Response Surface Methodology to Optimize the Isolation of Dominant Volatile Compounds from Monofloral Greek Thyme Honey Using SPME-GC-MS
Abstract
:1. Introduction
2. Results and Discussion
2.1. Physicochemical and Melissopalynological Analysis
2.2. Isolation of Volatile Compounds
2.3. Evaluation of Factors
2.4. Evaluation and Optimization of Dominant Volatile Compounds
3. Materials and Methods
3.1. Honey Samples
3.2. Experimental Design
3.3. Isolation and Analysis of Volatile Compounds
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Aggregate Functions | Fructose + Glucose a (%w/w) | Sucrose b (%w/w) | Moisture c (%w/w) | Electrical Conductivity d (μS cm−1) | Diastase Activity e (Schade) | HMF f (mg kg−1) | Thymbra capitata L. Pollen g (%) |
---|---|---|---|---|---|---|---|
Min | 60.1 | 0.0 | 13.8 | 251 | 11.1 | 1.0 | 18.0 |
Max | 86.4 | 2.1 | 17.9 | 600 | 51.1 | 14.7 | 77.9 |
Average | 68.1 | 0.3 | 15.8 | 457 | 27.3 | 5.2 | 33.1 |
No. | Volatile Compounds | RT a | RI b | Boiling Point (°C) | Min (mg kg−1) | Max (mg kg−1) | Average (mg kg−1) |
---|---|---|---|---|---|---|---|
Esters | |||||||
1 | methyl octanoate | 18.3 | 1123 | 190.6 | 0.00 | 2.72 | 0.46 |
2 | methyl nonanoate | 21.3 | 1222 | 213.5 | 0.09 | 11.63 | 1.41 |
3 | methyl decanoate | 24.3 | 1321 | 236.4 | 0.00 | 1.17 | 0.12 |
4 | methyl hexadecanoate | 39.7 | 1929 | 373.6 | 0.00 | 0.46 | 0.07 |
Aldehydes | |||||||
5 | furan-2-carbaldehyde | 9.8 | 822 | 139.7 | 0.20 | 4.54 | 1.90 |
6 | benzaldehyde | 12.6 | 957 | 162.0 | 0.52 | 10.40 | 3.64 |
7 | 2-phenylacetaldehyde | 15.6 | 1041 | 184.8 | 0.39 | 3.56 | 1.78 |
8 | nonanal | 17.7 | 1104 | 181.0 | 0.00 | 1.45 | 0.31 |
9 | decanal | 20.8 | 1205 | 203.9 | 0.00 | 1.41 | 0.21 |
10 | 4-isopropylbenzaldehyde | 21.8 | 1240 | 235.1 | 0.00 | 0.20 | 0.05 |
Alcohols | |||||||
11 | 2-phenylethan-1-ol | 17.9 | 1111 | 228.4 | 0.00 | 5.28 | 1.94 |
12 | 5-isopropyl-2-methylphenol (carvacrol) | 23.5 | 1299 | 267.1 | 0.00 | 0.26 | 0.06 |
Ketones | |||||||
13 | 1-phenylbutane-2,3-dione | 20.9 | 1210 | 289.7 | 0.00 | 1.37 | 0.48 |
14 | 2-isopropyl-5-methylcyclohexa-2,5-diene-1,4-dione (thymoquinone) | 22.0 | 1247 | 323.0 | 0.00 | 0.59 | 0.08 |
15 | 3-hydroxy-4-phenyl-2-butanone | 24.9 | 1343 | 327.5 | 0.00 | 3.87 | 0.93 |
16 | (Z)-3-hydroxy-4-phenylbut-3-en-2-one | 27.7 | 1427 | 332.0 | 0.00 | 0.37 | 0.09 |
Hydrocarbons | |||||||
17 | butane | 1.6 | <800 | 18.0 | 0.00 | 20.58 | 1.03 |
18 | heptane | 3.4 | <800 | 86.6 | 0.00 | 10.32 | 0.58 |
19 | octane | 5.9 | 800 | 109.5 | 0.00 | 5.83 | 0.45 |
