Eco-Friendly Stability Indicating HPLC Method for Estimation of Elbasvir and Grazoprevir by Quality by Design Approach

Introduction: The pharmaceutical industry faces a significant problem as a result of the worldwide requirement to modify processes in order to comply with the green analytical chemistry (GAC) requirements. An enormous amount of organic hazardous waste is produced by high-performance liquid chromatography (HPLC), one of the methods employed the most frequently at different stages in the pharmaceutical sector. Aim: To develop analytical quality by design-aided stability indicating green high-performance liquid chromatography (HPLC) method for estimation of Elbasvir and Grazoprevir in a dosage form. Material and Methods: The critical chromatographic factors were the % of ethanol in the mobile phase, flow rate, and their overall effect on the responses like asymmetry, theoretical plates, and resolution were studied to optimize the method. Green analytical chemistry (GAC) has mainly focused on developing analytical methods that are safe for the environment. Therefore, it is imperative that the GAC principles be applied in pharmacological analysis. A rotatable central composite design was employed, and the optimized conditions for chromatographic separation were made with a run time of 5 minutes using Zorbax C18 column (4.6× 150 mm, 5 µm) with 0.1% Trifluoroacetic acid and ethanol (40:60 v/v) as components of a mobile phase, flowing at a rate of 1.0 ml/minute. Photodiode array detection was carried out at 253 nm. Results: The retention time was 1.8 min for EBS and 2.84 min for GZP. According to the ICH guidelines, the proposed method was validated and stress studies revealed that Elbasvir and Grazoprevir are prone to acidic, basic, and oxidation stress conditions. An analytical eco-scale score evaluated the greenness profile and a software-based evaluation. Conclusion: The developed HPLC method is eco-friendly and shall be adopted   in the routine quality control of Elbasvir and Grazoprevir in a tablet dosage form

Polymorphs of Curcumin and Its Cocrystals With Cinnamic Acid

YesWe report formation of polymorphs and new eutectics and cocrystals of curcumin, a sparingly water-soluble active component in turmeric, structurally similar to cinnamic acid. The curcumin polymorphs were formed using liquid antisolvent precipitation, where acetone acted as a solvent and water was used as the antisolvent. The metastable form 2 of curcumin was successfully prepared in varied morphology over a wide range of solvent-to-antisolvent ratio and under acidic pH conditions. We also report formation of new eutectics and cocrystals of curcumin with cinnamic acid acting as a coformer. The binary phase diagrams were studied using differential scanning calorimetry and predicted formation of the eutectics at the curcumin mole fraction of 0.15 and 0.33, whereas a cocrystal was formed at 0.3 mole fraction of curcumin in the curcumin–cinnamic acid mixture. The formation of the cocrystal was supported with X-ray powder diffraction, the enthalpy of fusion values, Fourier-transform infrared spectroscopy, and scanning electron microscopy. The hydrogen bond interaction between curcumin and cinnamic acid was predicted from Fourier-transform infrared spectra, individually optimized curcumin and cinnamic acid structures by quantum mechanical calculations using Gaussian-09 and their respective unit cell packing structures

Vacuum pyrolysed biochar for soil amendment

Biochar, a highly carbonaceous charred organic material obtained from biomass conversion can be deliberately applied as a conditioner/ amender in order to improve soil quality and associated environmental services. Napier grass (Pennisetum purpureum), a lignocellulosic biomass, can potentially be used to produce biochar. The aim of the present work is to manufacture, comprehensively characterize, and apply biochar obtained from the vacuum pyrolysis and investigate its potential for soil amendment. Biochar produced from Napier grass was characterized for its pH, electrical conductivity, soil water retention capacity, surface acidity and/or basicity, elemental composition, Infrared spectra, X-ray diffraction spectra, surface area, porosity, soil-water relation and morphological properties. Experiments on the methylene blue adsorption of the biochar indicated an equilibrium uptake capacity of 35 mg.g−1 and showed good agreement with the Langmuir-Freundlich model. Kinetic studies revealed Lagergren pseudo-first-order fit with intra-particle diffusion appearing to be one of the rate controlling mechanisms. Pot trials with Cicer grown in neutral and acidic soil amended with biochar validated that biochar augmented plant growth in terms of enhanced biomass weight and number of seed germinations. The entire investigation revealed that the properties of the produced biochar are in line with those necessary for it to act as a suitable agent for soil amendment

Rapid and sensitive High-Performance Thin-Layer Chromatographic (HPTLC) method for identification and quantification of luteolin by densitometry in Kasamarda (Cassia occidentalis L.)

