mittal
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Intended Use

A simple and sensitive RP-HPLC method developed for estimation of Polmacoxib in bulk by using a high performance liquid chromatography with PDA detector using Phenomenex luna C18 column (250mmx4.6mm), 5 µm; mobile phase comprises of Water : ACN as (1:1) at the flow rate 1.0 ml/min and the wavelength of detection  238 nm and eluted at 8.12 minutes. The proposed method is validated for specificity, Linearity, Precision, accuracy, ruggedness, and Robustness. All the parameters were found within the acceptable limits. RP-HPLC method was a simple, reliable economic and acceptable and it confirmed that method is suitable for the intended use for routine quality control and assay of drugs. This method is successfully applied for the determination of commercial dosage form capsule preparation. This method is validated as per ICH (International conference on harmonization) Guidelines. Keywords: Polmacoxib, RP-HPLC, ICH, PDA Detector, Precision

NEW VALIDATED RP-HPLC METHOD FOR THE DETERMINATION OF RIZATRIPTAN BENZOATE IN BULK AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (12) ◽  
pp. 32-36
Author(s):  
T. Vishalakhi ◽  
◽  
S. K Kumar ◽  
K Sujana ◽  
P Rani
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Detector Response ◽  
Mobile Phase Flow Rate ◽  
Pharmaceutical Dosage Form ◽  
Rizatriptan Benzoate ◽  
Rp Hplc ◽  
Bulk Drug

A simple validated RP HPLC method for the estimation of rizatriptan benzoate in pharmaceutical dosage form and bulk was developed for routine analysis. This method was developed by selecting Agilent TC C18 (250 x 4.6 mm, 5 μ) column as stationary phase and acrylonibrile:water (45:55), pH adjusted to 3, as mobile phase. Flow rate of mobile phase was maintained at 4: 1 mL/min at ambient temperature throughout the experiment. Quantification was achieved with ultraviolet (DAD) detection at 220 nm. The retention time obtained for rizatriptan was 2.8 min. The detector response was linear in the concentration range of 2-25μg/mL. This method was validated and shown to be specific, sensitive, precise, linear, accurate, rugged and robust. Hence, this method can be applied for routine quality control of rizatriptan benzoate in dosage forms as well as in bulk drug.

Simultaneous determination of Sulphadoxine and Pyrimethamine by taking Tolterodine as an internal standard in Pharmaceutical dosage form by RP-HPLC

2021 ◽  
pp. 145-150
Author(s):  
Sushil D. Patil ◽  
Pravin B. Shelke ◽  
Priti Aher ◽  
Maswood Ahmed Hafizur Rahman
Keyword(s):  
Simultaneous Determination ◽  
Dosage Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Control Analysis ◽  
Pharmaceutical Dosage Form ◽  
Quality Control Analysis ◽  
Rp Hplc ◽  
Sulphadoxine Pyrimethamine

A simple, rapid, economic, sensitive and precise HPLC method has been developed for the simultaneous determination of Sulphadoxine and Pyrimethamine in pharmaceutical dosage form by taking Tolterodine as an internal standard. The method was carried out using Phenomenex C18 (4.6ID × 250mm; 5µm) column and mobile phase comprised of methanol and Phosphate Buffer in proportion of ratio 60:40 v/v. The flow rate was 1.0mL/min and detection was carried out at 276nm. The retention time of Sulphadoxine, Pyrimethamine and Tolterodine were found to be 2.967, 4.058 and 6.908 respectively. Linearity of Sulphadoxine and Pyrimethamine in the range of 2 to 12μg/mL and 4 to 24μg/mL respectively. The % recoveries of Sulphadoxine and Pyrimethamine were found to be in between 99.93% to 99. 96 % respectively. The proposed method is suitable for the routine quality control analysis for simultaneous determination of Sulphadoxine and Pyrimethamine was in bulk and pharmaceutical dosage form.

scholarly journals Development and Validation of RP-HPLC Method for the Simultaneous Determination of Rabeprazole Sodium and Itopride Hydrochloride in Solid Dosage Form

2010 ◽  
Vol 7 (3) ◽  
pp. 947-952 ◽  
Author(s):  
Rajesh Sharma ◽  
Ganesh Prasad Mishra ◽  
Subhash Chandra Chaturvedi
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Solid Dosage Form ◽  
Solid Dosage ◽  
Rabeprazole Sodium ◽  
Itopride Hydrochloride

A simple, sensitive, precise, accurate, rapid and reproducible reverse phase high performance liquid chromatographic procedure is developed for simultaneous determination of rabeprazole sodium and itopride hydrochloride in solid dosage form. The mobile phase used was a combination of acetonitrile: buffer (35:65 v/v) and the pH was adjusted to 7.0 ± 0.1 by addition of triethylamine. The detection of the capsule dosage form was carried out at 266 nm and a flow rate employed was 1 mL/min. Linearity was obtained in the concentration range of 2 to 16 μg/mL of rabeprazole sodium and 5 to 55 μg/mL of itopride hydrochloride with a correlation coefficient of 0.9992 and 0.9996 respectively. The results of the analysis were validated statistically and recovery studies confirmed the accuracy of the proposed method.

