DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF SOFOSBUVIR AND LEDIPASVIR IN TABLET DOSAGE FORM

Simple, specific, accurate and precise reversed phase high pressure liquid chromatographic method has been developed for the simultaneous determination of Sofosbuvir and Ledipasvir in tablet dosage form by reversed phase C18 column (Kromasil C18 5μ, 250 mm x 4.6 mm). The sample was analyzed using 0.1% OPA: Acetonitrile in the ratio of 55:45 as a mobile phase at a flow rate of 1.0 ml/min and detection at 230 nm. Calibration curves were linear with correlation coefficient (r2 ) 0.999 over a concentration range of 100-600 µg/mL for Sofosbuvir and 0.999 over a concentration range of 22.5-135 µg/mL for Ledipasvir. The retention time was found to be 6 min. The mean recoveries were found to be 99.10% and 99.30% for Sofosbuvir and Ledipasvir respectively. The relative standard deviation (RSD) was found to be < 2.0% for both drugs. The proposed method was validated and successfully applied to the estimation of Sofosbuvir and Ledipasvir in tablet dosage form. Keywords: Sofosbuvir, Ledipasvir, RP-HPLC, Validation, Stability

Bioanalytical Method Development and Validation of Memantine in Human Plasma by High Performance Liquid Chromatography with Tandem Mass Spectrometry: Application to Bioequivalence Study

A simple, sensitive, and rapid HPLC-MS/MS method was developed and validated for quantitative estimation of memantine in human plasma. Chromatography was performed on Zorbax SB-C18 (4.6 × 75 mm, 3.5 μm) column. Memantine (ME) and internal standard Memantine-d6(MED6) were extracted by using liquid-liquid extraction and analyzed by LC-ESI-MS/MS using multiple-reaction monitoring (MRM) mode. The assay exhibited a linear dynamic range of 50.00–50000.00 pg/ml for ME in human plasma. This method demonstrated an intra- and interday precision within the range of 2.1–3.7 and 1.4–7.8%, respectively. Further intra- and interday accuracy was within the range of 95.6–99.8 and 95.7–99.1% correspondingly. The mean recovery of ME and MED6 was 86.07 ± 6.87 and 80.31 ± 5.70%, respectively. The described method was successfully employed in bioequivalence study of ME in Indian male healthy human volunteers under fasting conditions

Bio-analytical method development and validation of Rasagiline by high performance liquid chromatography tandem mass spectrometry detection and its application to pharmacokinetic study

The most suitable bio-analytical method based on liquidâliquid extraction has been developed and validated for quantification of Rasagiline in human plasma. Rasagiline-13C3 mesylate was used as an internal standard for Rasagiline. Zorbax Eclipse Plus C18 (2.1 mmÃ50 mm, 3.5 μm) column provided chromatographic separation of analyte followed by detection with mass spectrometry. The method involved simple isocratic chromatographic condition and mass spectrometric detection in the positive ionization mode using an API-4000 system. The total run time was 3.0 min. The proposed method has been validated with the linear range of 5â12000 pg/mL for Rasagiline. The intra-run and inter-run precision values were within 1.3%â2.9% and 1.6%â2.2% respectively for Rasagiline. The overall recovery for Rasagiline and Rasagiline-13C3 mesylate analog was 96.9% and 96.7% respectively. This validated method was successfully applied to the bioequivalence and pharmacokinetic study of human volunteers under fasting condition. Keywords: High performance liquid chromatography, Mass spectrometry, Rasagiline, Liquidâliquid extractio

Design and invitro evaluation of gastro retentive oral matrix tablet formulations of ketorolac tromethamine

Ketorolac Tromethamine floating tablets were prepared by using combination of hydrophilic polymers such as Hydroxy Propyl Methyl Cellulose 4000 cps grade and 100000 cps grade. Eight set of formulations were prepared by gradual increasing and decreasing concentrations of above two polymers. The floating pattern was found to be instant for all the formulations and best controlled release profile was achieved for few set of formulations. The drug content, tablet weight, friability and weight variation were found to be within the limits. Validated UV spectrophotometric method was developed and standard linear regression was used to determine the concentration of released drug during the course of dissolution. The release studies were subjected to zero order, first order, higuchi and ritger-peppas kinetics and the parameters for controlled release were calculated

Synthesis, Characterization and Anti-Microbial Activity of Novel Pyramidine Derivatives

