Stability Indicating UPLC Method Development and Validation for the Quantification of Ibandronate Sodium and Characterisation of its Degradation Products

In the present study a new stability indicating UPLC method has been developed and validated for the quantification of Ibandronate sodium. The developed method was validated as per ICH guidelines. The parameters which are validated are linearity, accuracy, precision, robustness and system suitability parameters. The chromatographic conditions were optimized before the development of the chromatogram. The mobile phase consisted of a mixture of pH 5.3 ammonium formate buffer and acetonitrile (70:30 v/v) under under isocratic mode of elution. The system suitability parameters such as theoretical plates, tailing factor and peak symmetry were determined to check the validity of the developed UPLC method. The developed chromatographic method proved to be superior to most of the reported methods in terms of accuracy, precision and sensitivity. The data obtained was subjected to statistical analysis. The proposed method was successfully applied to the determination of the selected drug in its pharmaceutical dosage form. The stability indicating UPLC method is useful to understand the degradation behaviour of Ibandronate sodium. Ibandronate sodium was subjected to forced degradation study. IBT was found to degrade in thermal degradation conditions and the degradation product was characterised by Mass spectrometry. Toxicity of the degradation product was checked by using Osiris software. It was found that the degradation product is non-toxic. Prediction results are colour coded in which the red colour shows high risks with undesired effects like mutagenicity or poor intestinal absorption and green colour indicates drug-conform behaviour. The proposed method is accurate, selective, sensitive and reproducible. The method is relatively free from any interference produced from common tablet excipients. Hence, the recommended procedure is well suited for the assay and evaluation of IBT in pharmaceutical quality control. The present work can be extended for the quantification of the selected drug in bioavailability, bioequivalence, pharmacokinetics, in-vitro and in-vivo correlation studies. A successful analyst must know what reactions are taking place during analysis and be able to understand and apply the theory upon which the method is dependent. The analyst must acquire skills of technique, patience, neatness and accuracy. Absolute integrity is demanded of every quantitative analyst. To become a successful analyst, one must realize that, analytical chemistry is not a simple routine procedure. Manipulative skill acquired by experience with the ability to follow directions under the supervision of a skilled analyst may enable one to carry out successfully certain analytical procedures

Selected Analytical Techniques of Solid State, Structure Identification, and Dissolution Testing in Drug Life Cycle

The textbook provides an overview of the main techniques applied in pharmaceutical industry, with the focus on solid-state analysis. It discusses spectral methods, thermal analysis, and dissolution testing, explains the theoretical background for each method and shows practical examples from a real-life drug-design and quality control applications. The textbook is thus intended for both pharmacy students and early career professionals

Advanced Materials in Drug Release and Drug Delivery Systems

Development of new drug molecules is costly and requires longitudinal, wide-ranging studies; therefore, designing advanced pharmaceutical formulations for existing and well-known drugs seems to be an attractive device for the pharmaceutical industry. Properly formulated drug delivery systems can improve pharmacological activity, efficacy and safety of the active substances. Advanced materials applied as pharmaceutical excipients in designing drug delivery systems can help solve problems concerning the required drug release—with the defined dissolution rate and at the determined site. Novel drug carriers enable more effective drug delivery, with improved safety and with fewer side effects. Investigations concerning advanced materials represent a rapidly growing research field in material/polymer science, chemical engineering and pharmaceutical technology. Exploring novel materials or modifying and combining existing ones is now a crucial trend in pharmaceutical technology. Eleven articles included in the the Special Issue “Advanced Materials in Drug Release and Drug Delivery Systems” present the most recent insights into the utilization of different materials with promising potential in drug delivery and into different formulation approaches that can be used in the design of pharmaceutical formulations

Nutritional abnormalities in patients receiving long-term home parenteral nutrition

The last two decades have seen an increased drive to administer parenteral nutrition (PN) to patients in their home environments, thereby reducing associated hospital costs and improving patient quality of life. The occurrence of deranged nutritional biochemistry results has baffled PN experts for years because PN additives are marketed for the general needs of patients and PN is tailored to each patient’s requirements (both formulation and regimen). This thesis documents the investigations into HPN population characteristics, the extent of nutritional abnormalities (deficiencies and excesses) in a cohort of LT PN patients in Wales. Both cross-sectional and longitudinal retrospective study designs were employed alongside small-scale laboratory efforts to investigate stability of vitamin D in PN additives using High Performance Liquid Chromatography (HPLC). Characteristics of the HPN population in Wales were shown to be variable in terms of PN requirements for a predominantly female sample population (2:1); in whom 78.6% of patients received PN for indications relating to short bowel syndrome (SBS). A database analysis of micronutrient test results revealed a high prevalence of deficiencies of vitamin D and selenium, as well as excesses of manganese and water-soluble vitamins; which can lead to clinically relevant effects in patients. The sample population was shown to have impaired bone health since first receiving PN; respective sites of the femoral neck and total hip presented 58% and 60.8% of patients had osteopenia, while 28% and 19.6% had osteoporosis. Evidence in the literature links these clinical outcomes of metabolic bone disease (MBD) to patients’ inadequate vitamin D status. A final study exploring the adequacy of the trace element (TE) preparation Additrace®, found it lacking in selenium and excessive in manganese for the general requirements of the PN population. Clinician-directed supplementation of PN outside of Additrace® was associate

