High Voltage Electrical Discharges as an Alternative Extraction Process of Phenolic and Volatile Compounds from Wild Thyme (Thymus serpyllum L.): In Silico and Experimental Approaches for Solubility Assessment
Abstract
:1. Introduction
2. Results
2.1. Theoretical Prediction
2.2. Experimental Procedure
3. Discussion
3.1. Theoretical Prediction of Solubility of Wild Thyme Compounds in Green Solvents
3.1.1. Wild Thyme Compounds Solubility in Green Solvents by HSPs
3.1.2. Wild Thyme Compounds Solubility in Green Solvents Assessed by COSMO-RS Software
3.1.3. Principal Component Analysis (PCA) of Theoretical Prediction Results
3.2. Experimental Assessment of Extraction of Wild Thyme Bioactive Compounds by Means of High Voltage Electrical Discharge (HVED)
3.2.1. Physical Properties of Wild Thyme Etracts Obtained by HVED Compared to Conventional Extraction
3.2.2. Effect of HVED-Assisted Extraction on Recovery of Bioactive Compounds from Wild Thyme
3.2.3. Effect of HVED on Phenolic Composition of the Extracts
3.2.4. Effect of HVED on the Content of Volatile Compounds in Wild Thyme Extracts
3.2.5. Determination of Pesticides and Heavy Metals in Wild Thyme Samples
4. Materials and Methods
4.1. Theoretical Prediction
4.1.1. Hansen Solubility Parameters (HSPs)
4.1.2. Conductor-Like Screening Model for Real Solvents (COSMO-RS) Software
4.2. Experimental Procedure
4.2.1. Plant Materials
4.2.2. High Voltage Electrical Discharge (HVED) and Conventional Extraction
4.2.3. Physical Properties of Wild Thyme Extracts
4.2.4. Determination of Total Phenolic Content (TPC)
4.2.5. Determination of Antioxidant Capacity
2,2-Diphenyl-2-Picrylhydrazyl (DPPH) Free Radical Assay
Ferric Reducing Antioxidant Power (FRAP) Assay
4.2.6. Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Characterization of Phenolic Compounds (UPLC-MS/MS)
4.2.7. Headspace Solid-Phase Microextraction (HS-SPME) Followed by Gas Chromatography and Mass Spectrometry Analysis (GC-MS)
4.2.8. Determination of Pesticides and Metals in Thyme Samples
4.2.9. Experimental Design and Statistical Analysis
5. Conclusions
Supplementary Materials
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Sample Availability: Samples of the compounds are not available from the authors. |
Solvents | n-Hexane | Ethyl Acetate | Methyl Acetate | Ethyloleate | Ethanol | 1-Butanol | Isopropanol | Methanol | Limonene | α-Pinene | Cymene | β-Myrcene | CPME | DMC | MeTHF | Water |
