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Elucidating the Degradation Pathways of Human Insulin in the solid state

Journal of Analysis and Testing 2024年第3期8卷 288-299页

作者： Andrew Fagan Lorraine M.Bateman Joseph P.O'Shea Abina M.Crean SSPC the SFI Centre for Pharmaceutical Research School of Pharmacy University College Cork School of Pharmacy University College Cork Analytical and Biological Chemistry Research Facility (ABCRF) University College Cork School of Chemistry University College Cork

While there have been significant advances in the development of peptide oral dosage forms in recent years, highlighted by the clinical and commercial success of approved peptides such as Rybelsus?, there remain several barriers in the way of broad range applicability of this approach to peptide delivery. One such barrier includes the poor physical and chemical stability inherent to their structures, which persists in the solid state although degradation typically occurs at different rates and via different pathways in comparison to the solution state. Using insulin as a model peptide, this work sought to contribute to the development of analytical techniques for investigating common insulin degradation pathways. Chemically denatured,deamidated and aggregated samples were prepared and used to benchmark circular dichroism spectroscopy, reverse phase HPLC and size exclusion chromatography methods for the investigation of unfolding, chemical modifications and covalent aggregation of the insulin molecule respectively. solid state degraded samples were prepared by heating insulin powder at 60 °C and 75% relative humidity for 1, 3, 5 and 7 d, and the degradation profiles of the samples were evaluated and compared with those observed in solution. While no unfolding was observed to occur, significant deamidation and covalent aggregation were detected. Reductive disulfide bond cleavage using dithiothreitol allowed for separation of the insulin A-and B-chains,offering a facile yet novel means of assessing the mechanisms of deamidation and covalent aggregation occurring in the solid state.

关键词： Biopharmaceutical analysis Covalent aggregation Deamidation Disulfide cleavage Insulin solid state Stability

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solid state Photochemistry of Nitrobenzaldehydes

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Chemical Research in Chinese Universities 1995年第2期11卷 111-116页

作者： DU Da-nung,WANG Yong-mei,XIONG Guo-xiangWANG Wen-guang and MENG Ji-ben (Department of Chemistry,Nankai University,Tianjin,300071) NANKAI UNIV DEPT CHEMTIANJIN 300071PEOPLES R CHINA

The photochemical reaction of nilrobenzaldehyde with indole and antipyrine was investigated in solid *** structures of the new products were identified by means of IR,MS,'H NMR and elemental analysis,and the crystal structure of audition product 2c was determined by X-ray diffraction *** mechanism of this reaction was also proposed.

关键词： Nitrobenzaldellyde Indole Aniipyrine solid state Photochemical reaction

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Use of solid state Carbothermic Reduction in Production of Transition Metals and Their Carbides

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Journal of Iron and Steel Research International 2000年第2期7卷 14-22页

作者： YANG Yin-dong SOMMERVILLE I D JOHNSTON R F McLEAN A University of Toronto LaTrobe University

The use of solid state carbothermic reduction as a precursor to the smelting of transition metal ores was examined . The advantages of the introduction of a prereduction stage include enabling the more efficient use of fines and the achievement of higher energy efficiencies. A solid state reduction using carbon as the reductant offers a simpler alternative for their treatment. Subsequent treatment of the reduced material could include intensive bath smelting to produce ferroalloys or, in some case, solid state separation of the transition metal carbide where this has commercial significance.

关键词： solid state carbothermic reduction transition metals carbide

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Novel Secondary Structure of Calcitonin in solid state as Revealed by Circular Dichroism Spectroscopy

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Chinese Journal of Chemistry 2002年第7期20卷 697-698页

作者：杜海宁丁金国崔大敷胡红雨 Institute of Biochemistry and Cell Biology Shanghai Institutes for Biological Sciences Chinese Academy of Sciences Shanghai 200031 China

The solid-state circular dichroic study reveals that salmon calci-toninpresents a typical α-helical structure while human calci-tonin appears to form a β-sheet in solidstate, although both of them adopt random coil ... 详细信息

关键词： calcitonin circular dichroism solid state secondary structure

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An Efficient solid state Method for Deoximation under Mild Conditions

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Chinese Chemical Letters 2006年第12期17卷 1559-1562页

作者： Wang ZHOU Qian He LI Sha PENG Institute of Fine Catalysis and Synthesis Hunan Normal University Changsha 410080

Oximes of ketones and aldehydes are efficiently converted to the corresponding carbonyl compounds, using a combination of NaHSO4.H20 and paraformaldehyde in good to excellent yields under solid state conditions at roo... 详细信息

关键词： solid state deoximation oxime carbonyl compound.

