Unifloral Autumn Heather Honey from Indigenous Greek Erica manipuliflora Salisb.: SPME/GC-MS Characterization of the Volatile Fraction and Optimization of the Isolation Parameters
Abstract
:1. Introduction
2. Materials and Methods
2.1. Honey Samples
2.2. Experimental Design
2.3. Isolation and Analysis of Volatile Compounds
3. Results and Discussion
3.1. Evaluation of Isolated Volatile Compounds
3.2. Optimization of Each Dominant Volatile Compound
3.3. Optimization and Validation of Dominant Volatile Compounds
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Run | A: Temperature | B: Equilibration Time | C: Extraction Time | D: Magnetic Stirrer Velocity | E: Sample Volume | F: Water: Honey Ratio |
---|---|---|---|---|---|---|
Units | °C | min | min | rpm | mL | v/w |
1 | 30.0 | 5.0 | 15.0 | 700.0 | 4.0 | 1:3 |
2 | 30.0 | 5.0 | 60.0 | 400.0 | 2.0 | 1:1 |
3 | 30.0 | 5.0 | 15.0 | 100.0 | 6.0 | 1:1 |
4 | 30.0 | 5.0 | 30.0 | 700.0 | 6.0 | 3:1 |
5 | 30.0 | 5.0 | 15.0 | 100.0 | 2.0 | 1:3 |
6 | 30.0 | 15.0 | 15.0 | 100.0 | 4.0 | 3:1 |
7 | 30.0 | 15.0 | 60.0 | 700.0 | 6.0 | 1:3 |
8 | 30.0 | 15.0 | 15.0 | 700.0 | 2.0 | 1:1 |
9 | 30.0 | 30.0 | 30.0 | 400.0 | 6.0 | 1:3 |
10 | 30.0 | 30.0 | 60.0 | 100.0 | 2.0 | 1:3 |
11 | 30.0 | 30.0 | 60.0 | 700.0 | 6.0 | 1:1 |
12 | 30.0 | 30.0 | 60.0 | 100.0 | 6.0 | 3:1 |
13 | 30.0 | 30.0 | 15.0 | 700.0 | 6.0 | 3:1 |
14 | 30.0 | 30.0 | 30.0 | 100.0 | 4.0 | 1:1 |
15 | 30.0 | 30.0 | 60.0 | 700.0 | 2.0 | 3:1 |
16 | 45.0 | 5.0 | 60.0 | 100.0 | 6.0 | 1:3 |
17 | 45.0 | 5.0 | 60.0 | 700.0 | 2.0 | 1:3 |
18 | 45.0 | 5.0 | 15.0 | 400.0 | 4.0 | 1:1 |
19 | 45.0 | 15.0 | 60.0 | 100.0 | 2.0 | 1:1 |
20 | 45.0 | 15.0 | 60.0 | 700.0 | 6.0 | 3:1 |
21 | 45.0 | 30.0 | 15.0 | 100.0 | 6.0 | 1:3 |
22 | 45.0 | 30.0 | 30.0 | 100.0 | 2.0 | 3:1 |
23 | 45.0 | 30.0 | 15.0 | 700.0 | 2.0 | 1:3 |
24 | 60.0 | 5.0 | 60.0 | 100.0 | 2.0 | 3:1 |
25 | 60.0 | 5.0 | 15.0 | 100.0 | 6.0 | 3:1 |
26 | 60.0 | 5.0 | 60.0 | 700.0 | 6.0 | 1:1 |
27 | 60.0 | 5.0 | 30.0 | 100.0 | 2.0 | 1:1 |
28 | 60.0 | 5.0 | 15.0 | 700.0 | 6.0 | 1:3 |
29 | 60.0 | 5.0 | 60.0 | 400.0 | 6.0 | 3:1 |
30 | 60.0 | 5.0 | 15.0 | 700.0 | 2.0 | 3:1 |
31 | 60.0 | 15.0 | 30.0 | 400.0 | 2.0 | 1:3 |
32 | 60.0 | 30.0 | 60.0 | 100.0 | 6.0 | 1:1 |
33 | 60.0 | 30.0 | 30.0 | 700.0 | 4.0 | 3:1 |
34 | 60.0 | 30.0 | 15.0 | 100.0 | 2.0 | 1:1 |
35 | 60.0 | 30.0 | 15.0 | 700.0 | 6.0 | 1:1 |
36 | 60.0 | 30.0 | 60.0 | 700.0 | 6.0 | 1:3 |
37 | 60.0 | 30.0 | 60.0 | 700.0 | 2.0 | 1:1 |
38 | 60.0 | 30.0 | 15.0 | 100.0 | 4.0 | 1:3 |