20 | nonane | 10.3 | 896 | 132.4 | 0.00 | 1.68 | 0.20 |
21 | undecane | 17.6 | 1100 | 178.1 | 0.04 | 34.49 | 2.33 |
Nitriles | |||||||
22 | isobutyronitrile | 2.2 | <800 | 119.6 | 0.00 | 11.66 | 0.92 |
23 | 2-methylbutanenitrile | 3.5 | <800 | 142.5 | 0.00 | 5.01 | 0.47 |
24 | 3-methylbutanenitrile | 3.7 | <800 | 142.5 | 0.05 | 59.16 | 7.01 |
25 | 2-phenylacetonitrile | 18.8 | 1136 | 215.4 | 0.25 | 5.35 | 1.93 |
Terpenoids | |||||||
26 | methylbenzene | 4.7 | <800 | 113.3 | 0.00 | 3.38 | 0.34 |
27 | 1-isopropyl-4-methylbenzene (p-cymene) | 14.9 | 1022 | 186.5 | 0.00 | 2.62 | 0.39 |
28 | 1-methyl-4-(prop-1-en-2-yl)benzene | 17.2 | 1088 | 183.5 | 0.00 | 1.14 | 0.17 |
Others | |||||||
29 | 2,5-diethyltetrahydrofuran | 10.0 | 890 | 147.1 | 0.00 | 7.22 | 1.35 |
30 | methyl 2-oxo-2-phenylacetate | 22.7 | 1271 | 271.1 | 0.00 | 0.54 | 0.18 |
31 | 1,1,5-trimethyl-1,2-dihydronaphthalene | 25.2 | 1351 | 270.9 | 0.00 | 1.39 | 0.37 |
Response | Volatile Compound | Min (%Area) | Max (%Area) | Mean (%Area) | Std. Dev. |
---|---|---|---|---|---|
R1 | benzaldehyde | 4.60 | 17.32 | 11.55 | 1.57 |
R2 | 2-phenylacetaldehyde | 0.82 | 13.48 | 6.99 | 1.03 |
R3 | undecane | 0.62 | 16.17 | 3.86 | 0.85 |
R4 | nonanal | 0.00 | 2.62 | 0.99 | 0.38 |
R5 | 2-phenylethan-1-ol | 0.00 | 16.72 | 8.12 | 1.94 |
R6 | 2-phenylacetonitrile | 1.40 | 11.59 | 6.97 | 1.31 |
R7 | 1-phenylbutane-2,3-dione | 0.00 | 6.49 | 1.22 | 0.52 |
R8 | methyl nonanoate | 0.53 | 15.23 | 4.32 | 2.27 |
R9 | 3-hydroxy-4-phenyl-2-butanone | 0.00 | 17.26 | 4.58 | 1.22 |
R10 | (Z)-3-hydroxy-4-phenylbut-3-en-2-one | 0.00 | 1.64 | 0.45 | 0.11 |
Response | Volatile Compound | A | B | C | D | E | F | R2 |
---|---|---|---|---|---|---|---|---|
R1 | benzaldehyde | 0.011 a | 0.198 | 0.101 | 0.259 | 0.439 | 0.007 | 0.965 |
R2 | 2-phenylacetaldehyde | 0.000 | 0.265 | 0.657 | 0.898 | 0.104 | 0.059 | 0.988 |
R3 | undecane | 0.000 | 0.319 | 0.001 | 0.010 | 0.013 | 0.001 | 0.991 |
R4 | nonanal | 0.090 | 0.951 | 0.843 | 0.004 | 0.168 | 0.007 | 0.958 |
R5 | 2-phenylethan-1-ol | 0.000 | 0.545 | 0.013 | 0.170 | 0.324 | 0.001 | 0.980 |
R6 | 2-phenylacetonitrile | 0.002 | 0.587 | 0.018 | 0.724 | 0.161 | 0.005 | 0.965 |
R7 | 1-phenylbutane-2,3-dione | 0.001 | 0.943 | 0.078 | 0.916 | 0.413 | 0.012 | 0.962 |
R8 | methyl nonanoate | 0.179 | 0.697 | 0.364 | 0.246 | 0.026 | 0.031 | 0.932 |
R9 | 3-hydroxy-4-phenyl-2-butanone | 0.000 | 0.656 | 0.001 | 0.175 | 0.542 | 0.000 | 0.991 |
R10 | (Z)-3-hydroxy-4-phenylbut-3-en-2-one | 0.014 | 0.092 | 0.011 | 0.680 | 0.357 | 0.026 | 0.994 |
