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G. V. H. Raju ¹, S. Ganapathy ¹, D. G. Sankar ¹, P. Y. Naidu ¹

Affiliations
1 Department of Pharmaceutical Sciences, Andhra University, Visakhapatnam-530003, IN

Abstract

A simple high-performance liquid chromatographic method for the determination of tadalafil in human plasma has been developed. Separation was achieved by Reverse phase chromatography on a Grace Genesis C18 (150 x 4.6 mm, 5μ) column with mobile phase A containing Triethylamine buffer (pH adjusted to 2.5±0.05 with Orthophosphoric acid) and mobile phase B containing Acetonitrile 95%(95:5 (Acetonitrile:water)) as eluent at a flow rate 1.2ml/min. UV detection was performed at 225nm. Lower limit of quantitation was 4.997ng/ml. Maximum between-run precision was 2.085%. Mean extraction recovery was found to be 97.38 to 97.45%. Stability study showed that after three freeze-thaw cycles the loss of three quality control samples were less than 10%. Samples were stable at room temperature for 48h and at -20° for 2months. Before injecting onto HPLC system, the processed samples were stable for at least 6h. The method can be used to perform bioequivalence study in human.

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R. Narendra Kumar ¹, G. Nageswara Rao ¹, P. Y. Naidu ¹

Affiliations
1 School of Chemistry, Andhra University, Visakhapatnam, IN

Abstract

A Fast LC method has been developed and subsequently validated for the determination of Cefditoren pivoxil and its related impurities in bulk and pharmaceutical formulation. Separation was achieved in Gradient mode using Hypersil BDS, C18, 100 x 4.6 mm, 3μm column with mobile phase A containing Ammonium formate buffer (pH adjusted to 6.0±0.05 with formic acid solution) and mobile phase B containing Methanol and Acetonitrile (40:60 v/v) at different time intervals as eluent at a flow rate 1.2ml/min. UV detection was performed at 230nm. The method is simple, rapid, and selective and stability indicating. The described method is linear over a range of 200.34μg/mL to 1520.56μg/mL. The method precision for the determination of assay was below 2.0% RSD .The Percentage recoveries of Active Pharmaceutical Ingredient (API) from dosage form is 99.2. LOD and LOQ of all related impurities of Cefditoren pivoxil was established and ranged from 0.0431μg/ml - 0.1843μg/ml for LOD and 0.1292μg/ml - 0.6014μg/ml for LOQ. The method is useful in the quality control of bulk manufacturing and also in pharmaceutical formulations.

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G. V. H. Raju ¹, S. Ganapathy ¹, D. G. Sankar ¹, P. Y. Naidu ¹

Affiliations
1 Department of Pharmaceutical Sciences, Andhra University, Visakhapatnam-530003, IN

Abstract

A simple, sensitive and reproducible UV-Visible spectrophotometric methods (Method A to Method C) are developed for the determination of Tadalafil (TADL) in pure and dosage forms. Method A is based on the formation of colored species on treatment of Tadalafil (TADL) with Folin-Ciocalteu reagent in presence of 4% NaOH Solution. Method B is based on the formation of colored species on treatment of Tadalafil (TADL) with Sodium nitroprusside and Hydroxyl amine. Method C represents UV Spectrophotometric determination of Tadalafil (TADL) and its dosage forms in pH 2.9 Buffer:Acetonitrile (40:60v/v) at 285nm.