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Monoterpenes | ||||||||||||||||
Carvacrol | 2.52 | 1.21 | 1.97 | 1.43 | 3.43 | 2.37 | 2.56 | 4.58 | 0.96 | 1.64 | 1.29 | 1.49 | 1.12 | 1.76 | 0.93 | 9.34 |
Thymol | 2.52 | 1.21 | 1.97 | 1.43 | 3.43 | 2.37 | 2.56 | 4.58 | 0.96 | 1.64 | 1.29 | 1.49 | 1.12 | 1.76 | 0.93 | 9.34 |
Carene | 0.94 | 1.75 | 3.05 | 0.40 | 4.77 | 3.64 | 3.82 | 5.86 | 0.72 | 0.00 | 0.59 | 0.32 | 0.77 | 2.65 | 1.18 | 10.75 |
α-thujene | 1.10 | 1.70 | 3.03 | 0.41 | 4.73 | 3.62 | 3.80 | 5.82 | 0.63 | 0.20 | 0.40 | 0.37 | 0.70 | 2.56 | 1.09 | 10.72 |
α-terpinene | 1.35 | 1.46 | 2.66 | 0.40 | 4.34 | 3.21 | 3.40 | 5.46 | 0.30 | 0.47 | 0.51 | 0.38 | 0.52 | 2.35 | 0.87 | 10.32 |
δ-terpinene | 1.33 | 1.42 | 2.63 | 0.35 | 4.33 | 3.20 | 3.10 | 5.44 | 0.34 | 0.46 | 0.54 | 0.34 | 0.48 | 2.32 | 0.84 | 15.50 |
Oxygenated monoterpenes | ||||||||||||||||
Borneol | 2.28 | 0.91 | 1.72 | 1.22 | 3.33 | 2.23 | 2.42 | 4.46 | 0.90 | 1.50 | 1.30 | 1.28 | 0.90 | 1.63 | 0.71 | 9.30 |
α-terpineol | 2.37 | 0.98 | 1.68 | 1.32 | 3.26 | 2.15 | 2.34 | 4.40 | 0.97 | 1.58 | 1.38 | 1.37 | 1.01 | 1.67 | 0.82 | 9.22 |
α-Cadinol | 1.89 | 1.24 | 2.35 | 0.82 | 3.95 | 2.85 | 3.04 | 5.08 | 0.32 | 0.99 | 0.69 | 0.86 | 0.61 | 2.02 | 0.67 | 9.91 |
Linalool | 2.10 | 1.02 | 1.86 | 1.07 | 3.49 | 2.37 | 2.56 | 4.63 | 0.73 | 1.32 | 1.17 | 1.11 | 0.80 | 1.82 | 0.72 | 9.46 |
Piperitone | 1.82 | 1.18 | 2.62 | 0.80 | 4.22 | 3.19 | 3.37 | 5.28 | 0.74 | 1.02 | 0.63 | 0.88 | 0.55 | 1.86 | 0.57 | 10.19 |
Sesquiterpenes | ||||||||||||||||
β-caryophyllene | 1.04 | 1.73 | 2.97 | 0.42 | 4.68 | 3.54 | 3.73 | 5.78 | 0.61 | 0.14 | 0.57 | 0.33 | 0.74 | 2.63 | 1.15 | 10.65 |
Copaene | 1.02 | 1.97 | 3.29 | 0.65 | 4.99 | 3.86 | 4.05 | 4.09 | 0.83 | 0.29 | 0.55 | 0.59 | 0.97 | 2.83 | 1.36 | 10.97 |
α-cubebene | 1.17 | 1.75 | 2.98 | 0.50 | 4.67 | 3.53 | 3.72 | 5.79 | 0.52 | 0.25 | 0.46 | 0.43 | 0.77 | 2.64 | 1.15 | 10.64 |
β-elemene | 0.83 | 1.77 | 3.12 | 0.42 | 5.92 | 3.73 | 3.91 | 4.85 | 0.87 | 0.18 | 0.68 | 0.35 | 0.80 | 2.65 | 1.21 | 10.84 |
β-cadinene | 1.10 | 1.69 | 2.94 | 0.40 | 4.64 | 3.51 | 3.69 | 5.74 | 0.55 | 0.18 | 0.50 | 0.32 | 0.70 | 2.58 | 1.09 | 10.62 |
δ-cadinene | 0.93 | 1.85 | 3.15 | 0.50 | 4.86 | 3.73 | 3.91 | 5.95 | 0.77 | 0.10 | 0.60 | 0.42 | 0.86 | 2.73 | 1.26 | 10.84 |
Oxygenated Sesquiterpenes | ||||||||||||||||
Isospathulenol | 1.97 | 1.26 | 2.25 | 0.92 | 3.84 | 2.73 | 2.92 | 4.99 | 0.39 | 1.09 | 0.83 | 0.95 | 0.72 | 2.05 | 0.76 | 9.79 |
Diterpenes | ||||||||||||||||
