Etude thermoanalytique de substances psychotherapeutiques. II. Substances antipsychotiques. Chlorprothixene,chlorhydrate de chlorpromazine,chlorhydrate de levomepromazine,dichlorhydrate de fluphenazine

The thermoanalytical study of chlorprothixene (a), chlorpromazine hydrochloride (b), levomepromazine hydrochloride (c), and fluphenazine hydrochloride (d), has enabled the existence of polymorphs for (b) and (d) to be shown. The thermal stability and decomposition kinetics of commercial forms of the drugs have been determined. The thermal behaviour of (c) and (d) does not permit their study by transparency method nor the determination of their degree of purity by differential scanning calorimetry. The temperatures and intervals of fusion are given for (a) and (b). Knowing the thermal behaviour, the degree of purity: 99.47 ± 0.11% (a), 99.61 ± 0.20% (b); enthalpy: 27.82 ± 1.05 (a), 28.42 ± 0.57 (b) kJ mole^?1; and entropy of fusion have been evaluated by differential scanning calorimetry.     

Gd10C4Cl18 und Gd10C4Cl17, zwei Seltenerdmetall-Clusterverbindungen mit interstitiellen C2-Gruppen

Gd₁₀C₄Cl₁₈ and Gd₁₀C₄Cl₁₇, Two Lanthanoid Cluster Compounds with Interstitial C₂ Units The compounds Gd₁₀C₄Cl₁₈ ( I ) and Gd₁₀C₄Cl₁₇ ( II ) are prepared by heating stoichiometric amounts of GdCl₃, Gd, and graphite in sealed tantalum tubes at 1070 ( I ) and 1 120 K ( II ). Single crystal investigations ( I : P2₁/c, Z = 2, a = 918.2, b = 1 612.0, c = 1 288.6 pm, β = 119.86°; II : P1 , Z = 1, a = 849.8, b = 917.4, c = 1 146.2 pm, α = 104.56°, β = 95.98°, γ = 111.35°) revealed the occurrence of novel Gd₁₀C₄Cl₁₈ clusters. The metal framework is formed by edge-sharing of two Gd₆ octahedra. These are centred by C₂ units (d_{C? C} = 147 pm) and Cl atoms bridge all available edges of the octahedra. The structure of I corresponds to a packing of such quasi molecular clusters, in II they are linked to chains via common Cl atoms. Both structures are discussed in terms of a model of close packed spheres as well as in the concept of condensed clusters.     

Détermination de la pureté de la sulfapyridine s par analyse thermométrique

Résumé L'étude thermoanalytique de la pureté de deux échantillons de sulfapyridine, médicament (I) et standard (II), a été réalisée par différentes méthodes. Par mesure de la transparence les valeurs moyennes de la température et du domaine de fusion indiquent une teneur en impureté plus faible pour (II) que pour (I). Disposant de deux analyseurs thermiques de conception différente, les auteurs ont montré l'excellente concordance des résultats: 99.790 ± 0.047 % et 99.800 ± 0.045 % (I). Seule l'analyse calorimétrique différentielle permet d'évaluer avec précision le taux de pureté de (II) 99.956 ± 0.028 %, valeur représentant un seuil pour l'analyse calorimétrique différentielle à compensation de puissance (DSC 1B).

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The thermoanalytical purities of two sulfapyridine samples, drug (I) and standard (II), have been studied with different methods. By transparency measurement the fusion temperatures and intervals indicate a lower percentage of impurity for (II) than for (I). By means of two thermal analyzers the authors have shown the good agreement of the results: 99.790±0.047% and 99.800±0.045% (I). Heat-flux differential scanning calorimetry is the only method able to give precisely the degree of purity of (II): 99.956±0.028 %, this value being a limit for the power-compensation differential scanning calorimetry analysis (DSC 1B).

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Zusammenfassung Das Studium der thermoanalytischen Reinheit der beiden Sulfapyridinproben drag(I) und standard(II) wurde durch verschiedene Methoden durchgeführt. Schmelztemperaturen sowie-bereiche zeigen im Falle von Transparenzmessungen einen geringeren Prozentsatz von Verunreinigungen für (II) als für (I). Unter Anwendung zweier Thermoanalyser zeigten die Autoren die gute Übereinstimmung der Ergebnisse: 99.790±0.047% und 99.800 ± 0.045 % für (I). Ein Wärmeströmungs-Differentialabtastkalorimeter bietet die einzige Möglichkeit den Reinheitsgrad von (II) genau zu bestimmen: 99.956 ± 0.028 %, wobei dieser Wert die Grenze für die Kraft-Kompensations-Differentialkalorimetrie (DSC 1B) darstellt.

