Headspace with Gas Chromatography-Mass Spectrometry for the Use of Volatile Organic Compound Profile in Botanical Origin Authentication of Honey
Abstract
:1. Introduction
2. Results and Discussion
2.1. HS-GC-MS Method Optimisation
2.2. Monitorisation of VOCs in Honey
2.3. Method Characterisation and Quantification of Identified VOCs
2.4. Non-Targeted Approach Using GC-MS Data
2.5. Chemometric Model for the Classification of Honey According to Botanical Origin
2.6. Application of the Proposed Method
3. Materials and Methods
3.1. Standards and Solvents
3.2. Honey Samples
3.3. Instrumentation and Software
3.4. HS-GC-MS Analysis
3.5. Data Processing
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Sample Availability
References
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Compound | RT 1 (min) | Target Ion (m/z) | Qualifier Ions (m/z) |
---|---|---|---|
2-Pentanone | 2.99 | 43 | 71, 86 |
Valeraldehyde | 3.16 | 44 | 29, 86 |
4-Methylpentan-2-one | 4.03 | 43 | 58, 85 |
Trans-2-pentenal | 4.46 | 55 | 84, 41 |
Toluene * | 4.70 | 91 | 92, 65 |
1-Pentanol | 4.80 | 42 | 31, 70 |
2-Hexanone | 5.54 | 43 | 58, 85 |
Hexanal | 5.88 | 44 | 57, 82 |
Ethyl butyrate | 5.96 | 71 | 43, 88 |
Trans-2-hexen-1-al | 7.86 | 41 | 69, 83 |
Ethyl isovalerate | 7.93 | 88 | 57, 115 |
p-Xylene * | 8.39 | 91 | 105, 106 |
1-Hexanol | 8.54 | 56 | 43, 84 |
2-Heptanone | 9.32 | 43 | 58, 71 |
Heptanal | 9.69 | 70 | 44, 96 |
Trans-2-heptenal | 11.73 | 41 | 70, 83 |
Benzaldehyde | 11.79 | 106 | 77, 107 |
6-Methyl-5-hepten-2-one | 12.86 | 43 | 69, 108 |
2-Octanone | 12.99 | 43 | 71, 85 |
2-Octanol | 13.33 | 45 | 70, 97 |
Octanal | 13.39 | 41 | 44, 128 |
Trans-2-octenal | 15.26 | 41 | 83, 97 |
1-Octanol | 15.70 | 56 | 41, 84 |
2-Nonanone | 16.39 | 43 | 71, 99 |
Linalool | 16.63 | 71 | 93, 136 |
Nonanal | 16.77 | 57 | 43, 98 |
4-Methylacetophenone | 19.25 | 119 | 91, 65 |
Decanal | 19.87 | 43 | 82, 112 |
Trans-2-decenal | 21.48 | 43 | 82, 110 |
Compound | Linear Range (μg g−1) | R2 | LOD 1 (LOQ 2) (μg g−1) |
---|---|---|---|
2-Pentanone | 0.016–1.00 | 0.993 | 0.005 (0.016) |
Valeraldehyde | 0.016–1.00 | 0.992 | 0.005 (0.016) |
4-Methylpentan-2-one | 0.016–1.00 | 0.993 | 0.005 (0.016) |
Trans-2-pentenal | 0.216–1.00 | 0.993 | 0.065 (0.216) |
1-Pentanol | 0.249–1.00 | 0.990 | 0.075 (0.249) |
2-Hexanone | 0.218–1.00 | 0.991 | 0.065 (0.218) |
Hexanal | 0.015–1.00 | 0.991 | 0.005 (0.015) |
Ethyl butyrate | 0.040–1.00 | 0.997 | 0.012 (0.040) |
Trans-2-hexen-1-al | 0.129–1.00 | 0.980 | 0.039 (0.129) |
Ethyl isovalerate | 0.040–1.00 | 0.995 | 0.012 (0.040) |
1-Hexanol | 0.083–1.00 | 0.994 | 0.025 (0.083) |
2-Heptanone | 0.083–1.00 | 0.994 | 0.025 (0.083) |
Heptanal | 0.016–1.00 | 0.991 | 0.005 (0.016) |
Trans-2-heptenal | 0.130–1.00 | 0.999 | 0.039 (0.130) |
Benzaldehyde | 0.016–1.00 | 0.992 | 0.005 (0.016) |
6-Methyl-5-hepten-2-one | 0.016–1.00 | 0.995 | 0.005 (0.016) |
2-Octanone | 0.016–1.00 | 0.996 | 0.005 (0.016) |