Carnosic acid | 2.99 | 1.69 | 2.05 | 1.94 | 3.29 | 2.26 | 2.46 | 4.48 | 1.38 | 2.10 | 1.72 | 1.98 | 1.66 | 2.09 | 1.48 | 9.09 |
Triterpenes | ||||||||||||||||
Rosmarinic acid | 4.56 | 2.95 | 2.76 | 3.49 | 3.11 | 2.55 | 2.69 | 4.20 | 2.93 | 3.65 | 3.18 | 3.53 | 3.17 | 2.85 | 2.91 | 8.29 |
Flavanons | ||||||||||||||||
Naringenin | 4.86 | 2.95 | 2.70 | 3.76 | 2.82 | 2.50 | 2.60 | 3.76 | 3.30 | 3.98 | 3.52 | 3.82 | 3.39 | 2.59 | 3.06 | 7.92 |
Eriodictyol | 4.53 | 2.75 | 2.89 | 3.44 | 3.31 | 2.85 | 2.98 | 4.26 | 2.99 | 3.64 | 3.13 | 3.50 | 3.08 | 2.43 | 2.77 | 8.55 |
Flavonoids | ||||||||||||||||
Apigenin | 4.37 | 2.78 | 2.61 | 3.30 | 3.07 | 2.43 | 2.59 | 4.19 | 2.74 | 3.46 | 3.01 | 3.35 | 2.99 | 2.74 | 2.74 | 8.35 |
Luteolin | 4.06 | 2.66 | 2.89 | 3.01 | 3.59 | 2.87 | 3.04 | 4.07 | 2.45 | 3.13 | 2.62 | 3.05 | 2.72 | 2.68 | 2.50 | 8.98 |
Thymusin | 4.25 | 2.68 | 2.57 | 3.18 | 3.11 | 2.44 | 2.60 | 4.23 | 2.63 | 3.34 | 2.88 | 3.23 | 2.87 | 2.65 | 2.62 | 8.45 |
Kaempherol-3-glucuronide | 5.73 | 3.62 | 2.85 | 4.64 | 2.17 | 2.40 | 2.41 | 2.85 | 4.24 | 4.91 | 4.53 | 4.71 | 4.26 | 3.10 | 3.90 | 6.71 |
Apigenin 6.8-di-c-glucoside | 3.87 | 2.12 | 2.42 | 2.78 | 3.18 | 2.52 | 2.67 | 4.22 | 2.35 | 2.99 | 2.51 | 2.85 | 2.42 | 1.93 | 2.11 | 8.75 |
Other Oxygenated | ||||||||||||||||
Quinic acid | 6.23 | 4.02 | 2.90 | 5.20 | 1.57 | 2.37 | 2.27 | 1.82 | 4.89 | 5.51 | 5.21 | 5.27 | 4.82 | 3.43 | 4.44 | 5.70 |
Caffeic acid | 5.94 | 4.03 | 3.15 | 4.87 | 2.46 | 2.47 | 2.59 | 3.27 | 4.38 | 5.09 | 4.71 | 4.92 | 4.53 | 3.71 | 4.22 | 6.66 |
Protocatechuic acid | 5.99 | 4.01 | 3.15 | 4.91 | 2.41 | 2.60 | 2.62 | 3.16 | 4.44 | 5.14 | 4.75 | 4.97 | 4.56 | 3.62 | 4.23 | 6.61 |
p-coumaric acid | 5.25 | 3.36 | 2.60 | 4.18 | 2.28 | 2.11 | 2.18 | 3.27 | 3.70 | 4.40 | 4.02 | 4.23 | 3.84 | 3.10 | 3.53 | 7.14 |
Vanillin | 4.74 | 2.69 | 2.47 | 3.64 | 2.61 | 2.34 | 2.43 | 3.49 | 3.25 | 3.90 | 3.46 | 3.71 | 3.25 | 2.20 | 2.89 | 7.84 |
Vanillic acid | 5.03 | 3.06 | 2.42 | 3.94 | 2.25 | 2.04 | 2.11 | 3.23 | 3.48 | 4.18 | 3.78 | 4.00 | 3.58 | 2.72 | 3.25 | 7.32 |
Vitamins (antioxidants) | ||||||||||||||||
α-tocopherol | 1.40 | 1.53 | 2.72 | 0.48 | 4.39 | 3.26 | 3.44 | 5.51 | 0.24 | 0.48 | 0.44 | 0.46 | 0.59 | 2.40 | 0.92 | 10.36 |
Ascorbic acid | 7.84 | 5.70 | 4.56 | 6.79 | 3.07 | 3.92 | 3.83 | 2.97 | 6.40 | 7.07 | 6.72 | 6.85 | 6.41 | 5.12 | 6.05 | 4.79 |
Solvents | n-Hexane | Ethyl Acetate | Methyl Acetate | Ethyloleate | Ethanol | 1-Butanol | Isopropanol | Methanol | Limonene | α-Pinene | Cymene | β-Myrcene | CPME | DMC | MeTHF | Water |
