scholarly journals Calorimetric Investigation of the Relaxation Phenomena in Amorphous Lyophilized Solids

Pharmaceutics ◽  
2021 ◽  
Vol 13 (10) ◽  
pp. 1735
Author(s):  
Sebastian Groёl ◽  
Tim Menzen ◽  
Gerhard Winter
Keyword(s):  
Thermal History ◽  
Drug Product ◽  
Scanning Calorimetry ◽  
Calorimetric Methods ◽  
Drug Products ◽  
Relevant Today ◽  
Freeze Dried ◽  
The Matrix ◽  
Amorphous Drug ◽  
Calorimetric Investigations

Studying the thermal history and relaxation of solid amorphous drug product matrices by calorimetry is a well-known approach, particularly in the context of correlating the matrix parameters with the long-term stability of freeze-dried protein drug products. Such calorimetric investigations are even more relevant today, as the application of new process techniques in freeze-drying (which strongly influence the thermal history of the products) has recently gained more interest. To revive the application of calorimetric methods, the widely scattered knowledge on this matter is condensed into a review and completed with new experimental data. The calorimetric methods are applied to recent techniques in lyophilization, such as controlled nucleation and aggressive/collapse drying. Phenomena such as pre-Tg events in differential scanning calorimetry and aging shoulders in isothermal microcalorimetry are critically reviewed and supplemented with data of freeze-dried products that have not been characterized with these methods before.

Sorption Isotherm, Glass Transitions and State Diagram for Freeze-dried Plum Skin and Pulp

2006 ◽  
Vol 12 (3) ◽  
pp. 181-187 ◽  
Author(s):  
V. R. Nicoletti Telis ◽  
P. J. do Amaral Sobral ◽  
J. Telis-Romero
Keyword(s):  
Glass Transition ◽  
Moisture Content ◽  
Sorption Isotherm ◽  
State Diagram ◽  
Transition Curve ◽  
Glass Transitions ◽  
Water Addition ◽  
Scanning Calorimetry ◽  
Freeze Dried ◽  
The Matrix

Differential scanning calorimetry (DSC) was used to determine phase transitions of freeze-dried plums. Samples at low and intermediate moisture contents, were conditioned by adsorption at various water activities (0.11≤aw≤0.90) at 25°C, whereas in the high moisture content region (aw>0.90) samples were obtained by direct water addition, with the resulting sorption isotherm being well described by the Guggenheim-Anderson-deBoer (GAB) model. Freeze-dried samples of separated plum skin and pulp were also analysed. At aw≤0.75, two glass transitions were visible, with the glass transition temperature (Tg) decreasing with increasing aw due to the water plasticising effect. The first Tg was attributed to the matrix formed by sugars and water. The second one, less visible and less plasticised by water, was probably due to macromolecules of the fruit pulp. The Gordon-Taylor model represented satisfactorily the matrix glass transition curve for aw≤0.90. In the higher moisture content range Tg remained practically constant around Tg′ (−57.5°C). Analysis of the glass transition curve and the sorption isotherm indicated that stability at a temperature of 25°C, would be attained by freeze dried plum at a water activity of 0.04, corresponding to a moisture content of 12.9% (dry basis).

scholarly journals Proof-of-Concept of Detection of Counterfeit Medicine through Polymeric Materials Analysis of Plastics Packaging

Polymers ◽  
2021 ◽  
Vol 13 (13) ◽  
pp. 2185
Author(s):  
Mohammad Salim ◽  
Riyanto Teguh Widodo ◽  
Mohamed Ibrahim Noordin
Keyword(s):  
Polymeric Materials ◽  
Proof Of Concept ◽  
Scanning Calorimetry ◽  
Counterfeit Drug ◽  
Drug Products ◽  
Counterfeit Medicines ◽  
Counterfeit Medicine ◽  
Counterfeit Pharmaceuticals ◽  
Purge Gas ◽  
Sample Set

