scholarly journals Preparation of DPPC liposomes using probe-tip sonication: investigating intrinsic factors affecting temperature phase transitions

2019 ◽  
Author(s):  
Monica D. Rieth ◽  
Andrew Lozano

AbstractLiposomes are an important tool and have gained much attention for their promise as an effective means of delivering small therapeutic compounds to targeted sites. In an effort to establish an effective method to produce liposomes from the lipid, dipalmitoyl-phosphatidylcholine or DPPC, we have found important aspects that must be taken into consideration. Here, we used probe-tip sonication to prepare liposomes on a batch scale. During this process we uncovered interesting steps in their preparation that altered the thermodynamic properties and phase transitions of the resulting liposome mixtures. Using differential scanning calorimetry to assess this we found that increasing the sonication time had the most dramatic effect on our sample, producing almost an entirely separate phase transition relative to the main phase transition. This result is consistent with reports from the current literature. We also highlight a smaller transition, which we attribute to traces of unincorporated lipid that seems to gradually disappear as the total lipid concentration decreases. Overall, sonication is an effective means of producing liposomes, but we cannot assert this method is optimal in producing them with precise physical properties. Here we highlight the physical effects at play during this process.

1999 ◽  
Vol 14 (1) ◽  
pp. 83-89 ◽  
Author(s):  
Jung-Kun Lee ◽  
Hyuk-Joon Youn ◽  
Kug Sun Hong

Morphotropic phase boundaries and temperature dependent phase transitions of (1 – x) PbZrO3 + x (Na1/2Bi1/2)TiO3 (0.01 ≤ x ≤ 0.15) solid solutions were investigated by x-ray diffraction, differential scanning calorimetry (DSC), and dielectric property analysis. Two morphotropic phase transitions at room temperature were found at x = 0.1 and 0.13, which were from antiferroelectric orthorhombic (with 4 × 4 × 2 superlattice [orthorhombic (I)]) to antiferroelectric orthorhombic (with 2 × 2 × 2 superlattice [orthorhombic (II)]) and from orthorhombic (II) to ferroelectric rhombohedral, respectively. With increasing temperature, the samples with 0.01 ≤ x < 0.1 showed two phase transitions, i.e., from orthorhombic (I) to orthorhombic (II) and from orthorhombic (II) to cubic. The other samples had only one phase transition with increasing temperature. Phase transition temperatures of all the samples were measured using DSC, and a phase diagram for the solid solutions was constructed. A model illustrating the antiparallel shift of Pb ions in the orthorhombic (II) phase was also proposed.


Author(s):  
Yuan Chen ◽  
Yang Liu ◽  
Binzu Gao ◽  
Chuli Zhu ◽  
Zunqi Liu

Two novel inorganic&ndash;organic hybrid supramolecular assemblies, namely, (4-HNA)(18-crown-6)(HSO4) (1) and (4-HNA)2(18-crown-6)2(PF6)2(CH3OH) (2) (4-HNA = 4-nitroanilinium), were synthesized and characterized by infrared spectroscopy, single X-ray diffraction, differential scanning calorimetry (DSC), and temperature-dependent dielectric measurements. The two compounds underwent reversible phase transitions at about 255 K and 265 K, respectively. These phase transitions were revealed and confirmed by the thermal anomalies in DSC measurements and abrupt dielectric anomalies during heating. The phase transition may have originated from the [(4-HNA)(18-crown-6)]+ supramolecular cation. The inorganic anions tuned the crystal packings and thus influenced the phase-transition points and types. The variable-temperature X-ray diffraction data for crystal 1 revealed the occurrence of a phase transition in the high-temperature phase with the space group of P21/c and in the low-temperature phase with the space group of P21/n. Crystal 2 exhibited the same space group P21/c at different temperatures. The results indicated that crystals 1 and 2 both underwent an iso-structural phase transition.


Author(s):  
Tamara J. Bednarchuk ◽  
Wolfgang Hornfeck ◽  
Vasyl Kinzhybalo ◽  
Zhengyang Zhou ◽  
Michal Dušek ◽  
...  