2-Octanol | 0.083–1.00 | 0.990 | 0.025 (0.083) |
Octanal | 0.016–1.00 | 0.995 | 0.005 (0.016) |
Trans-2-octenal | 0.016–1.00 | 0.991 | 0.005 (0.016) |
1-Octanol | 0.016–1.00 | 0.991 | 0.005 (0.016) |
2-Nonanone | 0.016–1.00 | 0.997 | 0.005 (0.016) |
Linalool | 0.015–1.00 | 0.994 | 0.005 (0.015) |
Nonanal | 0.016–1.00 | 0.998 | 0.005 (0.016) |
4-Methylacetophenone | 0.016–1.00 | 0.994 | 0.005 (0.016) |
Decanal | 0.016–1.00 | 0.998 | 0.005 (0.016) |
Trans-2-decenal | 0.218–1.00 | 0.995 | 0.065 (0.218) |
Compound | Albaida | Orange Blossom | Thousand Flowers | Rosemary | Others | |
---|---|---|---|---|---|---|
2-Pentanone | Mean (ng g−1) | 26.0 ± 1.3 a | 33 ± 8 a,b | 32 ± 9 b | 34 ± 7 b | 36 ± 10 b |
Range (ng g−1) | NQ 1–27.4 | NQ–45.8 | 19.4–49.4 | 26.7–46.0 | 0.00–61.4 | |
Incidence (%) | 66.7 | 83.3 | 100.0 | 100.0 | 86.4 | |
Valeraldehyde | Mean (ng g−1) | 208 ± 38 b | 35 ± 15 a | 41 ± 24 a,b | 46 ± 9 a,b | 42 ± 18 a |
Range (ng g−1) | NQ–235.2 | NQ–69.4 | 0.00–86.3 | 34.0–56.9 | 0.00–69.0 | |
Incidence (%) | 33.3 | 75.0 | 94.1 | 100.0 | 63.6 | |
4-Methylpentan-2-one | Mean (ng g−1) | ND 2,a | ND a | 46 ± 10 b | ND a | 43 ± 8 b |
Range (ng g−1) | – | – | 0.00–59.1 | – | 0.00–48.3 | |
Incidence (%) | – | – | 35.3 | – | 54.5 | |
Trans-2-pentenal | Mean (ng g−1) | ND a,b | ND a | ND a | ND a,b | 287 ± 38 b |
Range (ng g−1) | – | – | – | – | 0.00–334.8 | |
Incidence (%) | – | – | – | – | 18.2 | |
2-Hexanone | Mean (ng g−1) | NQ | NQ | NQ | NQ | NQ |
Range (ng g−1) | NQ | 0.00–NQ | 0.00–NQ | 0.00–NQ | 0.00–NQ | |
Incidence (%) | – | – | – | – | – | |
Hexanal | Mean (ng g−1) | 15.4 a | 69 ± 17 a | 70 ± 24 a | 83 ± 11 a | 173 ± 140 b |
Range (ng g−1) | 0.00–15.4 | 0.00–94.0 | 0.00–99.1 | 74.9–90.5 | 0.00–463.7 | |
Incidence (%) | 16.7 | 50.0 | 47.1 | 33.3 | 72.7 | |
Ethyl butyrate | Mean (ng g−1) | 289 ± 16 b | ND a | ND a | ND a | ND a |
Range (ng g−1) | 0.00–300.8 | – | – | – | – | |
Incidence (%) | 33.3 | – | – | – | – | |
2-Heptanone | Mean (ng g−1) | ND a,b | 94 ± 12 b | ND a | ND a,b | ND a |
Range (ng g−1) | – | 0.00–85.4 | – | – | – | |
Incidence (%) | – | 16.7 | – | – | – | |
Heptanal | Mean (ng g−1) | 28 ± 3 a,b | 27 ± 2 a,b | 46 ± 40 b | 34 ± 5 a,b | 31 ± 5 a |
Range (ng g−1) | 23.3–32.9 | 22.2–30.8 | 0.00–142.1 | 26.6–39.9 | 0.00–38.6 | |
Incidence (%) | 100.0 | 100.0 | 82.4 | 100.0 | 63.6 | |
Trans-2-heptenal | Mean (ng g−1) | ND a | ND a | ND a | ND a | 84 ± 3 a |
Range (ng g−1) | – | – | – | – | 0.00–86.8 | |
Incidence (%) | – | – | – | – | 9.1 | |
Benzaldehyde | Mean (ng g−1) | NQ a | 43 ± 2 a | 42 ± 19 a,b | 42 ± 11 a,b | 102 ± 72 b |
Range (ng g−1) | 0.00–NQ | 0.00–44.4 | 0.0–80.2 | 0.00–50.5 | 0.00–213.9 | |
Incidence (%) | – | 16.7 | 70.6 | 66.7 | 50.0 | |
6-Methyl-5-hepten-2-one | Mean (ng g−1) | 46.7 ± 0.4 a,b | 43 ± 6 b | 41.6 ± 0.1 a | 41.5 ± 0.3 a,b | 48 ± 2 a |
Range (ng g−1) | 0.00–47.0 | 0.00–49.1 | 0.00–41.6 | 0.00–41.7 | 0.00–50.1 | |
Incidence (%) | 33.3 | 66.7 | 11.8 | 33.3 | 18.2 | |