The detection of counterfeit pharmaceuticals is always a major challenge, but the early detection of counterfeit medicine in a country will reduce the fatal risk among consumers. Technically, fast laboratory testing is vital to develop an effective surveillance and monitoring system of counterfeit medicines. This study proposed the combination of Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) and Differential Scanning Calorimetry (DSC) for the quick detection of counterfeit medicines, through the polymer analysis of blister packaging materials. A sample set containing three sets of original and counterfeit medicine was analyzed using ATR-FTIR and DSC, while the spectra from ATR-FTIR were employed as a fingerprint for the polymer characterization. Intending to analyze the polymeric material of each sample, DSC was set at a heating rate of 10 °C min−l and within a temperature range of 0- 400 °C, with nitrogen as a purge gas at a flow rate of 20 ml min−an. The ATR-FTIR spectra revealed the chemical characteristics of the plastic packaging of fake and original medicines. Further analysis of the counterfeit medicine’s packaging with DSC exhibited a distinct difference from the original due to the composition of polymers in the packaging material used. Overall, this study confirmed that the rapid analysis of polymeric materials through ATR-FTIR and comparing DSC thermograms of the plastic in their packaging effectively distinguished counterfeit drug products.

scholarly journals Characteristics of Reconstituted Collagen Fibers from Chicken Keel Cartilage Depends on Salt Type for Removal of Proteoglycans

Molecules ◽  
2021 ◽  
Vol 26 (12) ◽  
pp. 3538
Author(s):  
Anna Pudło ◽  
Szymon Juchniewicz ◽  
Wiesław Kopeć
Keyword(s):  
Electron Microscopy ◽  
Rheological Properties ◽  
Thermal Denaturation ◽  
Surface Structures ◽  
Scanning Calorimetry ◽  
Cartilage Extracellular Matrix ◽  
Oscillatory Rheometry ◽  
Freeze Dried ◽  
Basic Features ◽  
Scanning Electron

The aim of the presented research was to obtain reconstituted atelocollagen fibers after extraction from poultry cartilage using the pepsin-acidic method in order to remove telopeptides from the tropocollagen. Firstly, we examined the extraction of collagen from the cartilage extracellular matrix (ECM) after proteoglycans (PG) had been removed by the action of salts, i.e., NaCl or chaotropic MgCl2. Additionally, the effects of the salt type used for PG and hyaluronic acid removal on the properties of self-assembled fibers in solutions at pH 7.4 and freeze-dried matrices were investigated. The basic features of the obtained fibers were characterized, including thermal properties using scanning calorimetry, rheological properties using dynamic oscillatory rheometry, and the structure by scanning electron microscopy. The fibers obtained after PG removal with both analyzed types of salts had similar thermal denaturation characteristics. However, the fibers after PG removal with NaCl, in contrast to those obtained after MgCl2 treatment, showed different rheological properties during gelatinization and smaller diameter size. Moreover, the degree of fibrillogenesis of collagens after NaCl treatment was complete compared to that with MgCl2, which was only partial (70%). The structures of fibers after lyophilization were fundamentally different. The matrices obtained after NaCl pretreatment form regular scaffolds in contrast to the thin, surface structures of the cartilage matrix after proteoglycans removal using MgCl2.

MICROSTRUCTURAL EVOLUTION OF Al-Cu-Mg-Ag ALLOY WITH TRACE Zr ADDITION DURING TWO-STEP HOMOGENIZATION

2009 ◽  
Vol 23 (06n07) ◽  
pp. 855-862 ◽  
Author(s):  
FEIYUE MA ◽  
ZHIYI LIU
Keyword(s):  
Melting Point ◽  
Grain Boundaries ◽  
Microstructural Evolution ◽  
Cast Alloy ◽  
Scanning Calorimetry ◽  
Zr Addition ◽  
Homogenization Time ◽  
The Matrix ◽  
Higher Temperature ◽  
Lower Temperature

