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  • Author or Editor: Zsuzsanna Éhen x
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Abstract  

Citronellol and citronellyl acetate have been entrapped with α-, β- and γ-cyclodextrin (CD). Evolved gas detection and TG-MS coupling was applied to prove the actual inclusion complex formation between monoterpens and CDs. The terpene content was determined by UV-VIS specrophotometry and RP-HPLC and the effect of storage time on the terpene content was also investigated. The α- and γ-cyclodextrin inclusion complexes showed higher thermal stabilities vs. dynamic heating compared to the β-CD complexes. On the contray, the retention of guest using β-cyclodextrin even after 10 years of storage was much more pronounced. Experimental data other than 1:1 complex compositions are assumed. Molecular modeling experiments also suggested multiple complex compositions.

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Summary Thermoanalytical techniques (TG, DSC) are frequently used in the investigation of the thermal properties of cyclodextrins and their inclusion complexes. However, the above techniques do not provide information on the chemical composition of the evolved fragments upon the thermal decomposition. In this study &-, &- and &-cyclodextrins and 4 methylated and 3 ethylated &-CD derivatives were investigated with a TG-MS combined thermoanalytical technique in order to get information about their fragmentation behaviour. By comparison of the TG/DTA curves, a different thermal behaviour was found for each of the native and the chemically modified cyclodextrins. Except for the water loss profiles and the solid-solid phase transformations, the thermal behaviour of the (investigated) native CDs do not show remarkable differences. However, the chemical modification of the native &-CD resulting in a new compound may change the strength of interactions between host and guest causing differences in the thermal stabilities of the derivatives. The mass spectrometry results supported the observed thermal differences and showed significant alterations in the fragmentation of ethylated and methylated compounds. The investigated natural CDs possess a very similar fragmentation profile, due to the common &-D-glucopyranose building units. In the case of modified CDs characteristic signals of the substituents are present.

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Journal of Thermal Analysis and Calorimetry
Authors:
Alaize de Martins
,
A. Craveiro
,
M. Machado
,
Fernanda Raffin
,
T. Moura
,
Cs. Novák
, and
Zsuzsanna Éhen

Abstract  

Inclusion complex between the essential oil of Mentha x villosa Hudson and β-cyclodextrin, with a 1:9 mass/mass oil–β-cyclodextrin ratio was prepared by co-precipitation and kneading methods in a hydroethanolic medium. The GC/MS analysis showed a total volatile content of 99.5% in the Mentha x villosa oil. The characterization of the complex involved the analysis of the original essential oil, the surface and the total extracted oils. Among 28 detected compounds in the original essential oil, 13 are monoterpenes and 10 sesquiterpenes, furthermore, piperitenone-oxide is the major component (35.4%). 12 compounds were totally and 11 partially complexed, 3 have been adsorbed only on the surface of the β-CD and 2 have not been detected neither in the surface oil nor in the complexed oil. A 13.6% encapsulation efficiency was observed, while the total oil and volatiles retention was 15 and 77%, respectively. Non-parametric statistic analysis of the data showed that the profile of the volatiles were not significantly different comparing the original oil and the complexed oil (p>0.04). The results of thermogravimetry-mass spectrometry and XRD analysis have proven the inclusion complex formation between the essential oil and cyclodextrin.

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Abstract  

Thermogravimetry (TG) and mass spectrometry (MS) combined techniques have been used to investigate the thermal degradation and catalytic decomposition of high-density polyethylene (HDPE) over solid acid catalysts as H-ZSM-5, Al-MCM-41 and a hybrid material with a bimodal pore size distribution (H-ZSM-5/Al-MCM-41). The silicon/aluminum ratio of all catalysts is 15. Both thermal and catalytic processes showed total conversion in a single mass loss step. Furthermore, the catalytic conversion presents average reduction of 27.4%, in the onset decomposition temperature. The kinetic parameters were calculated using non-isothermal method. These parameters do not indicate significant differences between the thermal and catalytic processes. Even though, the presence of the catalysts changes the reaction mechanism, from phase boundary controlled reaction to random nucleation mechanism. Important difference in distribution of evolved products was detected when several catalysts were used. However, in all cases the main products were alkanes (C2, C3 and C4), alkenes (C3 and C4), dienes (C4 and C5) and traces of aromatic compounds.

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