HPLC

ABSTRACTThe introduction of imatinib, an oral tyrosine kinase inhibitor, as first-line standard therapy in patients with unresectable, metastatic, or recurrent gastro-intestinal stromal tumor (GIST), strongly improved their treatment outcomes. A fast and cheap method was developed and validated using high-performance liquid chromatography-mass spectrometry for quantification of imatinib in human serum and tamsulosin as the internal standard. Remarkable advantages of the method includes use of serum instead of plasma, less time spent on processing and analysis, simpler procedures, and requiring reduced amounts of biological material, solvents, and reagents. LC-MS, HPLC and UV Spectrophotometry validated methods have proved to be linear, accurate, precise, and robust, it is suitable for pharmacokinetic assays, such as bioavailability and bioequivalence, and is being successfully applied in routine therapeutic drug monitoring in the hospital service Keywords: Imatinib, LC-MS, HPLC, UV Spectrophotometry.

ABSTRACTA simple, Precised, Accurate method was developed for the estimation of Abiraterone by RP-HPLC technique. Chromatographic conditions used are stationary phase  Azilent  C18 (150mm x 4.6 mm, 5m )Mobile phase 0.01%KH2PO4:Acetonitrile  in the ratio of 60:40 and flow rate was maintained at 1.0 ml/min, detection wave length was 235 nm, column temperature was set to 30oC and diluent was mobile phase Conditions were finalized as optimized method. System suitability parameters were studied by injecting the standard six times and results were well under the acceptance criteria. Linearity study was carried out between 25% to150 % levels, R2 value was found to be as 0.999. Precision was found to be 0.7 for repeatability and 0.2for intermediate precision. LOD and LOQ are 1.629µg/ml and 4.937µg/ml respectively. By using above method assay of marketed formulation was carried out 100.81% was present. Degradation studies of Abiraterone were done, in all conditions purity threshold was more than purity angle and within the acceptable range .Full length method was not performed ; if it is done this method can be used for routine analysis of AbirateroneKeywords: HPLC ,  Abiraterone , Method development , ICH Guidelines  

ABSTRACTDoxofylline a bronchodilator and anti-tussive is used for chronic obstructive pulmonary disease (COPD) and asthma that acts as phosphor diesterase inhibitor with minimum cardiovascular side effects due to low affinity foradenosine receptors (both A1 and A2) unlike theophylline and other xanthine derivatives. Doxofylline is water soluble and comes under biopharmaceutical classification class III with high solubility and low permeability. In this study an attempt has been made in development and to evaluate the formulation of Doxofylline tablets of 400mg and these compressed tablets were tested for friability, thickness, disintegration time, hardness, weight variation and assay. The formulation trial F4 was optimized considering the drug release profile and the disintegration time of tablets as they were very close to the reference product values. From this study, it may be concluded that for Doxofylline tablets, F4 stands as a successful formulation and can be manufactured with reproducible characteristics from batch to batch to match the release profile with the reference product. The in-vitro release of Doxofylline tablets was studied in 900 ml of distilled water as dissolution medium using an I.P dissolution paddle assembly at 100rpm and 37±2°C for 45min. Keywords: Doxofylline tablets, Micro crystalline cellulose, HPLC, Antiasthmatic

ABSTRACTA new precise, accurate, robust and stability indicating high-performance liquid chromatographic method has been developed and validated for the simultaneous estimation of domperidone (DOM) and esomeprazole (ESO) in their pharmaceutical formulation. The proposed method carried out on Waters Symmetry C18 column (250 mm x 4.6 mm, 5.0 µm particle size) using an isocratic elution technique at a column temperature of 30 ?C. The mobile phase was a mixture of 0.01M sodium acetate buffer: methanol (45:55 v/v) and it was adjusted to pH 4.5 using glacial acetic acid with a flow rate of 1 mL/min and an injection volume of 20 µL. The retention times were 3.7 and 5.0 min with UV detection at 290 nm for DOM and ESO, respectively. The proposed method was linear over the concentration ranges of 0.04-60.0 and 0.08-120.0 µg/mL for DOM and ESO, respectively. Limit of detection and limit of quantitation values were 0.48 and 1.44 µg/mL for DOM and 0.47 and 1.43 µg/mL for ESO, respectively. The method also exhibited good levels of recovery from 100.23% to 101.59% for DOM and from 99.74% to 101.57% for ESO. From the validation study, it was found that the method was specific, rapid, accurate and reproducible. The high percentage of recovery and low relative standard deviation confirm the suitability of the method for routine pharmaceutical analysis of both drugs separately or in their combined dosage form. Keywords: HPLC; Esomeprazole; Domperidone; Validation; Formulation.

