STABILITY INDICATING RP-HPLC METHOD FOR SIMULTANEOUS DETERMINATION OF CEFTRIAXONE SODIUM AND SALBUTAMOL

An isocratic liquid chromatographic method with UV detection at 230 nm is described for simultaneous determination of ceftriaxone sodium and salbutamol in bulk. Chromatographic separation of the two drugs was achieved on an Inertsil ODS© C18 (250 × 4.6 mm, 5 μ) using a mobile phase consisting of 50 mM potassium dihydrogen orthophosphate and methanol (77:23 %V/V) adjusted to pH 7.0 with triethylamine at a fl ow rate of 1.0mL min-1. The optimum separation was achieved in less than 10 minutes. The developed liquid chromatographic method offers symmetric peak shape, good resolution and reasonable retention time for both drugs. The method was validated as per ICH guidelines.

METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS DETERMINATION OF AZELNIDIPINE AND TELMISARTAN IN TABLET DOSAGE FORM BY RP- HPLC

A simple, accurate and precise method for the simultaneous determination of azelnidipine and telmisartan in bulk drug and pharmaceutical dosage has been developed by RPHPLC method. Separation was performed on a Hyperchrom ODS C18 HPLC Column (250*4.6mm) column and Buffer 0.05M Potassium dihydrogen orthophosphate (KH₂PO₄) Buffer (pH-4.0): Methanol (60:40) as a mobile phase, at a flow rate 1ml/min and UV detection wavelength 215 nm. The calibration of the method was performed by concentration range of 20-60μg/ml for telmisartan and 40-120 μg/ml for azelndipine. The validation of proposed method was carried out for accuracy, precision, ruggedness, specificity for both alzenidipine and telmisartan the method can be used for routine quality analysis of titled drug in tablet formulation.

DEVELOPMENT OF LIQUID CHROMATOGRAPHIC METHOD FOR ESTIMATION OF ACAMPROSATE CALCIUM AND BACLOFEN COMBINATION USED IN TREATMENT OF NEUROLOGICAL DISORDERS

A specific, accurate, precise, and reproducible liquid chromatographic method has been developed and validated for the estimation of acamprosate calcium and baclofen in combination. The separation was achieved using stationary phase Phenomenex C18 column (150 mm× 4.6 mm.) in isocratic mode, with mobile phase containing 0.05 M potassium dihydrogen orthophosphate buffer (pH 7) : acetonitrile (10:90 V/V), at a flow rate of 1.0 mL/min and effluents were monitored at 210 nm. The retention time of acamprosate calcium and baclofen were found to be 1.9 min and 5.3 min, respectively. The linearity for acamprosate calcium and baclofen were in the range of 2-64 µg/mL and 1.2- 38.4 µg/mL, respectively. The method was validated as per ICH guideline. The recoveries of Acamprosate calcium and baclofen were found in the range of 98.90 - 100.13 % and 98.60 -100.02 %, respectively. The method was successfully applied for the determination of both the drugs in combination.

NOVEL RPHPLC-PDA METHOD FOR SIMULTANEOUS ESTIMATION OF HEPARIN AND ITS CO-ADMINISTERED DRUG (FENOFIBRIC ACID) IN MIXTURE

The poly prescription and co-administration of more than two drugs to treat patients for the disease conditions are inexorable. Heparin is and anticoagulant often administered with fenofibric acid in cardiac treatments. A reverse phased high-performance liquid chromatography method based on photo diode array detection has been developed for their simultaneous determination from admixture. They were separated using potassium dihydrogen orthophosphate: acetonitrile (20:80, V/V), on C18 column, at a flow rate of 0.8 mL/min. The retention time of Heparin and fenofibric acid was 3.8 and 13.1 min, respectively. The validation parameters were studied as per ICH guidelines to ascertain the validity of the method for the purpose intended. The linearity was observed between 0.5-3 I.U./mL of heparin and 0.25-1.5 µg/mL of fenofibric acid. The method was applied to a synthetically prepared admixture, and found to be satisfactorily resolving two drugs without any interference, with good precision and reproducibility in the established condition.

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF ESCITALOPRAM OXALATE AND FLUPENTIXOL DIHYDROCHLORIDE IN COMBINED DOSAGE FORM AND PLASMA

Objective: The objective of the study was to develop a simple and rapid chromatographic method for quantification of escitalopram oxalate and flupentixol dihydrochloride in combined dosage form and plasma. Methods: The separation was achieved with a sun fire C8 [150×4.6 mm] 3.5 µm column with an isocratic mobile phase containing a mixture of potassium dihydrogen orthophosphate buffer: methanol: acetonitrile [30:60:10 v/v/v] pH adjusted to 11. The flow rate of the mobile phase was 1.5 ml/min with a Photodiode array [PDA] detection at 230 nm. Results: The HPLC method was developed and validated with respective linearity, accuracy, and precision, detection of limit, robustness, and specificity. The precision of the results stated as the relative standard deviation was below 2 %. The calibration curve was linear over a concentration range from 10-50 µg/ml for escitalopram oxalate and 1-5 µg/ml for flupentixol dihydrochloride with a correlation co-efficient 0.994 and 0.977 respectively. The accuracy of the method was demonstrated at levels in the range of 100 % and 120 % of the specification limit. The recovery of escitalopram oxalate and flupentixol dihydrochloride was found to be in the range of 90 % to 88 %, respectively. The lowest detection limits were found to be 2 µg/ml for escitalopram oxalate and 0.1 µg/ml for flupentixol dihydrochloride. The lowest quantification limits were found to be 5 µg/ml of escitalopram oxalate and 0.5 µg/ml of flupentixol dihydrochloride. Conclusion: The developed method was validated for linearity, accuracy, precision, the limit of detection and quantification, specificity. The method was applied successfully for the determination of escitalopram oxalate and flupentixol dihydrochloride in the combined dosage form and plasma.