The organic–inorganic hybrid compound 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2] (4apFeS), was obtained by slow evaporation of the solvent at room temperature and characterized by single-crystal X-ray diffraction in the temperature range from 290 to 80 K. Differential scanning calorimetry revealed that the title compound undergoes a sequence of three reversible phase transitions, which has been verified by variable-temperature X-ray diffraction analysis during cooling–heating cycles over the temperature ranges 290–100–290 K. In the room-temperature phase (I), space group C2/c, oxygen atoms from the closest Fe-atom environment (octahedral) were disordered over two equivalent positions around a twofold axis. Two intermediate phases (II), (III) were solved and refined as incommensurately modulated structures, employing the superspace formalism applied to single-crystal X-ray diffraction data. Both structures can be described in the (3+1)-dimensional monoclinic X2/c(α,0,γ)0s superspace group (where X is ½, ½, 0, ½) with modulation wavevectors q = (0.2943, 0, 0.5640) and q = (0.3366, 0, 0.5544) for phases (II) and (III), respectively. The completely ordered low-temperature phase (IV) was refined with the twinning model in the triclinic P{\overline 1} space group, revealing the existence of two domains. The dynamics of the disordered anionic substructure in the 4apFeS crystal seems to play an essential role in the phase transition mechanisms. The discrete organic moieties were found to be fully ordered even at room temperature.


2010 ◽  
Vol 66 (3) ◽  
pp. 387-395 ◽  
Author(s):  
Heng-Yun Ye ◽  
Li-Zhuang Chen ◽  
Ren-Gen Xiong

Pyridinium-3-carboxylic acid perchlorate was synthesized and separated as crystals. Differential scanning calorimetry (DSC) measurements show that this compound undergoes a reversible phase transition at ∼ 135 K with a wide hysteresis of 15 K. Dielectric measurements confirm the transition at ∼ 127 K. Measurement of the unit-cell parameters versus temperature shows that the values of the c axis and β angle change abruptly and remarkably at 129 (2) K, indicating that the system undergoes a first-order transition at T c = 129 K. The crystal structures determined at 103 and 298 K are all monoclinic in P21/c, showing that the phase transition is isosymmetric. The crystal contains one-dimensional hydrogen-bonded chains of the pyridinium-3-carboxylic acid cations, which are further linked to perchlorate anions by hydrogen bonds to form well separated infinite planar layers. The most distinct differences between the structures of the higher-temperature phase and the lower-temperature phase are the change of the distance between the adjacent pyridinium ring planes within the hydrogen-bonded chains and the relative displacement between the hydrogen-bonded layers. Structural analysis shows that the driving force of the transition is the reorientation of the pyridinium-3-carboxylic acid cations. The degree of order of the perchlorate anions may be a secondary order parameter.


2014 ◽  
Vol 70 (12) ◽  
pp. 1153-1160 ◽  
Author(s):  
Jan Fábry ◽  
Michal Dušek ◽  
Přemysl Vaněk ◽  
Iegor Rafalovskyi ◽  
Jiří Hlinka ◽  
...  

The structures of 4-chloro-3-nitroaniline, C6H5ClN2O2, (I), and 4-iodo-3-nitroaniline, C6H5IN2O2, (II), are isomorphs and both undergo continuous (second order) phase transitions at 237 and 200 K, respectively. The structures, as well as their phase transitions, have been studied by single-crystal X-ray diffraction, Raman spectroscopy and difference scanning calorimetry experiments. Both high-temperature phases (293 K) show disorder of the nitro substituents, which are inclined towards the benzene-ring planes at two different orientations. In the low-temperature phases (120 K), both inclination angles are well maintained, while the disorder is removed. Concomitantly, thebaxis doubles with respect to the room-temperature cell. Each of the low-temperature phases of (I) and (II) contains two pairs of independent molecules, where the molecules in each pair are related by noncrystallographic inversion centres. The molecules within each pair have the same absolute value of the inclination angle. The Flack parameter of the low-temperature phases is very close to 0.5, indicating inversion twinning. This can be envisaged as stacking faults in the low-temperature phases. It seems that competition between the primary amine–nitro N—H...O hydrogen bonds which form three-centred hydrogen bonds is the reason for the disorder of the nitro groups, as well as for the phase transition in both (I) and (II). The backbones of the structures are formed by N—H...N hydrogen bonding of moderate strength which results in the graph-set motifC(3). This graph-set motif forms a zigzag chain parallel to the monoclinicbaxis and is maintained in both the high- and the low-temperature structures. The primary amine groups are pyramidal, with similar geometric values in all four determinations. The high-temperature phase of (II) has been described previously [Gardenet al.(2004).Acta Cryst.C60, o328–o330].