The microstructural evolution in an Al - Cu - Mg - Ag alloy with trace Zr addition during homogenization treatment was characterized by Differential Scanning Calorimetry (DSC), Scanning Electron Microscopy (SEM) and Energy-dispersive X-ray Spectroscopy (EDS). It was shown that the low-melting-point phase segregating toward grain boundaries is Al 2 Cu , with a melting point of 523.52°C. A two-step homogenization process was employed to optimize the microstructure of the as-cast alloy, during which the alloy was first homogenized at a lower temperature, then at a higher temperature. After homogenized at 420°C for 6 h, Al 3 Zr particles were finely formed in the matrix. After that, when the alloy was homogenized at an elevated temperature for a longer time, i.e., 515°C for 24 h, most of the precipates at the grain boundaries were removed. Furthermore, the dispersive Al 3 Zr precipitates were retained, without coarsening greatly in the final homogenization step. A kinetics model is employed to predict the optimal homogenization time at a given temperature theoretically, and it confirms the result in present study, which is 420°C/6h+515°C/24h.

Properties of aluminum metal matrix composites manufactured by selective laser melting

2021 ◽  
Vol 112 (7) ◽  
pp. 552-564
Author(s):  
Christian Felber ◽  
Florian Rödl ◽  
Ferdinand Haider
Keyword(s):  
Additive Manufacturing ◽  
Aluminum Alloys ◽  
Selective Laser Melting ◽  
Metal Matrix ◽  
High Hardness ◽  
High Strength ◽  
Laser Melting ◽  
Scanning Calorimetry ◽  
Particle Reinforcement ◽  
The Matrix

Abstract The most promising metal processing additive manufacturing technique in industry is selective laser melting, but only a few alloys are commercially available, limiting the potential of this technique. In particular high strength aluminum alloys, which are of great importance in the automotive industry, are missing. An aluminum 2024 alloy, reinforced by Ti-6Al-4V and B4C particles, could be used as a high strength alternative for aluminum alloys. Heat treating can be used to improve the mechanical properties of the metal matrix composite. Dynamic scanning calorimetry shows the formation of Al2Cu precipitates in the matrix instead of the expected Al2CuMg phases due to the loss of magnesium during printing, and precipitation processes are accelerated due to particle reinforcement and additive manufacturing. Strong reactions between aluminum and Ti-6Al-4V are observed in the microstructure, while B4C shows no reaction with the matrix or the titanium. The material shows high hardness, high stiffness, and low ductility through precipitation and particle reinforcement.

scholarly journals Thermal Kinetics of SiCp Reinforced Al-Zn-Mg-Cu Alloy Composite

2021 ◽  
Author(s):  
Saikat Das ◽  
R. Govinda Rao ◽  
Prasanta Kumar Rout
Keyword(s):  
Base Alloy ◽  
Accelerated Aging ◽  
Stir Casting ◽  
Hardness Profile ◽  
Scanning Calorimetry ◽  
Transmission Electron ◽  
The Matrix ◽  
Aging Kinetics ◽  
Aging Phenomena ◽  
Kinetics Of

Abstract In the present work, the artificial aging kinetics of SiCp particles reinforced AA7075-SiCp composite fabricated by stir casting method was investigated. The aging behavior of AA7075-SiCp composite was investigated by Rockwell hardness tests and differential scanning calorimetry (DSC). Results show there are no changes in the sequences of formation and dissolution of precipitate. Reinforced particles are uniformly distributed throughout the matrix. The hardness profile shows increase in hardness with the comparison of AA7075 base alloy. In addition to SiCp in the matrix, precipitation kinetics has changed compared with base alloy since higher dislocations present in composite, hence requires lower activation energy to form ή precipitate and takes less time to reach the maximum hardness. In contrast, the addition of SiCp at low volume percent also showing accelerated aging phenomena in the composite during the aging process. High-resolution transmission electron microscope (HRTEM) micrograph of peak age (T6) condition divulges that enormous fine and plate-like ή (MgZn2) precipitates are uniformly distributed in the composite.