No. | Volatile Compounds | CAS Number | RT a | RI b | Min (mg kg−1) | Max (mg kg−1) | Average (mg kg−1) |
---|---|---|---|---|---|---|---|
Esters | |||||||
1 | methyl benzoate | 93-58-3 | 17.3 | 1093 | 0.00 | 0.33 | 0.02 |
2 | methyl octanoate | 111-11-5 | 18.3 | 1124 | 0.00 | 0.17 | 0.06 |
3 | ethyl benzoate | 93-89-0 | 19.6 | 1165 | 0.00 | 1.68 | 0.11 |
4 | methyl 2-phenylacetate | 101-41-7 | 19.8 | 1179 | 0.00 | 0.32 | 0.04 |
5 | methyl 2-hydroxybenzoate (methyl salicylate) | 119-36-8 | 20.4 | 1192 | 0.00 | 0.54 | 0.06 |
6 | methyl nonanoate | 1731-84-6 | 21.3 | 1222 | 0.06 | 0.44 | 0.16 |
7 | methyl decanoate | 110-42-9 | 24.3 | 1322 | 0.00 | 0.10 | 0.05 |
8 | ethyl 4-methoxybenzoate (Ethyl anisate) | 94-30-4 | 28.7 | 1458 | 0.00 | 0.24 | 0.02 |
9 | methyl dodecanoate | 111-82-0 | 30.8 | 1521 | 0.00 | 0.06 | 0.01 |
10 | bis(2-methylpropyl) benzene-1,2-dicarboxylate | 84-69-5 | 39.0 | 1859 | 0.00 | 0.07 | 0.02 |
Hydrocarbons | |||||||
11 | octane | 111-65-9 | 6.3 | 800 | 0.00 | 0.18 | 0.06 |
12 | nonane | 111-84-2 | 10.3 | 898 | 0.00 | 0.16 | 0.03 |
13 | undecane | 1120-21-4 | 17.6 | 1101 | 0.10 | 0.52 | 0.21 |
14 | dodecane | 112-40-3 | 20.7 | 1201 | 0.00 | 0.18 | 0.02 |
Alcohols | |||||||
15 | oct-1-en-3-ol | 3391-86-4 | 13.4 | 981 | 0.00 | 0.26 | 0.02 |
16 | 2-ethylhexan-1-ol | 104-76-7 | 15.1 | 1029 | 0.00 | 0.16 | 0.03 |
17 | 5-(3,3-dimethyloxiran-2-yl)-3-methylpent-1-en-3-ol (cis-linalool oxide) | 5989-33-3 | 16.6 | 1072 | 0.00 | 0.35 | 0.07 |
18 | 2-phenylethan-1-ol | 60-12-8 | 17.9 | 1114 | 0.00 | 0.34 | 0.06 |
19 | 4-methyl-1-(prop-1-en-2-yl)cyclohex-3-en-1-ol (1,8-methadien-4-ol) | 3419-02-1 | 20.0 | 1183 | 0.00 | 0.54 | 0.02 |
20 | 3,4,5-trimethylphenol | 527-54-8 | 24.0 | 1314 | 0.00 | 0.93 | 0.08 |
21 | 4,6,10,10-tetramethyl-5-oxatricyclo[4.4.0.01,4]dec-2-en-7-ol | 97371-50-1 | 29.3 | 1476 | 0.00 | 0.11 | 0.01 |
22 | 6,6-dimethyl-5-methylenebicyclo[2.2.1]heptan-2-ol (6-camphenol) | 3570-04-5 | 30.5 | 1510 | 0.00 | 0.38 | 0.02 |
Aldehydes | |||||||
23 | furan-2-carbaldehyde (furfural) | 98-01-1 | 7.4 | 826 | 0.01 | 2.61 | 1.14 |
24 | benzaldehyde | 100-52-7 | 12.6 | 959 | 0.02 | 1.44 | 0.18 |
25 | octanal | 124-13-0 | 14.2 | 1001 | 0.00 | 0.15 | 0.05 |
26 | 2-phenylacetaldehyde | 122-78-1 | 15.6 | 1041 | 0.00 | 0.85 | 0.16 |
27 | nonanal | 124-19-6 | 17.7 | 1104 | 0.07 | 0.46 | 0.19 |
28 | 2,6,6-trimethylcyclohexa-1,3-diene-1-carbaldehyde (safranal) | 116-26-7 | 20.6 | 1198 | 0.00 | 0.54 | 0.12 |
29 | decanal | 112-31-2 | 20.8 | 1205 | 0.00 | 0.35 | 0.15 |