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G. V. H. Raju ¹, S. Ganapathy ¹, D. G. Sankar ¹, P. Y. Naidu ¹

Affiliations
1 Department of Pharmaceutical Sciences, Andhra University, Visakhapatnam-530003, IN

Abstract

A simple, sensitive and reproducible UV-Visible spectrophotometric methods (Method A to Method F) are developed for the determination of Aripiprazole (ARIP) in pure and dosage forms. Method A is based on the formation of colored species on treatment of Aripiprazole (ARIP) with 3-Methyl-2-benzo thiazolinone hydrazone (MBTH) and Cerric Ammonium Sulphate (CAS). Method B is based on the formation of colored species on treatment of Aripiprazole (ARIP) with Fecl₃ and 1,10 PTL. Method C is based on the formation of colored species on treatment of Aripiprazole (ARIP) with Folin-Ciocalteu reagent in presence of 4% NaOH Solution. Method D is based on the formation of colored species on treatment of Aripiprazole (ARIP) with DCQC (2,6-dichloroquinone N-chlorimide, Gibbs Reagent). Method E is based on the formation of colored species on treatment of Aripiprazole (ARIP) with NQS (1,2-napthaquinone-4-sulphonic acid). Method F represents UV Spectrophotometric determination of Aripiprazole (ARIP) and its dosage forms in pH 3.0 Buffer:Acetonitrile (62:38v/v) at 250 nm.

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G. V. H. Raju ¹, S. Ganapathy ¹, D. G. Sankar ¹, P. Y. Naidu ¹

Affiliations
1 Department of Pharmaceutical Sciences, Andhra University, Visakhapatnam-530003, IN

Abstract

A simple Reverse Phase liquid chromatographic (HPLC) method for the determination of Levetiracetam in human plasma has been developed. Separation was achieved on a Prontosil C8 (150×4.6 mm, 5 μm) column with mobile phase composition of [pH 3.8 buffer:acetonitrile] (Solution A): HPLC grade water (Solution B) in the ratio 60:40 v/v with ultra violet detection at 210 nm. Lower limit of quantitation was 200 ng/ml. Maximum between-run precision was 5.91%. Mean extraction recovery was found to be 100.02 to 103.06%. Stability study showed that after three freeze-thaw cycles the loss of three quality control samples were less than 10%. Samples were stable at room temperature for 48h and at -20° for 2 months. Before injecting onto HPLC system, the processed samples were stable for at least 6 h. The method was used to perform bioequivalence study in human.

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R. Narendra Kumar , G. Nageswara Rao , P. Y. Naidu

Abstract

An isocratic stability indicating liquid chromatographic method has been developed and validated for the determination of Eszopiclone in bulk drug and its pharmaceutical dosage form. Separation of the drug with degradation products was achieved using Peerless HT, C8, 50×4.6 mm; 1.8 μm column as stationary phase and pH 4.5(±0.05) buffer:Acetonitrile:Tetrahydrofuran (81:18:1, v/v) as mobile phase at a flow rate of 1.0 mL/min. UV detection was performed at 304 nm. The method is linear over the range of 10-150 μg/mL. The percent recovery of drug in dosage forms was ranged from 97.7 to 100.5. The method is simple, rapid, precise, selective and stability indicating and can be used for the assay in quality control and stability studies samples.

Keywords

Bird Flu, Chemsketch, Docking, Hex, Rasmol.

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G. V. H. Raju ¹, S. Ganapathy ¹, D. G. Sankar ¹, P. Y. Naidu ¹

Affiliations
1 SIPCOT Industrial Park, Plot No’s. B3-B6, Irungattukottai, Sriperumbudur-602105, Kancheepuram District, IN

Abstract

An Rapid Resolution Liquid Chromatographic method (RRLC) has been developed and subsequently validated for the determination of Aripiprazole and its intermediates in bulk and pharmaceutical formulation. Separation was achieved with a Hypersil gold, C18, 50×4.6 mm, 5 μm column with Mixture of Potassium Dihydrogen Phosphate and Triethylamine (pH adjusted to 3.0±0.05 with Orthophosphoric acid):Acetonitrile:Methanol (60:20:20 ,v/v) as eluent at a flow rate 1.0 ml/min. UV detection was performed at 252 nm. The method is simple, rapid, selective and stability indicating. The described method is linear over a range of 30.507 μg/mL to 183.040 μg/mL. The method precision for the determination of assay was below 2.0% RSD. The Percentage recoveries of Active Pharmaceutical Ingredient (API) from dosage forms ranged from 97.4 to 100.2 for all available strengths of Arpiprazole in market. LOD and LOQ of all related impurities of Aripiprazole was established and ranged from 0.015 μg/ml-0.034 μg/ml for LOD and 0.04 μg/ml-0.101 μg/ml for LOQ. The method is useful in the quality control of bulk manufacturing and also in pharmaceutical formulations.