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: (I) (II). , , II , I. , : 99.790±0.047% 99.800 ± 0.045% I. II: 99.956 ± 0.028% ( 1).

     

微乳液的热力学性质 I: 芳烃类的侧链链长对微乳液热力学函数影响

本文研究以非离子型表面活性剂-正辛醇-水-芳烃类所组成的微乳液, 探讨醇从油相转移到界面相时的自由能变化, 以及温度对自由能的影响。计算出熵和焓的变化, 发现在实验范围内, 上述热力学函数的对数值与芳烃侧链的碳原子数(n)呈线性关系。这些关系式对微乳液的构成和稳定性的讨论是重要的, 还对几种芳烃异构体所构成的微乳液的热力学函数进行了实验和讨论。     

AutoLink: automated sequential resonance assignment of biopolymers from NMR data by relative-hypothesis-prioritization-based simulated logic

We have developed a new computer algorithm for determining the backbone resonance assignments for biopolymers. The approach we have taken, relative hypothesis prioritization, is implemented as a Lua program interfaced to the recently developed computer-aided resonance assignment (CARA) program. Our program can work with virtually any spectrum type, and is especially good with NOESY data. The results of the program are displayed in an easy-to-read, color-coded, graphic representation, allowing users to assess the quality of the results in minutes. Here we report the application of the program to two RNA recognition motifs of Apobec-1 Complementation Factor. The assignment of these domains demonstrates AutoLink's ability to deliver accurate resonance assignments from very minimal data and with minimal user intervention.     

Bacteria encapsulation in colloidal inorganic matrices: Is it a general method?

Zirconium oxyhydroxide nanoparticles prepared by an aqueous route were evaluated for Escherichia coli bacteria encapsulation. A low viability rate was measured 24 hours after immobilization that could be attributed to nanoparticle cytotoxicity. Moreover, the presence of glycerol, a long-term cell-preserving molecule, hindered gel formation, probably due to its adsorption on the nanoparticle surface. A comparison with boehmite and ferrihydrite gels previously synthesized following a similar aqueous colloidal route suggests that the generalization of this method will rely on a careful control of the nanoparticle surface reactivity and may require surface chemical modification.     

The effect of pH on the separation of manure nutrients with reverse osmosis membranes

This paper reports on the effect of pH on the retention of dry matter (DM), total ammonia-nitrogen (TAN), potassium, phosphorus and volatile fatty acids (VFAs) during the filtration of pretreated swine manure by three highly selective reverse osmosis (RO) membranes. The manure was pretreated using various combinations of biological and physical technologies, namely anaerobic digestion (AD), vacuum filtration through diatomaceous earth (DE), nanofiltration (NF), and a first stage RO filtration. The objective was to establish the level of acidification required to optimize permeate quality while minimizing chemical addition.     

Etude thermoanalytique et spectrale de l'interaction lorazepam/PEG 6000

Résumé The solubility and rate of dissolution of a poorly-soluble active principle are of importance when substances are destined for oral administration. Physical blends in wich drug and carrier are able to form particular compositions, such as a eutectic, may exibit an increased rate of dissolution. In this work the interactions lorazepam and PEG 6000, were examined, the particular thermal behaviour of lorazepam being taken into account. An eutectic was obtained and its composition was studied by means of differential scanning calorimetry, thermomicroscopy, infrared spectroscopy and X-ray methods.

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Zusammenfassung Bei der oralen Darreichung von Substanzen ist die L?slichkeit und Aufl?sungsgeschwindigkeit schlechtl?slicher aktiver Komponenten von gro?er Bedeutung. Physikalische Gemische, in denen Wirkstoffe und Tr?gersubstanzen besondere Zusammensetzungen wie zum Beispiel Eutektika zu bilden in der Lage sind, k?nnen eine erh?hte Aufl?sungsgeschwindigkeit zeigen. Vorliegend wird die Wechselwirkung zwischen Lorazepam und PEG 6000 untersucht, wobei das besondere thermische Verhalten von Lorazepam berücksichtigt wurde. Es wurde ein Eutektikum erhalten und dessen Zusammensetzung mittels DSC, Thermomikroskopie, Infrarotspektroskopie und R?ntgenmethoden untersucht.