Enhancing the targeted and untargeted analysis of honey by vacuum-assisted SPME-GC × GC-MS. A green, practical, and highly informative approach
The use of vacuum-assisted headspace (Vac-HS) coupled with solid-phase microextraction (SPME) is a technique that has been recently proven to be highly beneficial for enhancing the extraction of semi-volatile in shorter time and milder temperatures. This technique indeed increases the extraction kin...
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Elsevier
2025-03-01
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| Series: | Green Analytical Chemistry |
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| Online Access: | http://www.sciencedirect.com/science/article/pii/S2772577425000047 |
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| author | Damien Eggermont Francesca Pardi Giorgia Purcaro |
| author_facet | Damien Eggermont Francesca Pardi Giorgia Purcaro |
| author_sort | Damien Eggermont |
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| description | The use of vacuum-assisted headspace (Vac-HS) coupled with solid-phase microextraction (SPME) is a technique that has been recently proven to be highly beneficial for enhancing the extraction of semi-volatile in shorter time and milder temperatures. This technique indeed increases the extraction kinetics by reducing the mass transfer resistance at the interface between the sample and headspace. In this work, we explored the use of Vac-HS coupled with comprehensive two-dimensional gas chromatography coupled with mass spectrometry to simultaneously determine 5-hydroxymethylfurfural (a semi-volatile processing marker in honey) and the entire volatile profile, which is recognized as a highly informative fingerprint of the geographical and botanical authenticity of honey. The use of Vac-HS-SPME has been optimized using an experimental design and compared to the atmospheric pressure extraction. Considering both 5-HMF and the entire volatile profile, an overall 10-fold higher signal was obtained using Vac-HS-SPME compared to simple HS-SPME. The absolute quantification of 5-hydroxymethylfurfural was fully validated, obtaining a limit of quantification of about 5 µg/g, largely below the lowest required limit for the presence of this compound in honey (i.e., 15 µg/g). The results obtained from a series of commercially available honey were compared with those obtained using the official high-performance liquid chromatography-UV method, obtaining comparable results but through a greener and more practical method. The overall volatile profile obtained by Vac-HS-SPME showed a significant increase in the response of the less volatile compounds, reaching up to a 90-fold increment compared to HS-SPME. |
| format | Article |
| id | doaj-art-f5ba567cd2404ea79e588c5edb09704b |
| institution | Kabale University |
| issn | 2772-5774 |
| language | English |
| publishDate | 2025-03-01 |
| publisher | Elsevier |
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| series | Green Analytical Chemistry |
| spelling | doaj-art-f5ba567cd2404ea79e588c5edb09704b2025-01-26T05:05:22ZengElsevierGreen Analytical Chemistry2772-57742025-03-0112100207Enhancing the targeted and untargeted analysis of honey by vacuum-assisted SPME-GC × GC-MS. A green, practical, and highly informative approachDamien Eggermont0Francesca Pardi1Giorgia Purcaro2Analytical Chemistry Lab, Gembloux Agro-Bio Tech, University of Liège, Bât. G1 Chimie des agro-biosystèmes, Passage des Déportés 2, Gembloux B-5030, BelgiumAnalytical Chemistry Lab, Gembloux Agro-Bio Tech, University of Liège, Bât. G1 Chimie des agro-biosystèmes, Passage des Déportés 2, Gembloux B-5030, Belgium; La Sapienza, University of Roma, Piazzale Aldo Moro 5, Roma 00185, ItalyAnalytical Chemistry Lab, Gembloux Agro-Bio Tech, University of Liège, Bât. G1 Chimie des agro-biosystèmes, Passage des Déportés 2, Gembloux B-5030, Belgium; Corresponding author.The use of vacuum-assisted headspace (Vac-HS) coupled with solid-phase microextraction (SPME) is a technique that has been recently proven to be highly beneficial for enhancing the extraction of semi-volatile in shorter time and milder temperatures. This technique indeed increases the extraction kinetics by reducing the mass transfer resistance at the interface between the sample and headspace. In this work, we explored the use of Vac-HS coupled with comprehensive two-dimensional gas chromatography coupled with mass spectrometry to simultaneously determine 5-hydroxymethylfurfural (a semi-volatile processing marker in honey) and the entire volatile profile, which is recognized as a highly informative fingerprint of the geographical and botanical authenticity of honey. The use of Vac-HS-SPME has been optimized using an experimental design and compared to the atmospheric pressure extraction. Considering both 5-HMF and the entire volatile profile, an overall 10-fold higher signal was obtained using Vac-HS-SPME compared to simple HS-SPME. The absolute quantification of 5-hydroxymethylfurfural was fully validated, obtaining a limit of quantification of about 5 µg/g, largely below the lowest required limit for the presence of this compound in honey (i.e., 15 µg/g). The results obtained from a series of commercially available honey were compared with those obtained using the official high-performance liquid chromatography-UV method, obtaining comparable results but through a greener and more practical method. The overall volatile profile obtained by Vac-HS-SPME showed a significant increase in the response of the less volatile compounds, reaching up to a 90-fold increment compared to HS-SPME.http://www.sciencedirect.com/science/article/pii/S2772577425000047Vacuum-assisted-headspace (Vac-HS)Solid-phase microextraction (SPME)GC × GC-MSHoney5-hydroxymethylfurfural (5-HMF)Volatile compounds |
| spellingShingle | Damien Eggermont Francesca Pardi Giorgia Purcaro Enhancing the targeted and untargeted analysis of honey by vacuum-assisted SPME-GC × GC-MS. A green, practical, and highly informative approach Green Analytical Chemistry Vacuum-assisted-headspace (Vac-HS) Solid-phase microextraction (SPME) GC × GC-MS Honey 5-hydroxymethylfurfural (5-HMF) Volatile compounds |
| title | Enhancing the targeted and untargeted analysis of honey by vacuum-assisted SPME-GC × GC-MS. A green, practical, and highly informative approach |
| title_full | Enhancing the targeted and untargeted analysis of honey by vacuum-assisted SPME-GC × GC-MS. A green, practical, and highly informative approach |
| title_fullStr | Enhancing the targeted and untargeted analysis of honey by vacuum-assisted SPME-GC × GC-MS. A green, practical, and highly informative approach |
| title_full_unstemmed | Enhancing the targeted and untargeted analysis of honey by vacuum-assisted SPME-GC × GC-MS. A green, practical, and highly informative approach |
| title_short | Enhancing the targeted and untargeted analysis of honey by vacuum-assisted SPME-GC × GC-MS. A green, practical, and highly informative approach |
| title_sort | enhancing the targeted and untargeted analysis of honey by vacuum assisted spme gc gc ms a green practical and highly informative approach |
| topic | Vacuum-assisted-headspace (Vac-HS) Solid-phase microextraction (SPME) GC × GC-MS Honey 5-hydroxymethylfurfural (5-HMF) Volatile compounds |
| url | http://www.sciencedirect.com/science/article/pii/S2772577425000047 |
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