The Effect of Milling on the Ethanolic Extract Composition of Dried Walnut (<i>Juglans regia</i> L.) Shells

This study investigates the ethanolic extract of dried walnut (<i>Juglans regia</i> L.) shells upon hammer milling (HM) and ball milling (BM) grinding processes. Marked differences were observed in the attenuated total reflection Fourier-transform infrared (ATR-FTIR) spectra. The two ext...

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Main Authors: Giovanni Ventura, Davide Mesto, Davide Blasi, Tommaso R. I. Cataldi, Cosima Damiana Calvano
Format: Article
Language:English
Published: MDPI AG 2023-08-01
Series:International Journal of Molecular Sciences
Subjects:
Online Access:https://www.mdpi.com/1422-0067/24/17/13059
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author Giovanni Ventura
Davide Mesto
Davide Blasi
Tommaso R. I. Cataldi
Cosima Damiana Calvano
author_facet Giovanni Ventura
Davide Mesto
Davide Blasi
Tommaso R. I. Cataldi
Cosima Damiana Calvano
author_sort Giovanni Ventura
collection DOAJ
description This study investigates the ethanolic extract of dried walnut (<i>Juglans regia</i> L.) shells upon hammer milling (HM) and ball milling (BM) grinding processes. Marked differences were observed in the attenuated total reflection Fourier-transform infrared (ATR-FTIR) spectra. The two extracts were investigated by reversed-phase liquid chromatography coupled with electrospray ionization and high-resolution mass spectrometry (RPLC-ESI-HRMS). Following enzymatic digestion, the fatty acids (FAs) were examined, and tandem MS of epoxidized species was applied to establish the C-C double bond position; the most abundant species were FA 18:2 Δ<sup>9,12</sup>, FA 18:1 Δ<sup>9</sup>, and FA 18:3 Δ<sup>9,12,15</sup>. However, no significant qualitative differences were observed between FAs in the two samples. Thus, the presence of potential active secondary metabolites was explored, and more than 30 phenolic compounds, including phenols, ellagic acid derivatives, and flavonoids, were found. Interestingly, the HM samples showed a high concentration of ellagitannins and hydrolyzable tannins, which were absent in the BM sample. These findings corroborate the greater phenolic content in the HM sample, as evaluated by the Folin–Ciocalteu test. Among the others, the occurrence of lanceoloside A at <i>m</i>/<i>z</i> 391.1037 [C<sub>19</sub>H<sub>20</sub>O<sub>9</sub>-H]<sup>−</sup>, and a closely related benzoyl derivate at <i>m</i>/<i>z</i> 405.1190 (C<sub>20</sub>H<sub>22</sub>O<sub>9</sub>-H]<sup>−</sup>), was ascertained. The study provides valuable information that highlights the significance of physical pre-treatments, such as mill grinding, in shaping the composition of extracts, with potential applications in the biorefinery or pharmaceutical industries.
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spelling doaj.art-2f8fb0ea8d1c4b68b468f127b86686c82023-11-19T08:11:48ZengMDPI AGInternational Journal of Molecular Sciences1661-65961422-00672023-08-0124171305910.3390/ijms241713059The Effect of Milling on the Ethanolic Extract Composition of Dried Walnut (<i>Juglans regia</i> L.) ShellsGiovanni Ventura0Davide Mesto1Davide Blasi2Tommaso R. I. Cataldi3Cosima Damiana Calvano4Department of Chemistry, University of Bari Aldo Moro, Via Orabona 4, 70126 Bari, ItalyDepartment of Chemistry, University of Bari Aldo Moro, Via Orabona 4, 70126 Bari, ItalyDepartment of Chemistry, University of Bari Aldo Moro, Via Orabona 4, 70126 Bari, ItalyDepartment of Chemistry, University of Bari Aldo Moro, Via Orabona 4, 70126 Bari, ItalyDepartment of Chemistry, University of Bari Aldo Moro, Via Orabona 4, 70126 Bari, ItalyThis study investigates the ethanolic extract of dried walnut (<i>Juglans regia</i> L.) shells upon hammer milling (HM) and ball milling (BM) grinding processes. Marked differences were observed in the attenuated total reflection Fourier-transform infrared (ATR-FTIR) spectra. The two extracts were investigated by reversed-phase liquid chromatography coupled with electrospray ionization and high-resolution mass spectrometry (RPLC-ESI-HRMS). Following enzymatic digestion, the fatty acids (FAs) were examined, and tandem MS of epoxidized species was applied to establish the C-C double bond position; the most abundant species were FA 18:2 Δ<sup>9,12</sup>, FA 18:1 Δ<sup>9</sup>, and FA 18:3 Δ<sup>9,12,15</sup>. However, no significant qualitative differences were observed between FAs in the two samples. Thus, the presence of potential active secondary metabolites was explored, and more than 30 phenolic compounds, including phenols, ellagic acid derivatives, and flavonoids, were found. Interestingly, the HM samples showed a high concentration of ellagitannins and hydrolyzable tannins, which were absent in the BM sample. These findings corroborate the greater phenolic content in the HM sample, as evaluated by the Folin–Ciocalteu test. Among the others, the occurrence of lanceoloside A at <i>m</i>/<i>z</i> 391.1037 [C<sub>19</sub>H<sub>20</sub>O<sub>9</sub>-H]<sup>−</sup>, and a closely related benzoyl derivate at <i>m</i>/<i>z</i> 405.1190 (C<sub>20</sub>H<sub>22</sub>O<sub>9</sub>-H]<sup>−</sup>), was ascertained. The study provides valuable information that highlights the significance of physical pre-treatments, such as mill grinding, in shaping the composition of extracts, with potential applications in the biorefinery or pharmaceutical industries.https://www.mdpi.com/1422-0067/24/17/13059biomassepoxidationfatty acidsLC-MS/MSmill grindingphenols
spellingShingle Giovanni Ventura
Davide Mesto
Davide Blasi
Tommaso R. I. Cataldi
Cosima Damiana Calvano
The Effect of Milling on the Ethanolic Extract Composition of Dried Walnut (<i>Juglans regia</i> L.) Shells
International Journal of Molecular Sciences
biomass
epoxidation
fatty acids
LC-MS/MS
mill grinding
phenols
title The Effect of Milling on the Ethanolic Extract Composition of Dried Walnut (<i>Juglans regia</i> L.) Shells
title_full The Effect of Milling on the Ethanolic Extract Composition of Dried Walnut (<i>Juglans regia</i> L.) Shells
title_fullStr The Effect of Milling on the Ethanolic Extract Composition of Dried Walnut (<i>Juglans regia</i> L.) Shells
title_full_unstemmed The Effect of Milling on the Ethanolic Extract Composition of Dried Walnut (<i>Juglans regia</i> L.) Shells
title_short The Effect of Milling on the Ethanolic Extract Composition of Dried Walnut (<i>Juglans regia</i> L.) Shells
title_sort effect of milling on the ethanolic extract composition of dried walnut i juglans regia i l shells
topic biomass
epoxidation
fatty acids
LC-MS/MS
mill grinding
phenols
url https://www.mdpi.com/1422-0067/24/17/13059
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