The photostability of vitamin K1 (phylloquinone) in bulk powder and in its dosage form was studied according to the conditions suggested by ICH Guideline (option 2).  The results showed that the rate of Photodegradation of vitamin K1 follows first order kinetics and it is higher in its dosage form than in bulk powder. Attempts have been made to improve the photostability of vitamin K1 by combination with different photoprotective agents such as p-aminobenzoic acid (PAPA), tartaric acid, boric acid, citric acid, sodium benzoate, titanium dioxide (TiO2), zinc oxide (ZnO), propyl 4-hydroxybenzoate and methyl 4-hydroxybenzoate. The photodecompositions products were monitored by UV-Vis spectrophotometric method and HPLC. It was found that 0.01% PABA was the best photoprotective agent, which improved the photostability of vitamin K1 by 46 fold. The method was validated according to ICH guideline. The calibration graph was linear over the concentration range of 1.1× 10-5- 30.0 ×10-5 mol L-1. The limit of detection and the limit of quantification were 2.42 × 10-6 and 7.35 ×10-6 mol L-1, respectively.

High performance liquid chromatography for estimation of Sulbactam Sodium and Ampicillin Trihydrate in their combine dosage form was developed and validated. The method was performed on Younglin Instrument  with Autochro-3000 Operation software using Varian C-18 (250 Χ 4.6 mm i.d, 5 μm particle size column and Ammonium acetate Buffer : Acetonitrile: Water (75:17:08, %v/v/v)  as mobile phase at ambient temperature. Detection was carried out at 228 nm in the concentration range 25-125 µg/ml for Sulbactam Sodium and 50-250 µg/ml for Ampicillin Trihydrate. The percentage recovery of Sulbactam Sodium and Ampicillin Trihydrate was found to be 99.15 -100.16 and 98.91-103.48 respectively.. Correlation coefficient for Sulbactam Sodium and Ampicillin Trihydrate was found 0.997 and 0.999 respectively. The Rt values for Sulbactam Sodium and Ampicillin Trihydrate were found to be 4.0 min ±0.02 and 5.97 min ±0.03 respectively. The method can successfully applicable to routine analysis.  And under Statistical analysis, Paired t-test is applied for comparison between developed method and reported method where, we reject the null hypothesis, because value of t is less than 0.05 so we can conclude that there is significance difference between the developed method and reported method for Sulbactam Sodium and Ampicillin Trihydrate.

A rapid and simple HPLC method has been developed for the simultaneous quantification of safranal and piperine in some marketed proprietary Chyawanprash products. Analysis was performed using C18 column (250 x 4.6 mm) by isocratic elution with acetonitrile: water (77:23) and detection at 308 nm using Ultra Violet (UV) detector. The calibration plot was linear over the range studied (safranal: 0.5-10 ppm; piperine: 2.5-50 ppm) with a correlation of 0.999 for safranal and 0.999 for piperine. The method was also validated for the linearity, range, precision, recovery and detection limits. Thus, the method is suitable for routine analysis of safranal and piperine in marketed proprietary Chyawanprash products.

Levocetirizine dihydrochloride (LCD) and Ambroxol Hydrochloride (ABH) are two chemicals used for the treatment of upper respiratory tract diseases and elevation of allergy symptoms.  Few HPLC methods were reported for the estimation of LCD and ABH in bulk and in tablet dosage form without extraction.  The present work describes a simple, precise and accurate isocratic reversed-phase HPLC method that was developed and validated for the estimation of Levocetirizine dihydrochloride and Ambroxol hydrochloride in bulk and in tablet dosage form. The proposed RP-HPLC method was carried out using Intersil C8 column (5 mm, 25 cm, 4.6 mm i.d.). The mobile phase of water: acetonitrile mixture (50:50 v/v) was adjusted to pH 3.3 using ortho-phosphoric acid and applied at a flow rate of 1mL/min and 20 mL injection volume. The detection was achieved with UV at 225 nm. The retention time of ABH and LCD was 1.80 ± 0.01 min and 3.21 ± 0.07 min, respectively. The proposed method was validated for linearity, accuracy, precision, LOD and LOQ. The calibration plot was linear over the concentration range of 5-400 μg/ml for ABH and 1-35 μg/ml for LCD. The mean absolute recoveries for ABH and LCD were about 98.97 % and 100.8 %, respectively. From the validation study, it was found that the method was specific, rapid, accurate, sensitive, and reproducible.  The high recovery and low relative standard deviation confirm the suitability of the method for routine pharmaceutical quality control of both these drugs separately and in their combined dosage form.