Kasamarda (C. occidentalis L.) is a traditional herb recently recognized as a potential nutraceutical in bone health. The current botanical nutraceutical regulations require consistent standardization for biological applications. The present study reported the standardization of bioactive flavonoid luteolin from Cassia occidentalis L. using validated high-performance thin-layer chromatographic (HPTLC) densitometric (DS) method. The mobile phase composition of toluene, ethyl acetate, and formic acid was optimized to separate and identify luteolin using silica gel 60F254 aluminum plates. The densitometric (DS) scanning was performed at 353 nm. This HPTLC-DS method was further validated as per ICH guidelines. The linearity was 200–700 ng/band with a correlation coefficient value of 0.994. The LOD and LOQ were found to be 54.06 ng/band and 163.84 ng/band, respectively. The recovery (88.38% and 100.72%) and precision (RSD,<5%) indicated method performance is robust and accurate for the routine analysis. Further, this bioactive flavonoid presence was confirmed and quantified by UV-spectrumin the sample matrix using this validated HPTLC-DS method. This HPTLC-DS method was robust, precise and accurate for quality control of active constituents present in C. occidentalis L

Comparison of urodynamic parameters with respect to neurological levels in post-traumatic spinal cord injury patients

Background: Urodynamic evaluation is mandatory in order to correctly assess and classify bladder dysfunction in spinal cord injury (SCI) patients. Study investigated patterns of neurogenic bladder dysfunction in patients with post traumatic spinal cord injury and assessed the relationship of detrusor leak point pressure with compliance, post void residual urine volume and maximum cystometric capacity.Methods: Eighty six patients with neurogenic bladder secondary to traumatic spinal cord injury (SCI) underwent cystometry with electromyography (EMG). T-test was used to compare detrusor leak point pressure (LPP) between complete and incomplete injury groups. Pearson correlation test was used to seek correlation between detrusor LPP and compliance, post void residual volume (PRV) and maximum cystometric capacity (MCC).Results: Mean detrusor LPP in suprasacral complete injury group, suprasacral incomplete injury group and sacral complete injury was 52±21 cm of H2O, 53±18 cm of H2O and 16±9 cm of H2O respectively. No significant difference in detrusor LPP was found between suprasacral complete and incomplete group on t-Test (p= 0.571068). Significant difference in detrusor LPP was found between suprasacral and sacral group (p= 5.71891E-12). Mean compliance in sacral injury group was 24±16 and in suprasacral complete injury group was 5±6. Mean compliance in suprasacral incomplete injury group was 4±2. Pearson correlation showed negative correlation (r = -0.6918934) between detrusor leak point pressure and compliance (p= 1.2744E-13). Negative correlation (r = -0.311409922) was observed between detrusor leak point pressure and post leak/ void residual urine volume (p= 0.003335033) and between detrusor LPP and maximum cystometric capacity (r = -0.31354), (p= 0.003115).Conclusions: Significant difference in urodynamic parameters exists between sacral and suprasacral injury patients. However there is no significant difference in urodynamic parameters between complete and incomplete injury at suprasacral level

Rapid and sensitive High-Performance Thin-Layer Chromatographic (HPTLC) method for identification and quantification of luteolin by densitometry in Kasamarda (Cassia occidentalis L.)

700-706Kasamarda (C. occidentalis L.) is a traditional herb recently recognized as a potential nutraceutical in bone health. The current botanical nutraceutical regulations require consistent standardization for biological applications. The present study reported the standardization of bioactive flavonoid luteolin from Cassia occidentalis L. using validated high-performance thin-layer chromatographic (HPTLC) densitometric (DS) method. The mobile phase composition of toluene, ethyl acetate, and formic acid was optimized to separate and identify luteolin using silica gel 60F254 aluminum plates. The densitometric (DS) scanning was performed at 353 nm. This HPTLC-DS method was further validated as per ICH guidelines. The linearity was 200–700 ng/band with a correlation coefficient value of 0.994. The LOD and LOQ were found to be 54.06 ng/band and 163.84 ng/band, respectively. The recovery (88.38% and 100.72%) and precision (RSD,<5%) indicated method performance is robust and accurate for the routine analysis. Further, this bioactive flavonoid presence was confirmed and quantified by UV-spectrumin the sample matrix using this validated HPTLC-DS method. This HPTLC-DS method was robust, precise and accurate for quality control of active constituents present in C. occidentalis L