ABSTRACT
A novel stability-indicating Reverse Phase High Pressure Liquid Chromatography (RP-HPLC-PDA) method was developed and validated for quantitative determination of Camptothecin (CPT) in bulk, formulation and in dissolution samples using Inertsil-C18 (250mm x 4.6mm, 5μm) column with mobile phase combination of 15mM Ammonium acetate and acetonitrile (60:40) at a flow rate of 1mL/min. Eluents were monitored at a wavelength of 254 nm with an injection volume of 20µL. CPT was completely degraded in oxidative and base hydrolysis conditions and around 37% in acidic conditions and no degradation of CPT was observed with thermal, thermal/humidity and photo conditions. CPT showed linearity over a concentration range of 2-10μg/mL with a regression coefficient (R2) of 0.994 and correlation coefficient (R) of 0.999. The limit of detection (LOD) and limit of quantification (LOQ) values for CPT were 0.025μg/mL and 0.077μg/mL respectively. The developed method was validated as per ICH guidelines. The method was also successfully applied to dissolution testing of controlled release formulation.
ABSTRACT
The aim of the present investigation is to develop enteric coated sustained release matrix tablets of Sertraline hydrochloride (STH) using HPMC K4M and Carbopol-971 as drug release retardants and cellulose acetate phthalate (CAP) as an enteric coat polymer. The tablets were prepared by direct compression process and evaluated for various physico-chemical/mechanical parameters. Among the two release retardants, HPMC K4M was selected based on controlling the STH release during dissolution. The effect of different fillers like microcrystalline cellulose (MCC), di calcium phosphate (DCP), spray dried lactose with maize starch (SDL) and pre gelatinized starch (PGS), on STH release was also studied. The percent of STH released at the end of dissolution with different fillers is in the order of SDL > MCC > DCP > PGS. The tablets containing 15% w/w of HPMC K4M & MCC as filler with 5% coating weight gain (1% v/v glycerine in 5%w/v CAP solution) gave a STH release of less than 10% in 0.1N HCl (pH 1.2) for 2 h and a sustained release of STH over a period of 12 h (99.17±0.54%) in pH 6.8 phosphate buffer and fulfilled the regulatory requirements. The dissolution data was also evaluated for drug release kinetics and mechanisms.
ABSTRACT
Aim: The aim of the present investigation was to perform the precolumn derivatization of Amantadine Hydrochloride (AMT) with phenylisothiocyanate and to develop a RP-HPLCPDA method for the quantification of Amantadine Hydrochloride-phenylisothiocyanate (AMT-PITC) complex in bulk and dosage forms which is rapid, sensitive and economical. Study Design: Method development and Validation study. Methodology: A Phenomenex C18 RP column of 250 x 4.6mm dimensions and 5μm particle size with mobile phase containing water and acetonitrile (40:60% v/v) was used at isocratic mode binary pump and eluent was monitored at 273nm. Results & Discussion: The retention time of AMT-PITC complex was 6.3 min. The developed method showed a good linearity in the concentration range of 10-50μg/mL with a correlation coefficient >0.998. The recoveries ranged between 95-105% with a Relative Standard Deviation of (RSD) < 2%. Conclusion: The developed method was validated as per ICH guidelines and successfully used for quantification of AMT by derivatization with PITC. The method was found to be rapid, specific and accurate.
ABSTRACT
The present investigation was undertaken with an objective of formulating mouth dissolving films (MDFs) of an anti-migraine drug, Sumatriptan Succinate (SUM) to enhance convenience and compliance to the elderly and pediatric patients for better therapeutic efficacy. Film former, Hydroxy Propyl Methyl Cellulose along with film modifier/solubilizing agents, Polyvinyl pyrrolidone K30 (PVP K30) and Sodium Lauryl Sulphate (SLS) were used to formulate MDFs. The MDFs were prepared by wet film applicator technique and were evaluated for in vitro dissolution characteristics, in vitro disintegration time, and their physico-mechanical properties. MDFs with 13% (w/w) of HPMC E5 gave better dissolution properties when compared to HPMC E15. MDFs with PVP K30 and SLS gave superior dissolution properties when compared to MDFs without PVP K30 and SLS. The dissolution properties of MDFs with PVP K30 were superior when compared to MDFs with SLS. Overall, SUM MDFs showed good mechanical properties like tensile strength, folding endurance and % elongation and dissolution properties. These results suggest that the HPMC is an excellent film former which gives rapid drug release.
ABSTRACT
The aim of the present work was to develop and validate a simple, efficient, economical and LC-MS compatible method for the analysis of Terbutaline sulphate in bulk, dosage forms and in dissolution samples of Terbutaline sulphate tablets by reverse phase high pressure liquid chromatography. A C18 reverse phase column (Phenomenex) of 250 x 4.6mm dimensions and 5μm particle size with mobile phase containing 15mM ammonium acetate: methanol (70:30% v/v) was used at isocratic mode binary pump and eluents were monitored at 220nm. The retention time of Terbutaline sulphate was 4.1min and showed a good linearity in the concentration range of 2-10μg/mL with a correlation coefficient >0.999. The validation characteristics included specificity, linearity, and limit of detection, limit of quantification, precision, robustness and stability. Validation acceptance criteria were met in all cases. The percent recoveries ranged between 98-102%, RSD < 2%. The method could be successfully used for the analysis of Terbutaline sulphate in bulk, dosage forms and in dissolution samples of marketed Terbutaline sulphate tablets.