2-Octanone | Mean (ng g−1) | 25.5 ± 1.4 a,b | 20 ± 2 a,b | 20.5 ± 0.4 a | 56.2 ± 0.3 b | 20.8 ± 1.8 a,b |
Range (ng g−1) | 0.00–26.5 | 0.00–23.5 | 0.00–20.8 | 0.00–56.4 | 0.00–24.9 | |
Incidence (%) | 33.3 | 50.0 | 11.8 | 33.3 | 36.4 | |
Octanal | Mean (ng g−1) | 79 ± 69 a | 84 ± 61 a | 72 ± 81 a | 41 ± 6 a | 142 ± 394 a |
Range (ng g−1) | 31.1–175.7 | 0.00–161.7 | 0.00–37.2 | 0.00–50.6 | 0.00–1717.8 | |
Incidence (%) | 100.0 | 75.0 | 64.7 | 66.7 | 81.8 | |
Trans-2-octenal | Mean (ng g−1) | 34 ± 2 a,b | 31 ± 2 a,b | 36 ± 3 b | 39 ± 9 b | 32 ± 5 a |
Range (ng g−1) | 28.7–36.3 | 27.0–32.9 | 0.00–44.3 | 31.3–55.4 | 0.00–40.7 | |
Incidence (%) | 100.0 | 100.0 | 88.2 | 100.0 | 72.7 | |
1-Octanol | Mean (ng g−1) | 61 ± 2 a,b | 89.2 ± 1.8 a,b | 84 ± 19 a,b | 77 ± 14 b | 155 ± 2 a |
Range (ng g−1) | 0.00–63.2 | 0.00–90.5 | 0.00–105.3 | 0.00–92.0 | 0.00–156.7 | |
Incidence (%) | 33.3 | 16.7 | 23.5 | 66.7 | 9.1 | |
2-Nonanone | Mean (ng g−1) | 38.1 ± 0.2 b | ND a | ND a | ND a | 48.3 ± 0.9 a,b |
Range (ng g−1) | 0.00–38.2 | – | – | – | 0.00–48.9 | |
Incidence (%) | 33.3 | – | – | – | 9.1 | |
Linalool | Mean (ng g−1) | NQ a | 35 ± 19 b | 20 ± 2 a | 23.8 ± 1.9 a | 19.1 ± 1.6 a |
Range (ng g−1) | NQ | NQ–72.0 | 0.00–21.8 | NQ–25.1 | NQ–21.7 | |
Incidence (%) | – | 66.7 | 29.4 | 33.3 | 27.3 | |
Nonanal | Mean (ng g−1) | 25.7 ± 1.7 a | 29 ± 12 a | 72 ± 2 a | 30 ± 14 a | 97 ± 75 a |
Range (ng g−1) | 0.00–26.8 | 0.00–45.9 | 0.00–96.1 | NQ–45.0 | 0.00–232.4 | |
Incidence (%) | 33.3 | 50.0 | 35.3 | 66.7 | 36.4 | |
4-Methylacetophenone | Mean (ng g−1) | NQ a | 57 ± 23 a | 70 ± 2 a | 82 ± 6 a | 161 ± 75 a |
Range (ng g−1) | 0.00–NQ | 0.00–88.1 | 0.00–72.9 | 77.2–86.3 | 0.00–232.4 | |
Incidence (%) | – | 50.0 | 11.8 | 33.3 | 18.2 | |
Decanal | Mean (ng g−1) | 35.6 ± 0.6 a | 36.0 ± 1.0 a | 36 ± 2 a | 260 ± 446 b | 36 ± 2 a |
Range (ng g−1) | 0.00–36.4 | 0.00–37.5 | 0.00–39.1 | 35.1–929.4 | 0.00–41.0 | |
Incidence (%) | 66.7 | 83.3 | 35.3 | 66.7 | 81.8 |
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Castell, A.; Arroyo-Manzanares, N.; Guerrero-Núñez, Y.; Campillo, N.; Viñas, P. Headspace with Gas Chromatography-Mass Spectrometry for the Use of Volatile Organic Compound Profile in Botanical Origin Authentication of Honey. Molecules 2023, 28, 4297. https://doi.org/10.3390/molecules28114297
Castell A, Arroyo-Manzanares N, Guerrero-Núñez Y, Campillo N, Viñas P. Headspace with Gas Chromatography-Mass Spectrometry for the Use of Volatile Organic Compound Profile in Botanical Origin Authentication of Honey. Molecules. 2023; 28(11):4297. https://doi.org/10.3390/molecules28114297
Chicago/Turabian StyleCastell, Ana, Natalia Arroyo-Manzanares, Yolanda Guerrero-Núñez, Natalia Campillo, and Pilar Viñas. 2023. "Headspace with Gas Chromatography-Mass Spectrometry for the Use of Volatile Organic Compound Profile in Botanical Origin Authentication of Honey" Molecules 28, no. 11: 4297. https://doi.org/10.3390/molecules28114297