scholarly journals Stability indicating RP-HPLC method for the estimation of flucloxacillin sodium in a tablet dosage form

2020 ◽  
Vol 1 (4) ◽  
pp. 95-100
Author(s):  
Sonalika Patro ◽  
S. Harshith Kumar ◽  
M. Barath kumar ◽  
E. Masthaniah ◽  
K. Sairam ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Theoretical Plate ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Suitability ◽  
Precision Study ◽  
Tablet Dosage

A Simple, accurate and precise method was developed and validated for the determination of flucloxacillin sodium in its tablet dosage form. The separation was eluted on xterra c18 column (4.6x150mm, 5micron) using a mixture of octane buffer and methanol as mobile phase in a ratio of (30:70) which was pumped through column at a flow rate of  1ml/min. Optimised wavelength for flucloxacillin was 237nm, the retention time was 2.305minutes and the percentage purity was found to be 98.14%. System suitability parameters such as theoretical plate and tailing factor for flucloxacillin sodium was found to be 2991.64 and 1.90 respectively, the proposed method was validated as per ICH guidelines (ICH, Q2 AND (R1)) the method was found to be linear at the concentration range of 20-100µg/ml and the correlation coefficient (r2) value was found to be 0.9994 percentage RSD for precision was 0.9% and percentage RSD for ruggedness was 0.5%. The precision study was precise, robust and repeatable. The LOD and LOQ values are 2.98 and 9.98 respectively. Hence the suggested RP-HPLC method can be used for routine analysis for flucloxacillin sodium in tablet dosage form.

APPLICATION OF HPTLC AND RP-HPLC METHODS FOR SIMULTANEOUS ESTIMATION OF OFLOXACIN AND PREDNISOLONE ACETATE IN OPHTHALMIC DOSAGE FORM

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (05) ◽  
pp. 17-26
Author(s):  
M. L Chavhan ◽  
◽  
A. S Patil ◽  
S. J Surana ◽  
A. A. Shirkhedkar
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Internal Standard ◽  
Prednisolone Acetate ◽  
Simultaneous Estimation ◽  
Hplc Separation ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Ophthalmic Formulation

Two simple, rapid, precise, accurate and robust (HPTLC and RP-HPLC) methods have been established for simultaneous determination of ofloxacin and prednisolone acetate in its combined ophthalmic formulation. HPTLC separation of two drugs was accomplished on a HPTLC aluminum-backed layer of silica gel 60 F254 using n-butanol: methanol: ammonia (60:10:30% V/V/V) as a mobile phase. The densitometric scanning was performed at 275 nm which showed Rf 0.43 for ofloxacin and 0.78 for prednisolone acetate, respectively. RP-HPLC separation of the two drugs was achieved on LC-GC Qualisil BDS C-18 column using mobile phase methanol: acetonitrile: 0.02 M potassium dihydrogen ortho-phosphate anhydrous (50:15:35% V/V/V), pH adjusted to 4.5 with triethylamine. Detection of both drugs was done at 275 nm. Aspirin was used as an internal standard (IS). The retention time for ofloxacin, prednisolone acetate and aspirin (IS), was found to be 4.36 min. and 6.60 min and 3.55 min, respectively. The proposed methods were successfully applied for the determination of both drugs in bulk and in combined ophthalmic formulation. Assay of both these methods were compared using student t-test.

scholarly journals A Validated RP-HPLC Method for Simultaneous Estimation of Atenolol and Indapamide in Pharmaceutical Formulations

2011 ◽  
Vol 8 (3) ◽  
pp. 1238-1245 ◽  
Author(s):  
G. Tulja Rani ◽  
D. Gowri Sankar ◽  
P. Kadgapathi ◽  
B. Satyanarayana
Keyword(s):  
Particle Size ◽  
Mobile Phase ◽  
Dosage Form ◽  
Orthophosphoric Acid ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Ich Guidelines

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.

scholarly journals Development of RP-HPLC Method for the Estimation of Rabeprazole in Pure and Tablet Dosage Form

2008 ◽  
Vol 5 (s2) ◽  
pp. 1149-1153 ◽  
Author(s):  
A. Lakshmana Rao ◽  
B. N. V. Ravi Kumar ◽  
G. G. Sankar
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Assay Method ◽  
Control Analysis ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, rapid, sensitive and precise High Performance Liquid Chromatographic (HPLC) method has been developed for the estimation of rabeprazole in bulk and tablet dosage form. In this method RP-C18column (150 mm x 4.6 mm I.D, 5 µ m particle size) with mobile phase consisting of methanol and water in the ratio of 65:35 v/v in isocratic mode was used. The detection wavelength is 284 nm and the flow rate is 0.8 mL/min. Tinidazole is used as internal standard. In the range of 0.25-20 µ g/mL, the linearity of rabeprazole shows a correlation coefficient of 0.9999. The drug and internal standard were eluted at 4.41± 0.05 and 2.16± 0.04 min. respectively. The intra- and inter-day variation was found to be less than 1% showing high precision of the assay method. The detection limit was found to be 100 ng/mL. The mobile phase selected for the proposed method is simple, fast, accurate and precise and hence can be applied for routine quality control analysis of rabeprazole in bluk and its tablet dosage from.

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