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Biblioteca(s): |
Embrapa Instrumentação. |
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Data corrente: |
19/03/2025 |
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Data da última atualização: |
19/03/2025 |
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Tipo da produção científica: |
Artigo em Periódico Indexado |
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Autoria: |
TOBIAS, T. J.; MORAES, T. B.; COLNAGO, L. A. |
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Afiliação: |
UNIVERSITY OF SAO PAULO (USP); UNIVERSITY OF SAO PAULO (USP); LUIZ ALBERTO COLNAGO, CNPDIA. |
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Título: |
Establishing optimal parameters to mitigate the heating effects caused by CPMAS sequence in 13C solid-state NMR studies of cocoa butter and other fat samples. |
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Ano de publicação: |
2025 |
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Fonte/Imprenta: |
Food Research International, v. 204,115944, 2025. |
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Páginas: |
9 p. |
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ISSN: |
0963-9969 |
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DOI: |
https://doi.org/10.1016/j.foodres.2025.115944 |
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Idioma: |
Inglês |
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Conteúdo: |
The physical and chemical properties of solid triacylglycerols (fats) have been investigated through the use of 13C solid-state nuclear magnetic resonance (SS-NMR). However, the 13C SS-NMR experiments performed with crosspolarization (CP), magic angle sample spinning (MAS) and high power for 1 H decoupling (DEC), known as CPMAS, have the potential to increase sample temperature, which may disrupt the solid–liquid content, crystallization dynamics, and polymorphism of the fat samples. While the heating effects observed in CPMAS experiments have been well documented, they have not yet been studied in fat samples. Accordingly, the present study examines the influence of sample spinning frequencies (SF) and radio frequency irradiation (RFI) due to DEC, on sample heating using cocoa butter (CB), chocolate, and animal fats. The results of the variation in the 1 H chemical shift of the water peak in the butter sample indicate that the use of routine CPMAS parameter results in an increase in sample temperature of up to 15 ◦C. This temperature is sufficient to affect various physicochemical properties of fats, including partial or total melting when the experiments are performed with an air stream at ambient temperature. The results demonstrate that a SF of approximately 3 kHz and a recycle delay exceeding 10 s for a decoupler power of 70 W for 50 ms result in an increase of less than 1 ◦C in sample temperature in 13C CPMAS experiments. These experimental conditions were successfully employed to study the CB crystallization process, which exhibited the presence of the α form at the beginning of the process and the β form at its conclusion. MenosThe physical and chemical properties of solid triacylglycerols (fats) have been investigated through the use of 13C solid-state nuclear magnetic resonance (SS-NMR). However, the 13C SS-NMR experiments performed with crosspolarization (CP), magic angle sample spinning (MAS) and high power for 1 H decoupling (DEC), known as CPMAS, have the potential to increase sample temperature, which may disrupt the solid–liquid content, crystallization dynamics, and polymorphism of the fat samples. While the heating effects observed in CPMAS experiments have been well documented, they have not yet been studied in fat samples. Accordingly, the present study examines the influence of sample spinning frequencies (SF) and radio frequency irradiation (RFI) due to DEC, on sample heating using cocoa butter (CB), chocolate, and animal fats. The results of the variation in the 1 H chemical shift of the water peak in the butter sample indicate that the use of routine CPMAS parameter results in an increase in sample temperature of up to 15 ◦C. This temperature is sufficient to affect various physicochemical properties of fats, including partial or total melting when the experiments are performed with an air stream at ambient temperature. The results demonstrate that a SF of approximately 3 kHz and a recycle delay exceeding 10 s for a decoupler power of 70 W for 50 ms result in an increase of less than 1 ◦C in sample temperature in 13C CPMAS experiments. These experimental conditions were successfully... Mostrar Tudo |
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Palavras-Chave: |
CPMAS; Sample heating; Solid state NMR. |
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Categoria do assunto: |
-- |
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Marc: |
LEADER 02380naa a2200217 a 4500
001 2174050
005 2025-03-19
008 2025 bl uuuu u00u1 u #d
022 $a0963-9969
024 7 $ahttps://doi.org/10.1016/j.foodres.2025.115944$2DOI
100 1 $aTOBIAS, T. J.
245 $aEstablishing optimal parameters to mitigate the heating effects caused by CPMAS sequence in 13C solid-state NMR studies of cocoa butter and other fat samples.$h[electronic resource]
260 $c2025
300 $a9 p.
520 $aThe physical and chemical properties of solid triacylglycerols (fats) have been investigated through the use of 13C solid-state nuclear magnetic resonance (SS-NMR). However, the 13C SS-NMR experiments performed with crosspolarization (CP), magic angle sample spinning (MAS) and high power for 1 H decoupling (DEC), known as CPMAS, have the potential to increase sample temperature, which may disrupt the solid–liquid content, crystallization dynamics, and polymorphism of the fat samples. While the heating effects observed in CPMAS experiments have been well documented, they have not yet been studied in fat samples. Accordingly, the present study examines the influence of sample spinning frequencies (SF) and radio frequency irradiation (RFI) due to DEC, on sample heating using cocoa butter (CB), chocolate, and animal fats. The results of the variation in the 1 H chemical shift of the water peak in the butter sample indicate that the use of routine CPMAS parameter results in an increase in sample temperature of up to 15 ◦C. This temperature is sufficient to affect various physicochemical properties of fats, including partial or total melting when the experiments are performed with an air stream at ambient temperature. The results demonstrate that a SF of approximately 3 kHz and a recycle delay exceeding 10 s for a decoupler power of 70 W for 50 ms result in an increase of less than 1 ◦C in sample temperature in 13C CPMAS experiments. These experimental conditions were successfully employed to study the CB crystallization process, which exhibited the presence of the α form at the beginning of the process and the β form at its conclusion.
653 $aCPMAS
653 $aSample heating
653 $aSolid state NMR
700 1 $aMORAES, T. B.
700 1 $aCOLNAGO, L. A.
773 $tFood Research International$gv. 204,115944, 2025.
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Embrapa Instrumentação (CNPDIA) |
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| 1. |  | TENÓRIO, J. S.; MIELE, M.; PIMENTA, C. L.; SANTOS, L. D. dos; BARROS, E. C.; BERNARDES, E.; BENELLI, D. A.; ROSA, K. V.; BLAINSK, J. L. Assistência técnica digital para a gestão ambiental na suinocultura. In: SALÃO INTERNACIONAL DE PROTEÍNA ANIMAL; INTERNATIONAL ANIMAL PROTEIN TRADE SHOW, 2024, São Paulo. Relatório SIAVS 2024. São Paulo: Associação Brasileira de Proteína Animal, 2024. p.154-156.| Tipo: Artigo em Anais de Congresso |
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