scholarly journals Container Closure and Delivery Considerations for Intravitreal Drug Administration

2021 ◽  
Vol 22 (3) ◽  
Author(s):  
Ashwin C. Parenky ◽  
Saurabh Wadhwa ◽  
Hunter H. Chen ◽  
Amardeep S. Bhalla ◽  
Kenneth S. Graham ◽  
...  
Keyword(s):  
Adverse Events ◽  
Product Development ◽  
Drug Product ◽  
Healthcare Providers ◽  
Standard Of Care ◽  
Volume Determination ◽  
Common Procedure ◽  
Drug Products ◽  
Fill Volume ◽  
Container Closure

AbstractIntravitreal (IVT) administration of therapeutics is the standard of care for treatment of back-of-eye disorders. Although a common procedure performed by retinal specialists, IVT administration is associated with unique challenges related to drug product, device and the procedure, which may result in adverse events. Container closure configuration plays a crucial role in maintaining product stability, safety, and efficacy for the intended shelf-life. Careful design of primary container configuration is also important to accurately deliver small volumes (10-100 μL). Over- or under-dosing may lead to undesired adverse events or lack of efficacy resulting in unpredictable and variable clinical responses. IVT drug products have been traditionally presented in glass vials. However, pre-filled syringes offer a more convenient administration option by reducing the number of steps required for dose preparation there by potentially reducing the time demand on the healthcare providers. In addition to primary container selection, product development studies should focus on, among other things, primary container component characterization, material compatibility with the formulation, formulation stability, fill volume determination, extractables/leachables, and terminal sterilization. Ancillary components such as disposable syringes and needles must be carefully selected, and a detailed administration procedure that includes dosing instructions is required to ensure successful administration of the product. Despite significant efforts in improving the drug product and administration procedures, ocular safety concerns such as endophthalmitis, increased intraocular pressure, and presence of silicone floaters have been reported. A systematic review of available literature on container closure and devices for IVT administration can help guide successful product development.

scholarly journals Freeze versus Spray Drying for Dry Wild Thyme (Thymus serpyllum L.) Extract Formulations: The Impact of Gelatin as a Coating Material

2021 ◽  
Author(s):  
Aleksandra A. Jovanović ◽  
Steva M. Lević ◽  
Vladimir B. Pavlovic ◽  
Smilja B. Markovic ◽  
Rada V. Pjanovic ◽  
...  
Keyword(s):  
Spray Drying ◽  
Dry Weight ◽  
Drying Process ◽  
Scanning Calorimetry ◽  
Coating Agent ◽  
Microwave Assisted ◽  
Freeze Dried ◽  
Wild Thyme ◽  
The Impact ◽  
Spray Dried

Freeze drying was compared with spray drying regarding feasibility to process wild thyme drug in order to obtain dry formulations at laboratory scale starting from liquid extracts produced by different extraction methods: maceration, heat-, ultrasound-, and microwave-assisted extractions. Higher powder yield (based on the dry weight prior to extraction) was achieved by freeze than spray drying and lower loss of total polyphenol content (TPC) and total flavonoid content (TFC) due to the drying process. Gelatin as a coating agent (5% w/w) provided better TPC recovery by 70% in case of lyophilization and higher powder yield in case of spray drying by diminishing material deposition on the wall of the drying chamber. The resulting gelatin-free and gelatin-containing powders carried polyphenols in amount ~190 and 53-75 mg gallic acid equivalents GAE/g of powder, respectively. Microwave-assisted extract formulation distinguished from others by higher content of polyphenols, proteins and sugars, higher bulk density and lower solubility. The type of the drying process affected mainly position of the gelatin-derived -OH and amide bands in FTIR spectra. Spray dried formulations compared to freeze dried expressed higher thermal stability as confirmed by differential scanning calorimetry analysis and higher diffusion coefficient; the last feature can be associated with the lower specific surface area of irregularly shaped freeze-dried particles (151-223 µm) compared to small microspheres (~8 µm) in spray-dried powder.