ZnO NP e compósitos PU/ZnO NP para libertação controlada de Ibuprofeno

Mestrado em Ciência e Engenharia de MateriaisFor the design of drug delivery systems, in which a large amount of drug should be stored and released over a sustained period of time, utilization of nanostructures is frequently advantageous as their high specific surface areas are beneficial for adsorptive drug loading. Additionally, the use of nanostructured drug carriers in concert with polymeric materials in composite drug delivery systems affords control over the drug release characteristics. While many combinations of materials can be imagined, the use of zinc-oxide and poly(urethane) is of particular interest in that nanostructures based on the former are easily producible and the latter is already an established material in biomedical applications. In this investigation, various aspects of the drug delivery properties were examined. In particular, the effects of altering the amount of drug loaded (by loading in solutions of 1, 2, 10, and 20 mg ibuprofen/mL ethanol) were studied and it was demonstrated that the amount of drug loaded can be controlled, which is important for customizing dosages in drug delivery systems. Additionally, the role of a washing procedure after loading the nanoparticles was examined in order to show that these procedures influence the drug loading by removal of loosely bound layers of drug. In completion of this study, the release of ibuprofen from both pure zinc oxide nanoparticles and the composites with poly(urethane) was investigated by tracking the concentration of drug present in a phosphate buffered saline solution containing the drug carrier with respect to time. In order better understand the mechanisms of drug release and analyze the degradation processes of the drug carrier, SEM images were produced for the samples at various times during the drug release process.Para projectar um sistema de entrega de fármacos, em que se pretende armazenar uma grande quantidade de fármaco a ser libertada durante um período de tempo longo, é vantajoso recorrer a nanoestruturas com elevada área específica para o carregamento do fármaco por processos adsortivos. Além disso, a combinação de transportadores nanoestruturados com materiais poliméricos, formando sistemas compósitos para a entrega de fármacos pode proporcionar o controlo de certos parâmetros associados à libertação do fármaco. Entre as várias combinações possíveis, o óxido de zinco (ZnO) e o poliuretano (PU) oferecem um particular interesse dado ser possível preparar ZnO nanoestruturado e o PU ser um polímero com reconhecida aptidão para aplicações médicas. Neste trabalho, estudaram-se vários aspectos do processo de libertação de um fármaco modelo (o ibuprofeno) a partir de nanoestruturas de óxido de zinco e de compositos ZnO/PU. Em particular, estudaram-se os efeitos da variação da carga do fármaco usando soluções etanólicas com diferentes concentrações do fármaco,i.e. 1, 2, 10, e 20 mg de ibuprofeno / mL de etanol, tendo-se demonstrado que por esta via se pode controlar a carga do fármaco , o que é importante para personalização da dose em sistemas de entrega de fármacos. Além disso, a importância dos procedimentos de lavagem das nanoestruturas após carregamento do fármaco foi também avaliada, concluindo-se que tais procedimentos condicionam a carga de fármaco por remoção das camadas de fármaco fracamente adsorvidas. Estudou-se também a libertação de ibuprofeno a partir das nanoestruturas de óxido de zinco puro e dos compositos ZnO/PU, medindo a variação no tempo da quantidade de fármaco libertada em solução tampão de fosfato. Os perfis de libertação do fármaco aliados às imagens de microscopia electrónica (SEM) dos materiais obtidas no fim de diferentes períodos de tempo de libertação são usados neste trabalho para discutir os mecanismos de libertação do fármaco e avaliar a sua relação com a degradação do material em análise

Inflammatory Bowel Disease

This book is dedicated to inflammatory bowel disease, and the authors discuss the advances in the pathogenesis of inflammatory bowel disease, as well as several new parameters involved in the etiopathogeny of Crohn's disease and ulcerative colitis, such as intestinal barrier dysfunction and the roles of TH 17 cells and IL 17 in the immune response in inflammatory bowel disease. The book also focuses on several relevant clinical points, such as pregnancy during inflammatory bowel disease and the health-related quality of life as an end point of the different treatments of the diseases. Finally, advances in management of patients with inflammatory bowel disease are discussed, especially in a complete review of the recent literature