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solid state ^(27)AL MAS-NMR STUDY OF POLYOXY-ALUMINUM PILLARED MONTMORILLONITE

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Chinese Chemical Letters 1992年第2期3卷 137-138页

作者： Si Fen XIANG~* Tong Wen HUA Qing JIANG Lian Bo WANG Department of Chemistry, Peking University, Beijing 100871

solid state magic-angle-spinning nuclear magnetic resonance spectroscopy (MAS-NMR) has been used to probe the signal of ^(27)Al in polyoxyaluminum pillared montmorillonite. The experimental results show that the polyh... 详细信息

关键词： NMR solid state AL MAS-NMR STUDY OF POLYOXY-ALUMINUM PILLARED MONTMORILLONITE MAS

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The Use of solid state NMR to Evaluate the Carbohydrates in Commercial Coffee Granules

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Food and Nutrition Sciences 2011年第4期2卷 350-355页

作者： Regina Freitas Nogueira Elisangela Fabiana Boffo Maria Inês Bruno Tavares Leonardo AMoreira Leila Aley Tavares Antonio Gilberto Ferreira Departamento de Química da Universidade Federal de Sao CarlosSao CarlosBrasil Institutito de Macromoléculas Universidade Federal do Rio de JaneiroRio de JaneiroBrasil Escola Técnica Federal de Minas GeraisBrasil

Coffee brings many health benefits due to its chemical constituents. Based on this information, it is essential to know the main chemical compounds from coffee granules;the intermolecular interaction among the coffees compounds and the molecular components homogeneity. In this study six types of roasted commercial coffee were evaluated by solid state nuclear magnetic resonance (NMR), employing carbon-13 (13C) and hydrogen (1H) nucleus. Carbon-13 was analyzed applying high field NMR techniques, such as: magic angle spinning (MAS);magic angle spinning with cross-polariza- tion (CPMAS) and magic angle spinning with cross-polarization and dipolar dephasing (CPMASDD). The hydrogen was evaluated via relaxation times. Proton spin-lattice relaxation time in the rotating frame was deter-mined through the carbon-13 decay, during the variable contact-time experiment, using high field NMR. Proton spin-lattice relaxation time was determined through the inversion-recovery pulse sequence, using low field NMR. Considering all NMR results, it was concluded that the major coffee compounds are: a) triacilglycerides, which constitute the mobile region in the granule coffee and b) Carbohydrates such as: polysaccharides and fibers that belong to the rigid domain. These constituents belong to different molecular mobility domain, although they have strong intermolecular interactions due to the granule organization.

关键词： solid state NMR Coffee

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Synergistic interactions between the charge‐transport and mechanical properties of the ionic‐liquid‐based solid polymer electrolytes for solid‐state lithium batteries

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Carbon Energy 2023年第11期5卷 44-53页

作者： Ashutosh Agrawal Saeed Yari Hamid Hamed Tom Gouveia Rongying Lin Mohammadhosein Safari Institute for Materials Research(IMOimomec) UHasseltHasseltBelgium Energyville GenkBelgium Solvionic ToulouseFrance IMEC Division IMOMEC DiepenbeekBelgium

The performance sensitivity of the solid‐state lithium cells to the synergistic interactions of the charge‐transport and mechanical properties of the electrolyte is well acknowledged in the literature,but the quantitative insights therein are very ***,the charge‐transport and mechanical properties of a polymerized ionic‐liquid‐based solid electrolyte are *** transference number and diffusion coefficient of lithium in the concentrated solid electrolyte are measured as a function of concentration and stack *** elastoplastic behavior of the electrolyte is quantified under compression,within a home‐made setup,to substantiate the impact of stack pressure on the stability of the Li/electrolyte interface in the symmetric lithium *** results spotlight the interaction between the concentration and thickness of the solid electrolyte and the stack pressure in determining the polarization and stability of the solid‐state lithium batteries during extended cycling.

关键词： battery diffusion pressure solid state transference

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New Type High Efficient Quasi-solid-state Ionic Liquid Electrolyte for Dye-Sensitized Solar Cells

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Chinese Journal of Chemistry 2007年第11期25卷 1601-1603页

作者：潘旭戴松元王孔嘉 Division of Solar Energy Materials and Engineering Institute of Plasma Physics (ASIPP) Chinese Academy of Sciences Hefei Anhui 230031 China

For the fist time the preparation of a mostly solid-state high efficiem electro-conductive material comprising 1-methyl-3-propylimidazolium iodide （MPII）, benzimidazole （BI）, iodine and lithium iodide was reported. In this electrolyte, BI acts as not only additives but also gelators. With its significant electrochemical properties, an overall efficiency of 3.07% was achieved under AM 1.5 （100 mW/cm^2）.

关键词： dye-sensitized solar cell ionic liquid solid state electrolyte

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Covalent triazine framework with efficient photocatalytic activity in aqueous and solid media

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Frontiers of Chemical Science and Engineering 2020年第3期14卷 397-404页

作者： Cyrine Ayed Wei Huang Kai A.I.Zhang Max Planck Institute for Polymer Research 55128 MainzGermany Graduate School for Excellence Materials Science in Mainz Johannes Gutenberg University Mainz55128 MainzGermany

Covalent triazine frameworks(CTFs)have been recently employed for visible light-driven photocatalysis due to their unique optical and electronic ***,the usually highly hydrophobic nature of CTFs,which originates from their overall aromatic backbone,leads to limitations of CTFs for applications in aqueous *** this study,we aim to extend the range of the application media of CTFs and design hybrid material of a CTF and mesoporous silica(SBA-15)for efficient photocatalysis in aqueous medium.A thiophene-containing CTF was directly synthesized in mesopores of *** to the high surface area and the added hydrophilic properties by silica,the hybrid material demonstrated excellent adsorption of organic molecules in *** leads not only to high photocatalytic performance of the hybrid material for the degradation of organic dyes in water,but also for efficient photocatalysis in solvent-free and solid ***,the reusability,stability and easy recovery of the hybrid material offers promising metal-free heterogeneous photocatalyst for broader applications in different reaction media.

关键词： photocatalysis covalent triazine framework aqueous medium SBA-15 solid state

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