ABSTRACT
Valsartan (VAL) is a potent, highly selective and orally active antihypertensive drug and is poorly soluble in aqueous fluids, especially in gastric fluids, and its absorption is thus dissolution rate limited. In the present research work an attempt has been made to improve the aqueous solubility of VAL by the recrystallization of VAL from a variety of different organic solvents, and evaluating the recrystallized VAL products for its physicochemical characteristics and in-vitro dissolution properties. The water solubility of methanol (MET), ethanol (ETH), isopropanol (ISP) and acetonitrile (AN) recrystallized products of VAL is significantly higher when compared to untreated VAL. Physicochemical characterization techniques like scanning electron microscopy, differential scanning calorimetry, powder X-RD reveal the change in crystallinity of VAL with recrystallized products and hence the increase in the solubility and superior dissolution properties when compared to the untreated VAL.
ABSTRACT
The present investigation was undertaken with an objective of formulating modified release (MR) matrix tablets of Oxcarbazepine (OXC) an anti-epileptic drug, based on cellulose ether polymers like Hydroxy Propyl Methyl Cellulose (HPMC K4M and LVCR 100) and Hydroxy Propyl Cellulose (HPC JF) as drug release retardants to overcome poor patient compliance and exposure to high doses associated with currently marketed immediate release (IR) dosage forms. The tablets were prepared by direct compression process and evaluated for various physico- chemical/mechanical parameters. Among three polymers used, HPMC LVCR 100 is selected as release retardant based on the viscosity and gel formation during dissolution. The effect of different fillers like Avicel PH 101, Avicel PH 105, Pre gelatinized starch (PGS), maize starch with spray dried lactose (FLOWLAC) and Di-calcium phosphate (DCP) on OXC release was also studied and the OXC percent release at the end of 12h is in the order of DCP>FLOWLAC>Avicel PH 101>Avicel PH 105>PGS. Based on the dissolution data obtained with different fillers and keeping in view of the results from the pre compression studies, and gel layer retaining with the matrix tablets, Avicel PH 105 was selected as carrier to carry out further formulation development. Since, OXC is poorly water soluble drug, solubilizing agents like surfactants, cyclodextrins and polyethylene glycols were included in the formulations and their effect on OXC release was studied in order to achieve therapeutic effective levels. Formulations containing 20% (w/w) of Hydroxy Propyl-β-Cyclodextrin gave superior OXC release of 85.50 ± 1.62% at the end of 12hours and fulfils the regulatory requirement. The dissolution data was also evaluated for drug release kinetics and mechanisms.
ABSTRACT
A simple, specific, and accurate reverse phase liquid chromatographic method was developed for the estimation of Tizanidine (TZN) and Baclofen (BCF) in combination. A Phenomenex -C18 (150×4.60 mm Dimensions, 5μm Particle size) column with mobile phase containing methanol: water (53:47) was used at isocratic mode and eluents were monitored at 228 nm. The retention times of TZN and BCF were 2.03 and 4.1min respectively and both the drugs showed good linearity in the concentration range of 10-50 μg/mL with a correlation coefficient (R) of 0.9992 and 0.9993 respectively. The proposed method was validated as per ICH guidelines and method showed good precision with percent relative standard deviation less than 2%. The percentage assay values of TZN and BCF were found to be 99.72 and 98.56 respectively and recovery values are within the limits of 98-102% indicating the proposed method was accurate and precise for the simultaneous estimation of TZN and BCF in bulk and pharmaceutical dosage forms.
ABSTRACT
The study describes development and subsequent validation of an RP-HPLC-PDA method for the simultaneous estimation of Tamsulosin (TAM) and Finasteride (FIN) in bulk and tablet dosage form. The chromatographic conditions comprised of a reversed-phase C18 column (150 x 4.6 mm, 5 μ) with a mobile phase consisting of a mixture of methanol and formic acid (0.02% v/v in water) at a flow rate of 1 mL/min and ran in gradient mode. Detection was carried out at 230 nm. The retention times were 2.7 min and 10.08 min respectively for TAM and FIN. A good linear relationship in the concentration range 0.4-20μg/mL with a correlation coefficient of 0.9981 for TAM and in the range of 5-50μg/mL a correlation coefficient of 0.9987 was observed. Limit of detection (LOD) was found to be 0.16μg/mL for TAM and 0.6μg/mL for FIN. The method was validated for accuracy, precision, robustness and assay. The percent recovery values were in the ranges of 99.15-100.8 for TAM and 99.21-101.83 for FIN. The results of all the validation parameters were well within their acceptance values.