Quantification and Stability Indicating Method Development and Validation of Vismodegib in Bulk and Pharmaceutical Dosage Form by Ultra Performance Liquid Chromatography

Background: Vismodegib (VMD) is a drug of choice for the treatment of basal-cell carcinoma. Present studies carried out to estimate VMD by RP-UPLC technique and to develop a simple, précised, accurate method for routine analysis. Methods: For this purpose Chromatographic conditions used were stationary phase STD BEH C18 column (100 mm x 2.1 mm, 1.8m), a mixture of Methanol:KH2PO4 taken in the ratio 50:50%v/v as a mobile phase with a pH 7.4 and flow rate was maintained at 0.3ml/min, detection wave length was Acquity TUV 254nm, column temperature was set to 30oC and diluent was mobile phase, Conditions were finalized as optimized method. Results: System suitability parameters were studied by injecting the standard six times. Linearity study was carried out between 25% to150% (37.5-225µg/ml) levels, R2 value was found to be as 0.9992. Precision was found to be 0.6 for repeatability and 0.4 for intermediate precision. LOD and LOQ are 0.33 µg/ml and 0.99 µg/ml respectively and results were well under the acceptance criteria. Conclusion: By using above method assay of marketed formulation was carried out and was found 100.12%. Degradation studies of VMD were done, in all conditions purity threshold was more than purity angle and within the acceptable range. The developed method was simple and can be used for routine analysis.

Structure, Bioactivity and Analytical Methods for the Determination of Yucca Saponins

Yucca is one of the main sources of steroidal saponins, hence different extracts are commercialized for use as surfactant additives by beverage, animal feed, cosmetics or agricultural products. For a deeper understanding of the potential of the saponins that can be found in this genus, an exhaustive review of the structural characteristics, bioactivities and analytical methods that can be used with these compounds has been carried out, since there are no recent reviews on the matter. Thus, a total of 108 saponins from eight species of the genus Yucca have been described. Out of these, the bioactivity of 68 saponins derived from the isolation of Yucca or other genera has been evaluated. Regarding the evaluation and quality control of the saponins from this genus LC-MS technique is the most often used. Nevertheless, the development of methods for their routine analysis in commercial preparations are needed. Moreover, most of the studies found in the literature have been carried out on Y. schidigera extract, since is the most often used for commercial purposes. Only eight of the 50 species that belong to this genus have been studied, which clearly indicates that the identification of saponins present in Yucca genus is still an unresolved question.

UV Spectrophotometric Method Development and Validation of Dasatinib in Bulk and Formulation

UV-Spectrophotometric method has been developed and validated for quantitative estimation of dasatinib in bulk and pharmaceutical formulation. Dasatinib is soluble in acetonitrile, so it was used as solvent. Dasatinib was dissolved in acetonitrile and resulting solution was scanned in UV range (200-400nm). The λmax was found to be 315nm. Beers law is valid in concentration range of 5-25µg/ml. The developed method was validated for linearity, accuracy, precision, robustness; LOD and LOQ. Linearity was obtained in the range of 5-25µg/ml with correlation coefficient 0.9992. LOD and LOQ were found to be 0.908µg/ml and 2.752µg/ml respectively. The method showed good reproducibility and recovery so; proposed method can be applied for routine analysis of dasatinib in bulk and pharmaceutical formulation.

Analytical Method Development and Validation of Prucalopride Succinate in Bulk and Formulation by UV-Visible Spectrophotometry

Purpose: Analytical method development and validation for the quantitative determination of Prucalopride succinate in bulk and tablet formulation which plays major role in the development and manufacture of pharmaceuticals. Methods: In the present work a simple, rapid and reproducible UV-Visible Spectrophotometric method was developed and validated according to ICH guidelines. Results and Conclusions: The parameters linearity, specificity, precision, accuracy, and robustness were studied. The wavelength 243nm was selected for the estimation of drug using methanol as a solvent. The drug obeys Beer-lambert’s law over the concentration range 2-10μg/ml. The accuracy of the method was assessed by recovery studies and was found between 97.2- 98.3 %. The method was successfully applied for routine analysis of Prucalopride succinate in bulk and formulation.

A new and ecological miniaturized method by spectrophotometry for quantification of vancomycin in dosage form

Vancomycin, an important antibiotic, is marketed as lyophilized powder. In the context of routine analysis of this product, the existence of a more advantageous and effective method is interesting. Thus, the objective of this work is to develop and validate a new analytical method, faster, low-cost, ecological and miniaturized for quantification of vancomycin in lyophilized powder using spectrophotometry in ultraviolet region. Buffer solution pH 6.8, quartz cuvette with capacity of 700 µL and 280 nm were chosen. The method proved to be linear in the range of 50-150 µg/mL (0.9997). The selectivity of the method was proven in two ways: The standard-sample overlay aimed to identify vancomycin in the sample; The forced degradation test (sample solutions prepared in 0.01 M HCl, 0.01 M NaOH and aqueous conditions and kept at 60 ºC by 8 hours, and UV 254 nm at ambient temperature during 24 hours) aimed to show the susceptibility of the method to consequently indicate the stability of the sample. It was precise in intraday (RSD 1.27%), interday (RSD 1.18%) and between analysts (RSD 1.92%) levels. It was robust when small variations were performed in seven important parameters (wavelength, cuvette, filtration step, dibasic and monobasic phosphate brand, ultrasound time and source of water). The accuracy was proved by the standard recovery test and showed mean recovery of 101.10%. This method can be applied in routine analysis of quality control of vancomycin lyophilized powder and it is an effective, accessible and ecological alternative, which follows the Green Analytical Chemistry principles, presenting less waste generation, no use of toxic solvents, smaller sample volumes and required diluents, which impacts on the final cost of the analyzes.

Paper-Based Immunosensors with Bio-Chemiluminescence Detection

Since the introduction of paper-based analytical devices as potential diagnostic platforms a few decades ago, huge efforts have been made in this field to develop systems suitable for meeting the requirements for the point-of-care (POC) approach. Considerable progress has been achieved in the adaptation of existing analysis methods to a paper-based format, especially considering the chemiluminescent (CL)-immunoassays-based techniques. The implementation of biospecific assays with CL detection and paper-based technology represents an ideal solution for the development of portable analytical devices for on-site applications, since the peculiarities of these features create a unique combination for fitting the POC purposes. Despite this, the scientific production is not paralleled by the diffusion of such devices into everyday life. This review aims to highlight the open issues that are responsible for this discrepancy and to find the aspects that require a focused and targeted research to make these methods really applicable in routine analysis.