A Novel UPLC-PDA Stability Indicating Method Development and Validation for the Simultaneous Estimation of Lamivudine and Dolutegravir in Bulk and Its Tablets

Aim: To develop a stability indicating Rp-UPLC method for the simultaneous determination of Lamivudine, Dolutegravir and their degradants in tablets. Methodology: The chromatographic separation was performed on BEH Shield RP18 (2.1 mmX100 mmX1.7 mm) using a isocratic mobile phase Potassium dihydrogen orthophosphate pH 3 adjusted with orthophosphoric acid: methanol (30:70,% v/v) at a flow rate of 0.5ml/min. Column was maintained at room temperature and eluents are monitored at 258 nm. Results: Retention times of the analytes were found to be at 0.81 and 2.78 mins for Lamivudine and Dolutegravir respectively. The calibration of peak area versus concentration, which was linear from 105 to 315 µg/ml for Lamivudine and 17.5 to 52.5 µg/ml for Dolutegravir, had regression coefficient (r2) greater than 0.999. The method had the requisite accuracy, precision and robustness for simultaneous determination of Lamivudine and Dolutegravir in tablets. Conclusion: The proposed method is simple, economical, accurate, precise and can be successfully employed in routine quality control for the simultaneous analysis of Lamivudine and Dolutegravir in pharmaceutical formulations.

A Versatile Stability-indicating Liquid Chromatographic Method for the Simultaneous Determination of Atenolol, Hydrochlorothiazide and Chlorthalidone

Background: Atenolol is a selective beta 1 blocker that can be used alone or in combination with hydrochlorothiazide or with chlorthalidone for the treatment of hypertension and prevention from a heart attack. Objective: The main target of this work was to improve modern, easy, accurate and selective liquid chromatographic method (RP-HPLC) for the determination of these drugs in the presence of their degradation products. These methods can be used as analytical gadgets in quality control laboratories for a routine examination. Methods: In this method, the separation was accomplished through an Inertsil® ODS-3V C18 column (250 mm x 4.6 mm, 5 μm), the mobile phase used was 25 mM aqueous potassium dihydrogen orthophosphate solution adjusted to pH 6.8 by using 0.1M sodium hydroxide and acetonitrile (77 : 23, v/v), the flow rate used was 1 ml/min and detection was achieved at 235 nm using UV. Results: All peaks were sharp and well separated, the retention times were atenolol degradation (ATN Deg.) 2.311 min, atenolol (ATN) 2.580 min, hydrochlorothiazide degradation (HCT Deg.) 5.890 min, hydrochlorothiazide (HCT) 7.016 min, chlorthalidone degradation CTD Deg 8.018 min and chlorthalidone (CTD) 14.972 min. Linearity was obtained and the range of concentrations was 20- 160 μg/ml for atenolol, 10-80 μg/ml for hydrochlorothiazide and 10-80 μg/ml for chlorthalidone. According to ICH guidelines, method validation was accomplished, these methods include linearity, accuracy, selectivity, precision and robustness. Conclusion: The optimized method demonstrated to be specific, robust and accurate for the quality control of the cited drugs in pharmaceutical dosage forms.

Study growth and characterization of chloride doped potassium dihydrogen orthophosphate crystal

Potassium dihydrogen phosphate (KDP) crystal has been doped with chloride to alter its physical and chemical properties.The pure and chloride mixtured KDP was grown by slow evaporation solution growth technique. The X-raydiffractometry (XRD) analys is shows that the crystalline perfection these optimum conditions is extremely good without having any internal structural grain boundaries and mosaic nature. The lattice parameters have been determined for pure KDP and chloride mixtured KDP from the single crystal XRD. The crystals grown by these optimum conditions show positive effects in the various characterization techniques.

A Study on Spectral and Morphological Analysis on Unidirectional Neodymium Doped KDP Single Crystal

A nonlinear optical unidirectional <101> Single crystal of Neodymium doped Potassium dihydrogen orthophosphate (KDP) was grown by Sankaranarayanan-Ramasamy (SR) method. The <101> oriented seed crystals were mounted at the bottom of the glass ampoule and the crystal of 16mm diameter; 120mm length were grown by SR method. The laser damage threshold was measured using Q-switched Nd:YAG laser (1064 nm) and was found to be 5.456 Gwcm-2 respectively.The presence of functional groups was examined by Fourier transform infrared (FTIR) analysis. The surface morphology and dislocations along <101> plane was observed using Scanning electron microscope (SEM) and Transmission electron microscope (TEM).

Synthesis, Characterization, Thermal, NLO and Quantum-Chemical Studies on N-Acetyl-2,6-bis(4-methoxyphenyl)-3-ethylpiperidin-4-one

Growth of a new organic single crystal of N-acetyl-2,6-bis(4-methoxyphenyl)piperidin-4-one (APM3EPO) is reported by using a slow evaporation method. The characterization of the crystal was done by IR and NMR spectra. Further, electronic spectrum and TG/DTA studies have also been carried out. The SHG efficiency of the crystal was found to be closer to that of standard KDP (potassium dihydrogen orthophosphate) using the modified Kurtz-Perry powder test employing Nd: YAG laser as the source of IR radiation. The calculated hyperpolarizability values were also projected to confirm the aptness of the crystal for non-linear optical applications. Optimization of the molecular structure of APM3EPO is done at the basic level of B3LYP/6-311(d,p) and the corresponding molecular properties such as HOMO-LOMO and Mulliken charge analyses are carried out at the same level of theory.