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G. V. H. Raju , S. Ganapathy , D. G. Sankar , P. Y. Naidu

Abstract

Fast LC method has been developed and subsequently validated for the determination of Tadalafil and its intermediates in bulk and pharmaceutical formulation. Separation was achieved in Gradient mode using Peerless HT gold, C18, 50×4.6 mm, 1.8 μm column with mobile phase A containing Potassium Dihydrogen Phosphate buffer (pH adjusted to 3.0±0.05 with Orthophosphoric acid) and mobile phase B containing Methanol 100% at different time intervals as eluent at a flow rate 0.8 ml/min. UV detection was performed at 220 nm. The method is simple, rapid, selective and stability indicating. The described method is linear over a range of 12.5748 μg/mL to 76.4548 μg/mL. The method precision for the determination of assay was below 2.0% RSD. The Percentage recoveries of Active Pharmaceutical Ingredient (API) from dosage forms ranged from 101.0 to 102.1 for all available strengths of Tadalafil in market. LOD and LOQ of all related impurities of Tadalafil was established and ranged from 0.006 μg/ml-0.011 μg/ml for LOD and 0.018 μg/ml-0.033 μg/ml for LOQ. The method is useful in the quality control of bulk manufacturing and also in pharmaceutical formulations.

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G. V. H. Raju ¹, S. Ganapathy ¹, D. G. Sankar ¹, P. Y. Naidu ¹

Affiliations
1 Department of Pharmaceutical Sciences, Andhra University, Visakhapatnam-530003, IN

Abstract

A simple high-performance liquid chromatographic method for the determination of Gemifloxacin in human plasma has been developed. Separation was achieved by Reverse phase chromatography on a Purospher RP18e (150×4.6 mm, 5 μm) column with mobile phase composition of pH 3.0 buffer: acetonitrile: Methanol in the ratio 75:17:8 v/v with ultra violet detection at 273 nm. Lower limit of quantitation was 50 ng/ml. Maximum between-run precision was 7.44%. Mean extraction recovery was found to be 92.53 to 109.87%. Stability study showed that after three freeze-thaw cycles the loss of three quality control samples were less than 10%. Samples were stable at room temperature for 48 h and at -20° for 2 months. Before injecting onto HPLC system, the processed samples were stable for at least 6 h. The method was used to perform bioequivalence study in human.

Keywords

RP HPLC, Validation, Atenolol.

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G. V. H. Raju ¹, S. Ganapathy ¹, D. G. Sankar ¹, P. Y. Naidu ¹

Affiliations
1 Orchid Healthcare, SIPCOT Industrial Park, B3-B6, Irungattukottai, Sriperumbudur-602105, Kancheepuram District, IN

Abstract

An isocratic reversed phase liquid chromatographic (RP-HPLC) method has been developed and subsequently validated for the determination of Levetiracetam in bulk and pharmaceutical formulation. Separation was achieved with a Hypersil Gold 150×4.6 mm; 5μ column with Mixture of Potassium Dihydrogen Phosphate and Sodium 1-Heptane Sulphonate (pH adjusted to 2.8±0.05 with Orthophosphoric acid):Acetonitrile (90:10, v/v) as eluent at a flow rate 1.0 ml/min. UV detection was performed at 220 nm. The method is simple, rapid, selective and stability indicating. The described method is linear over a range of 43.444 μg/mL to 289.629 μg/mL. The method precision for the determination of assay was below 1.0% RSD. The Percentage recoveries of Active Pharmaceutical Ingredient(API) from dosage forms ranged from 100.2 to 101.0. The method is useful in the quality control of bulk manufacturing and also in pharmaceutical formulations.

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