Estimation of the hydration of polar groups of ?-amino acids by differential scanning calorimetry

1996 ◽  
Vol 45 (9) ◽  
pp. 2121-2126 ◽  
Author(s):  
M. M. Vorob'ev ◽  
A. N. Danilenko
2019 ◽  
Author(s):  
P. Garidel ◽  
A. Eiperle ◽  
M. Blech ◽  
J. Seelig

AbstractThe thermal unfolding of a recombinant monoclonal antibody IgG1 (mAb) was measured with differential scanning calorimetry (DSC). The DSC thermograms reveal a pre-transition at 72°C with an unfolding enthalpy of ΔHcal ∼ 200-300 kcal/mol and a main transition at 85 °C with an enthalpy of ∼900 - 1000 kcal/mol. In contrast to single-domain molecules, mAb unfolding is a complex reaction that is analysed with the multi-state Zimm-Bragg theory. For the investigated mAb, unfolding is characterised by a cooperativity parameter σ ∼10−4 and a Gibbs free energy of unfolding of gnu ∼100 cal/mol per amino acid. The enthalpy of unfolding provides the number of amino acid residues v participating in the unfolding reaction. On average, v∼220±50 amino acids are involved in the pre-transition and v∼850±30 in the main transition, accounting for ∼90% of all amino acids. Thermal unfolding was further studied in the presence of guanidineHCl. The chemical denaturant reduces the unfolding enthalpy ΔHcal and lowers the midpoint temperature T0. Both parameters depend linearly on the concentration of denaturant. The guanidineHCl concentrations needed to unfold mAb at 25 °C are predicted to be 2-3 M for the pre-transition and 5-7 M for the main transition, varying with pH. GuanidineHCl binds to mAb with an exothermic binding enthalpy, which partially compensates the endothermic mAb unfolding enthalpy. The number of guanidineHCL molecules bound upon unfolding is deduced from the DSC thermograms. The bound guanidineHCl-to-unfolded amino acid ratio is 0.79 for the pre-transition and 0.55 for the main transition. The pre-transition binds more denaturant molecules and is more easily destabilised than the main transition.Overall, the current study shows the strength of the Zimm-Bragg model for the quantitative description of unfolding events of large, therapeutic proteins, such as a monoclonal antibody.Statement of significanceFirst quantitative thermodynamic study of an antibody with differential scanning calorimetry and analyzed with the multi-state Zimm-Bragg theory.


2019 ◽  
Author(s):  
Andreas Boelke ◽  
Yulia A. Vlasenko ◽  
Mekhman S. Yusubov ◽  
Boris Nachtsheim ◽  
Pavel Postnikov

<p>The thermal stability of pseudocyclic and cyclic <i>N</i>-heterocycle-stabilized (hydroxy)aryl- and mesityl(aryl)-l<sup>3</sup>-iodanes (NHIs) through thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) is investigated. NHIs bearing <i>N</i>-heterocycles with a high N/C-ratio such as triazoles show among the lowest descomposition temperatures and the highest decomposition energies. A comparison of NHIs with known (pseudo)cyclic benziodoxolones is made and we further correlated their thermal stability with reactivity in a model oxygenation. </p>


Author(s):  
Hariyanti Hariyanti ◽  
Sophi Damayanti ◽  
Sasanti Tarini

Sinkonin praktis tidak larut dalam air, sedikit larut dalam kloroform dan alkohol. Hal ini berdampak pada rendahnya penetrasi transfollicular sinkonin, karena hanya bahan aktif hidrofilik yang mampu melewati hair follicle. Dengan demikian dibutuhkan satu sistem penghantaran yang mampu menurunkan hidrofobisitas sinkonin untuk meningkatkan penetrasi sinkonin ke follicle. Niosom merupakan vesikel ampifilik dengan struktur lapisan rangkap yang terbentuk dari hidrasi kombinasi surfaktan nonionik dan kolesterol yang mampu menurunkan hidrofobisitas sinkonin. Penelitian ini bertujuan untuk menentukan proses pembuatan niosom sinkonin yang optimum. Pembuatan niosom sinkonin diawali dengan menentukan temperatur gelasi (Tg) dari span 60 dengan Differential Scanning Calorimetry (DSC), kemudian dilanjutkan dengan optimasi proses meliputi: optimasi kecepatan rotavapor pembentukan film lapis tipis, temperatur hidrasi, kecepatan rotavapor hidrasi, waktu hidrasi, dan waktu sonikasi. Karakteristik vesikel niosom yang optimal meliputi: ukuran partikel dan indeks polidispersitas dengan menggunakan Particle Size Analized (PSA) serta efisiensi penjeratan sinkonin dengan menggunakan KCKT. Temperatur gelasi (Tg) span 60 45±2 oC, kecepatan rotavapor pembentukan film lapis tipis niosom 210 rpm, temperatur hidrasi 55±2 oC, kecepatan rotavapor hidrasi 210 rpm, waktu hidrasi 20 menit, waktu sonikasi suspensi niosom 1 menit. Ukuran vesikel yang diperoleh adalah 100–200 nm, indeks polidispersitas 0,2–0,4 dan efisiensi penjeratan niosom sinkonin 84,49±0,0025%. Proses pembuatan niosom sinkonin memiliki pengaruh besar terhadap hasil ukuran vesikel dan efisiensi penjeratan niosom sinkonin.


Author(s):  
Sheila Liza B. Dal

Abstract The choice of epoxy mold compound (EMC) for an electronic package is based mostly on how much protection it provides to the active components in the package. But the choice is not a straightforward process. Rather it is mostly trial and error using different assembly parameters to find the most robust material while assembly defects are monitored. One such defect associated to EMC processing is wire sweep, and many studies have shown that it is mainly caused by viscosity changes in the EMC. In this study, samples of EMC in various stages of shelf life and staging times were analyzed for degree of cure using a method called differential scanning calorimetry (DSC). Samples are then processed at assembly for wire sweep measurement. It was found out that degree of cure increases with staging time at different rates for each shelf life. It was also found out that wire sweep did not only increase with degree of cure but it was also found to be predictable with respect to the latter. Using this information, the age and staging limit for each material was identified that would not cause wire sweep issues.


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