Pyrimidine is a heterocyclic aromatic organic compound similar to benzene and pyridine, containing two nitrogen atoms at positions 1 and 3 of the six-member ring. Three nucleobases found in nucleic acids, cytosine (C), thymine (T), and uracil (U), are pyrimidine derivatives. A pyrimidine has many properties in common with pyridine, as the number of nitrogen atoms in the ring increases the ring pi electrons become less energetic and electrophilic aromatic substitution gets more difficult while nucleophilic aromatic substitution gets easier. Chalcones react with aminoguanidine to give intermediate compounds which on further reacts with substituted ketones to give Pyramidine derivatives. A total of 6 compounds were synthesized from one scheme and they were recrystallized by appropriate solvents. They were identified and characterized by various spectral methods. In the present study, all synthesized compounds tested for anti bacterial activity and anti-fungal activity. They shown significant activity when compared with standard drug Streptomycin and Miconazole respectively. Keywords: Pyramidines, Characterization, Streptomycin, Miconazole, Anti-microbial activity

Innovative cervical splint: overcoming an obstacle

Cervical splints are used to maintain the neck position in burn patients with involvement of neck, which provides pain relief and prevent hypertrophic scarring and contracture. Due to the technical difficulty, cervical splinting often deferred in patients with tracheostomy. To overcome the difficulty the authors have described a simple modification of hard cervical collar, which provided adequate immobilization and adequate space for tracheostomy care. Innovative modification of hard cervical collar proposed in this case report can be a solution to overcome the difficulty posed by tracheostomy in patients sustained with neck burns

Autologous platelet rich plasma - an adjunct to early tangential excision and grafting in burns

Aim: To affirm that autologous platelet rich plasma is a useful adjunct to early tangential excision and skin grafting to enhance wound epithelization rates and improve scar quality.Methods: The study was conducted in JIPMER Tertiary Burn Care Centerfrom November 2017 to February 2018. The study was purely descriptive in nature and no statistical analysis was performed. A total of 12 patients were included with burn wounds involving 10% to 25% total body surface area.Results: There was 100% epithelization noted at the end of 2 weeks for all the 12 participants. Skin graft take was faster with mean 85.4% take for all the 12 patients within 5 days.Conclusion: Since it is an autologous component, platelet rich plasma is extremely safe and free of antigenic components. It is relatively simple to prepare, less time taking, cost effective and highly efficacious in improving wound healing and improving the efficacy of the traditional techniques like tangential excision and skin grafting in burn patients

Low level laser as an adjunct therapy for second degree superficial burns

Aim: Second degree superficial burns are painful and heal over a period of two to three weeks time. Multimodality treatment approach is effective in reducing time of healing, pain, rate of complications and overall cost of treatment. Aim of this study is to observe effect of low level laser therapy (LLLT) as an adjunct to conventional therapy for second degree superficial burn.Methods: This article presents a case series of twenty patients in which LLLT was used as an adjunct therapy for target burn areas.Results: Average time taken for complete healing of areas with second degree superficial burns was 11.75 (SD 2.86) days. One patient was healed on day 6; ten patients were healed on day 10, six patients on day 13, and three on day 17.Conclusion: We could not found significant evidence of positive effect of LLLT over rate of wound healing. However its effects are promising and further large multicentric trials are needed to establish its role and standardize its dose parameters

Role of newer technologies in wound bed preparation in Fournier’s gangrene

Fournier’s gangrene or necrotizing fasciitis of the perineum scrotum and penis is a highly debilitating condition with a high mortality rate of 20% to 88% reported in the literature. Management is multimodal, and the importance of aggressive debridement, broad-spectrum antibiotics and intensive supportive care cannot be emphasised. The addition of newer modalities of ulcer/wound management like low level laser therapy, hydrojet debridement and platelet rich plasma can be used to augment the existing principles of management and reduce the morbidity and mortality associated with the condition. This article is the authors’ experience with the condition and the above stated newer modalities in the management while staying true to the principles of management

Estimation of Rabeprazole Sodium and Itopride Hydrochloride in Tablet Dosage Form Using Reverse Phase High Performance Liquid Chromatography

A reversed phase high performance liquid chromatography (RP-HPLC) method was developed, validated and used for the quantitative determination of rabeprazole sodium (RP) and itopride hydrochloride (IH), from its tablet dosage form. Chromatographic separation was performed on a Phenomenex C18 column (250 mm × 4.6 mm, 5 μm), with a mobile phase comprising of a mixture of 50 mM ammonium acetate buffer and methanol (20:80v/v), pH 4.5 adjusted with acetic acid, at a flow rate of 1.3 mL/min with detection at 286 nm. Separation was completed in less than 10 min. As per International Conference on Harmonization (ICH) guidelines the method was validated for linearity, accuracy, precision, limit of quantitation and limit of detection. Linearity of RP was found to be in the range of 37.5-375 μg/mL and IH was found to be in the range of 5-50 μg/mL. The correlation coefficients were 0.9997 and 0.9995 for RB and IH respectively. The accuracy of the developed method was found to be 98.6-100.7 for RP and 99.42 -100.81 for IH. The experiment shows the developed method is free from interference of excipients. It indicates the developed RP-HPLC method is simple, linear, precise and accurate and it can be conveniently adopted for the routine quality control analysis of the tablet dosage form