30 | 4-methoxybenzaldehyde (p-anisaldehyde) | 123-11-5 | 22.4 | 1261 | 0.00 | 1.36 | 0.23 |
Ketones | |||||||
31 | 1-(furan-2-yl)ethan-1-one | 1192-62-7 | 10.6 | 907 | 0.07 | 0.34 | 0.16 |
32 | cyclohex-2-en-1-one | 930-68-7 | 14.7 | 1015 | 0.00 | 0.15 | 0.01 |
33 | 3,5,5-trimethylcyclohex-2-en-1-one (a-isophorone) | 78-59-1 | 18.2 | 1120 | 0.01 | 4.16 | 0.43 |
34 | 2,6,6-trimethylcyclohex-2-ene-1,4-dione (4-oxoisophorone) | 1125-21-9 | 18.9 | 1143 | 0.01 | 0.89 | 0.13 |
35 | 2-hydroxy-3,5,5-trimethylcyclohex-2-en-1-one (2-hydroxyisophorone) | 4883-60-7 | 19.0 | 1145 | 0.00 | 0.29 | 0.09 |
36 | 1-(1,4-dimethylcyclohex-3-en-1-yl)ethanone | 43219-68-7 | 19.1 | 1149 | 0.00 | 0.22 | 0.02 |
37 | (E)-1-(2,6,6-trimethylcyclohexa-1,3-dien-1-yl)but-2-en-1-one (β-damascenone) | 23726-93-4 | 26.0 | 1377 | 0.00 | 0.16 | 0.05 |
38 | (E)-4-(2,4,4-trimethylcyclohexa-1,5-dien-1-yl)but-3-en-2-one | 187519 c | 27.6 | 1420 | 0.00 | 0.10 | 0.01 |
39 | (E)-1,6,6-trimethyl-7-(3-oxobut-1-en-1-yl)-3,8-dioxatricyclo[5.1.0.02,4]octan-5-one | 192009 c | 28.0 | 1437 | 0.00 | 0.23 | 0.05 |
40 | (E)-4-(2,6,6-trimethylcyclohexa-1,3-dien-1-yl)but-3-en-2-one (Dehydro-beta-ionone) | 1203-08-3 | 29.2 | 1474 | 0.00 | 0.10 | 0.01 |
41 | 1-(4-(tert-butyl)-2,6-dimethylphenyl)ethan-1-one | 2040-10-0 | 33.3 | 1584 | 0.00 | 0.14 | 0.04 |
42 | (E)-3,5,5-trimethyl-4-(3-oxobut-1-en-1-yl)cyclohex-2-en-1-one | 20194-68-7 | 35.0 | 1654 | 0.00 | 0.09 | 0.02 |
Acids | |||||||
43 | nonanoic acid | 112-05-0 | 23.2 | 1288 | 0.00 | 0.27 | 0.11 |
Terpenoids | |||||||
44 | 1-methyl-4-propan-2-ylbenzene (p-cymene) | 99-87-6 | 14.9 | 1022 | 0.00 | 0.15 | 0.01 |
45 | 1-methyl-4-(prop-1-en-2-yl)benzene (p-cymenene) | 1195-32-0 | 17.2 | 1090 | 0.00 | 0.18 | 0.02 |
46 | 1-methoxy-4-propylbenzene (4-propylanisole) | 104-45-0 | 23.5 | 1299 | 0.00 | 0.83 | 0.04 |
Others | |||||||
47 | (2S,8aR)-2,5,5,8a-tetramethyl-3,5,6,8a-tetrahydro-2H-chromene | 41678-29-9 | 23.9 | 1306 | 0.00 | 0.09 | 0.01 |
48 | 1,1,5-trimethyl-1,2-dihydronaphthalene | 357258 c | 25.2 | 1352 | 0.00 | 0.19 | 0.08 |
49 | 8-isopropyl-1-methyl-1,2,3,4-tetrahydronaphthalene | 81603-43-2 | 31.5 | 1535 | 0.00 | 0.11 | 0.05 |
Response | Volatile Compound | Min (%Area) | Max (%Area) | Mean (%Area) | Std. Dev. |
---|---|---|---|---|---|
R1 | benzaldehyde | 1.59 | 6.70 | 4.52 | 1.22 |
R2 | 3,5,5-trimethylcyclohex-2-en-1-one | 0.00 | 1.11 | 0.59 | 0.36 |
R3 | 2,6,6-trimethylcyclohex-2-ene-1,4-dione | 0.00 | 2.90 | 1.32 | 0.75 |