scholarly journals Rotulagem de medicamentos industrializados: uma análise das diretrizes legais brasileiras e contribuições para a qualidade de produtos

2020 ◽  
Vol 20 (81) ◽  
Author(s):  
Márcia Lombardo
Keyword(s):  
Drug Product ◽  
Regulatory Agencies ◽  
Quality And Safety ◽  
Sources Of Information ◽  
Normative Documents ◽  
Drug Products ◽  
Legal Provisions ◽  
Product Surveillance ◽  
Study Results ◽  
Regulatory Knowledge

RESUMOObjetivos: a rotulagem é um aspecto de qualidade fundamental no uso de medicamentos, seja pelo profissional de saúde, seja pelo paciente. Este trabalho propôs uma análise crítica do tema com base na legislação em vigor, bem como a triagem de documentos normativos úteis no processo de elaboração ou de avaliação da conformidade da rotulagem de medicamentos. Métodos: foi realizada uma pesquisa documental empregando-se como fonte de informações os sítios eletrônicos oficiais do Ministério da Saúde e da Agência Nacional de Vigilância Sanitária. Os documentos contendo itens pertinentes a rotulagem de medicamentos e classificados como vigentes ou vigentes com alteração foram selecionados para a realização do estudo. Resultados: os quesitos mais relevantes das disposições gerais e das disposições específicas da norma vigente para rotulagem de medicamentos foram sistematizados, verificando-se suas contribuições na qualidade e segurança de produtos. Embora a padronização da rotulagem de medicamentos seja necessária, a ocorrência de elevados graus de semelhança entre rótulos, embalagens ou mesmo nomenclaturas é discutida no âmbito da prática clínica e esta questão merece atenção especial. A busca de material complementar à legislação vigente resultou no levantamento de um total de 20 documentos, incluindo normas, guias, bancos de consulta e planilhas, que podem auxiliar no cumprimento dos requisitos de rotulagem de medicamentos. Conclusão: rótulos de medicamentos são recursos técnicos que contribuem na eficácia e na segurança do tratamento. Os esforços das Agências Reguladoras têm permitido a consolidação de diretrizes legais para que informações e formatos adequados de rotulagem sejam aplicados nas embalagens de medicamentos industrializados. A elaboração ou a análise da rotulagem de medicamentos requer amplo conhecimento regulatório, o qual é dinâmico e, portanto, um grande desafio.Palavras-chave: Rotulagem de Medicamentos. Legislação de Medicamentos. Vigilância de Produtos Comercializados. Segurança do Paciente. ABSTRACTObjectives: the labeling of drug products is an aspect of quality that is fundamental to the use of medicines, whether by the health professional or by the patient. This work proposed a critical analysis of the current legislation on the labeling of drug products, as well as the screening of normative documents useful for the process of preparing or assessing the conformity of labels. Methods: a documentary research was carried out using the official websites of the Ministry of Health and the National Health Surveillance Agency (Brazil) as sources of information. The documents containing relevant items on labeling of drug products and classified as current or current with changes were selected for the study. Results: the most important requirements of the general and specific provisions from the current legislation have been systematized, and their contributions to the quality and safety of products have been verified. Although the standardization of the labeling is necessary, the occurrence of high degrees of similarity between labels, packaging or even nomenclatures is discussed in the context of clinical practice and this issue deserves special attention. The search for material complementary to the current legislation resulted in the collection of a total of 20 documents, including normative documents, guides, databases and spreadsheets, which might help in complying with the requirements for the labeling of drug products. Conclusion: the labeling of drug products are technical resources that contribute to the effectiveness and safety of treatment. The efforts of the Regulatory Agencies have allowed the consolidation of legal provisions for the dissemination of appropriate information and labeling formats in the packaging of drug products. The drafting or analysis of the labels requires extensive regulatory knowledge, which is dynamic and, therefore, a great challenge.Keywords: Drug Labeling. Legislation, Drug. Product Surveillance, Postmarketing. Patient Safety.

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