Response | Volatile Compound | A | B | C | D | E | F | Desirability | Predicted Mean (%Area) |
---|---|---|---|---|---|---|---|---|---|
R1 | benzaldehyde | 60 | 5 | 15 | 700 | 6 | 1:1 | 0.810 | 14.9 ± 1.6 |
R2 | 2-phenylacetaldehyde | 60 | 15 | 15 | 400 | 6 | 1:1 | 0.975 | 13.2 ± 1.0 |
R3 | undecane | 30 | 15 | 15 | 400 | 2 | 3:1 | 0.940 | 15.2 ± 0.9 |
R4 | nonanal | 45 | 15 | 30 | 700 | 4 | 3:1 | 0.933 | 2.4 ± 0.4 |
R5 | 2-phenylethan-1-ol | 60 | 15 | 15 | 400 | 6 | 1:3 | 0.923 | 15.4 ± 1.9 |
R6 | 2-phenylacetonitrile | 60 | 15 | 30 | 400 | 6 | 1:3 | 0.957 | 11.1 ± 1.3 |
R7 | 1-phenylbutane-2.3dione | 60 | 30 | 30 | 700 | 6 | 1:3 | 0.966 | 6.3 ± 0.6 |
R8 | methyl nonanoate | 60 | 30 | 30 | 400 | 2 | 3:1 | 0.814 | 12.5 ± 2.3 |
R9 | 3-hydroxy-4-phenyl-2-butanone | 60 | 30 | 30 | 700 | 4 | 1:3 | 0.841 | 14.5 ± 1.2 |
R10 | (Z)-3-hydroxy-4-phenylbut-3-en-2-one | 60 | 5 | 30 | 700 | 6 | 1:3 | 0.947 | 1.5 ± 0.3 |
Factor | Name | Units | Minimum | Maximum | Coded Low | Coded High | Mean | Std. Dev. |
---|---|---|---|---|---|---|---|---|
A | Temperature | °C | 30.0 | 60.0 | −1 ↔ 30.0 | +1 ↔ 60.0 | 45.0 | 13.5 |
B | Equilibration time | min | 5.0 | 30.0 | −1 ↔ 5.0 | +1 ↔ 30.0 | 17.7 | 11.6 |
C | Extraction time | min | 15.0 | 60.0 | −1 ↔ 15.0 | +1 ↔ 60.0 | 36.7 | 20.8 |
D | Magnetic stirrer speed | rpm | 100.0 | 700.0 | −1 ↔ 100.0 | +1 ↔ 700.0 | 407.8 | 283.2 |
E | Sample volume | mL | 2.0 | 6.0 | −1 ↔ 2.0 | +1 ↔ 6.0 | 4.1 | 1.8 |
F | Water:honey ratio | v/w | 1:3 | 3:1 |
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Xagoraris, M.; Skouria, A.; Revelou, P.-K.; Alissandrakis, E.; Tarantilis, P.A.; Pappas, C.S. Response Surface Methodology to Optimize the Isolation of Dominant Volatile Compounds from Monofloral Greek Thyme Honey Using SPME-GC-MS. Molecules 2021, 26, 3612. https://doi.org/10.3390/molecules26123612
Xagoraris M, Skouria A, Revelou P-K, Alissandrakis E, Tarantilis PA, Pappas CS. Response Surface Methodology to Optimize the Isolation of Dominant Volatile Compounds from Monofloral Greek Thyme Honey Using SPME-GC-MS. Molecules. 2021; 26(12):3612. https://doi.org/10.3390/molecules26123612
Chicago/Turabian StyleXagoraris, Marinos, Alexandra Skouria, Panagiota-Kyriaki Revelou, Eleftherios Alissandrakis, Petros A. Tarantilis, and Christos S. Pappas. 2021. "Response Surface Methodology to Optimize the Isolation of Dominant Volatile Compounds from Monofloral Greek Thyme Honey Using SPME-GC-MS" Molecules 26, no. 12: 3612. https://doi.org/10.3390/molecules26123612