1990 ◽  
Vol 68 (4) ◽  
pp. 604-611 ◽  
Author(s):  
Julian Haines ◽  
D. F. R. Gilson

The phase transition behaviour of cycloheptene has been investigated by differential scanning calorimetry, proton spin-lattice relaxation, and vibrational spectroscopy (infrared and Raman). Two solid–solid phase transitions were observed, at 154 and 210 K, with transition enthalpies and entropies of 5.28 and 0.71 kJ mol−1 and 34.3 and 3.4 JK−1, respectively. Cycloheptene melted at 217 K with an entropy of melting of 4.5 JK−1 mol−1. The bands in the vibrational spectra of the two high temperature phases were broad and featureless, characteristic of highly disordered phases. The presence of other conformers, in addition to the chair form, was indicated from bands in the spectra. The ring inversion mode was highly phase dependent and exhibited soft mode type behaviour prior to the transition from the low temperature phase. The low frequency Raman spectra (external modes) of these phases indicated that the molecules are undergoing isotropic reorientation. In the low temperature phase, the vibrational bands were narrow; the splitting of the fundamentals into two components and the presence of nine external modes are consistent with unit cell symmetry of either C2 or Cs with two molecules per primitive unit cell. A glassy state can be produced from the intermediate phase and the vibrational spectra were very similar to those of the high temperature phases, indicating that static disorder was present. The barriers to reorientation, as obtained from proton spin-lattice relaxation measurements, are 9.0 kJ mol−1 in both the high temperature phases, and 15.4 kJ mol−1 in the low temperature, ordered phase. Keywords: cycloheptene, phase transition, differential scanning calorimetry, NMR, vibrational spectroscopy.


2018 ◽  
Vol 1 ◽  
pp. 10-17 ◽  
Author(s):  
Victoriya Gnitsevych ◽  
Tatiana Yudina ◽  
Liudmyla Deinychenko ◽  
Radion Nykyforov ◽  
Iryna Nazarenko

The aim of this article is to investigate changes in the structure, color and microbiological parameters of milk-protein concentrates (MPC) made of buttermilk with the use of cranberry or viburnum purees in the process of storage. Necessary results were obtained after analyzing phase transitions, changes in color-parametric and microbiological characteristics of the studied products. Low-temperature phase transitions and their influence on the structure of MPC were investigated using the method of differential scanning calorimetry. This method was used to obtain information on the change in the temperature function, depending on the change in heat absorption typical for melting, crystallization, or glass transition of components of MPC. The obtained dependences indicated an increase of heat absorption leaps of concentrates in relation to control, which indicates an increase in the amount of bound moisture and, accordingly, a decrease in significant changes in the structure of concentrates in the process of storage. In addition, it was found that rational was the rapid freezing of MPC at a temperature of –20...–30 ° C. The CIE XYZ and CIELab methods were used to evaluate the change in the color-parametric characteristics of MPC. According to the data obtained, red or yellow spectral tone dominates for the samples, but with an increase in the storage time, one can see a significant shift in the color of both concentrates towards the yellow color. It is also established that with increasing of storage time there is a gradual darkening of MPC. It was defined, that rational was the shelf life of up to 30 days from the time of studied products making. It was also determined that with the use of deep freezing of the MPC, the storage time has no significant effect on the development of the microflora.


2022 ◽  
Vol 130 (1) ◽  
pp. 84
Author(s):  
А.С. Крылов ◽  
А.Н. Втюрин ◽  
И.А. Гудим ◽  
И.В. Немцев ◽  
С.Н. Крылова

The Raman spectra of four crystals of TbFe3-хGax (BO3) 4 solid solutions (x from 0 to 0.54) were studied in the temperature range from 8 to 350 K. The temperatures of structural phase transitions were determined. The observed spectral behavior is characteristic to condensation and restoration of soft modes. Soft modes are associated with a structural phase transition from the R32 phase to the P3121 phase. The Compositions-Temperature phase diagram was constructed


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