R4 | 2-hydroxy-3,5,5-trimethylcyclohex-2-en-1-one | 0.53 | 2.88 | 1.42 | 0.55 |
R5 | 2,6,6-trimethylcyclohexa-1,3-diene-1-carbaldehyde | 0.98 | 4.57 | 2.37 | 0.81 |
R6 | 4-methoxybenzaldehyde | 0.00 | 13.52 | 6.25 | 4.07 |
R7 | 3,4,5-trimethylphenol | 0.00 | 0.72 | 0.22 | 0.29 |
R8 | 1,1,5-trimethyl-1,2-dihydronaphthalene | 0.00 | 6.09 | 2.00 | 1.53 |
R9 | (E)-1-(2,6,6-trimethylcyclohexa-1,3-dien-1-yl)but-2-en-1-one | 0.00 | 1.80 | 1.13 | 0.40 |
R10 | (E)-1,6,6-trimethyl-7-(3-oxobut-1-en-1-yl)-3,8-dioxatricyclo[5.1.0.02,4]octan-5-one | 0.00 | 1.38 | 0.63 | 0.53 |
R11 | ethyl 4-methoxybenzoate | 0.00 | 3.96 | 1.39 | 1.30 |
R12 | (E)-4-(2,6,6-trimethylcyclohexa-1,3-dien-1-yl)but-3-en-2-one | 0.00 | 2.18 | 0.37 | 0.48 |
R13 | 4,6,10,10-tetramethyl-5-oxatricyclo[4.4.0.01,4]dec-2-en-7-ol | 0.00 | 1.35 | 0.75 | 0.40 |
ANOVA (p-Value < 0.05) | Box-Cox | R2 | ||||||||
---|---|---|---|---|---|---|---|---|---|---|
Response | A * | B * | C * | D * | E * | F * | CI Low a | Current Lambda | CI High a | |
R1 | 0.19 | 0.50 | 0.40 | 0.35 | 0.60 | 0.00 | 0.26 | 1.00 | 3.02 | 0.988 |
R2 | 0.23 | 0.84 | 0.11 | 0.05 | 0.04 | 0.01 | −0.04 | 1.00 | 1.09 | 0.979 |
R3 | 0.09 | 0.12 | 0.54 | 0.19 | 0.44 | 0.00 | 0.28 | 1.00 | 1.24 | 0.988 |
R4 | 0.00 | 0.30 | 0.33 | 0.44 | 0.11 | 0.04 | −1.63 | 1.00 | 2.28 | 0.932 |
R5 | 0.09 | 0.53 | 0.73 | 0.36 | 0.17 | 0.07 | −2.22 | 1.00 | 2.35 | 0.895 |
R6 | 0.00 | 0.53 | 0.00 | 0.64 | 0.74 | 0.00 | 0.33 | 1.00 | 2.35 | 0.997 |
R7 | 0.39 | 0.05 | 0.74 | 0.52 | 0.35 | 0.00 | −0.79 | 1.00 | 1.23 | 0.978 |
R8 | 0.00 | 0.41 | 0.37 | 0.07 | 0.59 | 0.00 | 0.00 | 1.00 | 1.88 | 0.985 |
R9 | 0.66 | 0.95 | 0.35 | 0.18 | 0.12 | 0.00 | 0.70 | 1.00 | 2.85 | 0.956 |
R10 | 0.00 | 0.39 | 0.97 | 0.24 | 0.32 | 0.09 | −0.17 | 1.00 | 1.78 | 0.991 |
R11 | 0.00 | 0.32 | 0.01 | 0.70 | 0.23 | 0.00 | −0.11 | 1.00 | 0.83 | 0.988 |
R12 | 0.11 | 0.31 | 0.66 | 0.18 | 0.98 | 0.72 | −0.61 | 1.00 | 1.40 | 0.913 |
R13 | 0.29 | 0.04 | 0.08 | 0.13 | 0.37 | 0.01 | 0.30 | 1.00 | 2.02 | 0.986 |
R1 | MT a | F | AD | DF | B2 | D2 | |||
CE b | +0.69 | +0.31 | +0.39 | +0.75 | −0.81 | ||||
R2 | MT | E | F | AC | AF | ||||
CE | +0.08 | +0.21 | −0.13 | −0.28 | |||||
R3 | MT | F | AC | AF | CF | DE | A2 | D2 | |
CE | +0.56 | −0.20 | +0.14 | +0.20 | +0.13 | −0.42 | −0.43 | ||
R4 | MT | A | F | ||||||
CE | −0.47 | +0.21 | |||||||
R5 | MT | No significant model terms | |||||||
CE | |||||||||
R6 | MT | A | C | F | |||||
CE | +0.99 | +0.53 | −0.14 | ||||||
R7 | MT | F | AB | AC | AD | BD | CF | A2 | E2 |
CE | −0.18 | +0.10 | +0.09 | +0.08 | −0.09 | −0.06 | +0.17 | +0.31 | |
R8 | MT | A | F | AF | |||||
CE | −0.88 | −0.12 | +0.60 | ||||||
R9 | MT | F | A2 | ||||||
CE | +0.21 | −0.39 | |||||||
R10 | MT | A | A2 | ||||||
CE | +0.50 | −0.42 | |||||||
R11 | MT | A | C | F | AF | ||||
CE | +0.96 | +0.27 | +0.60 | +0.40 | |||||
R12 | MT | No significant model terms | |||||||
CE | |||||||||
R13 | MT | B | F | AB | AF | BE | DE | E2 | |
CE | −0.09 | +0.16 | −0.12 | +0.13 | +0.12 | −0.11 | −0.21 |
Response | A * | B * | C * | D * | E * | F * | Desirability | Predicted Mean (%Area) |
---|---|---|---|---|---|---|---|---|
R1 | 60 | 5 | 60 | 700 | 6 | 1:1 | 1.000 | 4.07 ± 0.36 |
R2 | 45 | 30 | 15 | 700 | 2 | 1:3 | 1.000 | 0.96 ± 0.18 |
R3 | 60 | 30 | 15 | 100 | 4 | 1:3 | 1.000 | 1.63 ± 0.22 |
R4 | 60 | 30 | 15 | 100 | 4 | 1:3 | 1.000 | 0.85 ± 0.19 |
R5 | 45 | 30 | 15 | 100 | 6 | 1:3 | 1.000 | 1.97 ± 0.71 |
R6 | 60 | 15 | 15 | 100 | 2 | 1:3 | 1.000 | 12.61 ± 0.64 |
R7 | 45 | 30 | 15 | 100 | 6 | 1:3 | 1.000 | 0.11 ± 0.02 |
R8 | 60 | 5 | 15 | 700 | 6 | 1:3 | 1.000 | 0.64 ± 0.11 |
R9 | 60 | 15 | 30 | 400 | 2 | 1:3 | 1.000 | 0,77 ± 0.23 |
R10 | 60 | 30 | 30 | 100 | 4 | 1:3 | 1.000 | 0.84 ± 0.22 |
R11 | 60 | 30 | 15 | 100 | 2 | 1:1 | 1.000 | 2.48 ± 0.39 |
R12 | 60 | 30 | 60 | 700 | 6 | 1:3 | 1.000 | 1.09 ± 0.39 |
R13 | 60 | 30 | 15 | 700 | 6 | 1:1 | 1.000 | 0.98 ± 0.27 |
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Xagoraris, M.; Chrysoulaki, F.; Revelou, P.-K.; Alissandrakis, E.; Tarantilis, P.A.; Pappas, C.S. Unifloral Autumn Heather Honey from Indigenous Greek Erica manipuliflora Salisb.: SPME/GC-MS Characterization of the Volatile Fraction and Optimization of the Isolation Parameters. Foods 2021, 10, 2487. https://doi.org/10.3390/foods10102487
Xagoraris M, Chrysoulaki F, Revelou P-K, Alissandrakis E, Tarantilis PA, Pappas CS. Unifloral Autumn Heather Honey from Indigenous Greek Erica manipuliflora Salisb.: SPME/GC-MS Characterization of the Volatile Fraction and Optimization of the Isolation Parameters. Foods. 2021; 10(10):2487. https://doi.org/10.3390/foods10102487
Chicago/Turabian StyleXagoraris, Marinos, Foteini Chrysoulaki, Panagiota-Kyriaki Revelou, Eleftherios Alissandrakis, Petros A. Tarantilis, and Christos S. Pappas. 2021. "Unifloral Autumn Heather Honey from Indigenous Greek Erica manipuliflora Salisb.: SPME/GC-MS Characterization of the Volatile Fraction and Optimization of the Isolation Parameters" Foods 10, no. 10: 2487. https://doi.org/10.3390/foods10102487