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Monoterpenes | ||||||||||||||||
Carvacrol | 10.96 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 30.90 | 16.98 | 34.67 | 33.11 | 100.00 | 100.00 | 100.00 | 0.03 |
Thymol | 16.98 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 70.79 | 38.90 | 24.55 | 45.71 | 43.65 | 100.00 | 100.00 | 100.00 | 0.01 |
Carene | 91.54 | 55.13 | 37.70 | 100.00 | 11.81 | 23.92 | 18.75 | 4.29 | 99.29 | 97.71 | 92.21 | 93.52 | 99.45 | 24.40 | 95.92 | 0.00 |
α-thujene | 93.33 | 51.29 | 33.88 | 100.00 | 10.47 | 22.39 | 18.62 | 3.89 | 98.40 | 98.86 | 89.13 | 91.20 | 97.72 | 21.38 | 93.33 | 0.00 |
α-terpinene | 87.10 | 60.26 | 41.69 | 100.00 | 12.02 | 23.99 | 19.05 | 4.27 | 100.00 | 95.50 | 95.50 | 97.72 | 100.00 | 27.54 | 100.00 | 0.00 |
γ-terpinene | 87.10 | 58.88 | 41.69 | 100.00 | 11.48 | 22.91 | 18.20 | 4.17 | 99.91 | 95.50 | 95.50 | 97.72 | 100.00 | 26.92 | 98.86 | 0.00 |
Oxygenated monoterpenes | ||||||||||||||||
Borneol | 11.22 | 100.00 | 89.13 | 81.28 | 85.11 | 100.00 | 100.00 | 41.69 | 17.78 | 13.49 | 16.98 | 16.60 | 100.00 | 38.02 | 100.00 | 0.02 |
α-terpineol | 11.22 | 75.86 | 57.54 | 50.12 | 60.26 | 87.10 | 77.62 | 30.90 | 20.42 | 14.45 | 20.89 | 20.42 | 97.72 | 31.62 | 100.00 | 0.02 |
α-Cadinol | 32.35 | 100.00 | 81.28 | 100.00 | 41.68 | 70.79 | 63.09 | 14.12 | 42.65 | 35.48 | 38.01 | 37.15 | 100.00 | 30.90 | 100.00 | 0.00 |
Linalool | 13.18 | 100.00 | 93.33 | 64.57 | 52.48 | 70.79 | 66.07 | 25.70 | 25.70 | 17.38 | 28.18 | 26.92 | 100.00 | 48.98 | 100.00 | 0.01 |
Piperitone | 32.35 | 100.00 | 89.12 | 85.11 | 91.20 | 100.00 | 100.00 | 51.28 | 72.44 | 46.77 | 87.09 | 83.17 | 87.09 | 70.79 | 100.00 | 0.06 |
Sesquiterpenes | ||||||||||||||||
β-caryophyllene | 99.95 | 53.70 | 33.11 | 100.00 | 7.94 | 18.62 | 14.12 | 2.34 | 100.00 | 100.00 | 89.12 | 89.53 | 100.00 | 18.19 | 100.00 | 0.00 |
Copaene | 100.00 | 31.62 | 17.78 | 93.32 | 6.02 | 15.48 | 11.22 | 1.47 | 93.32 | 100.00 | 74.13 | 75.85 | 95.49 | 8.91 | 89.12 | 0.00 |
α-cubebene | 100.00 | 37.15 | 21.37 | 97.72 | 6.30 | 16.21 | 11.48 | 1.62 | 97.72 | 100.00 | 81.28 | 81.28 | 100.00 | 10.96 | 97.72 | 0.00 |
β-elemene | 83.17 | 79.43 | 54.95 | 100.00 | 10.00 | 19.49 | 15.48 | 3.23 | 100.00 | 91.20 | 100.00 | 99.83 | 100.00 | 32.35 | 100.00 | 0.00 |
β-cadinene | 100.00 | 45.70 | 27.54 | 100.00 | 7.07 | 16.98 | 12.58 | 1.86 | 99.83 | 100.00 | 85.11 | 85.11 | 100.00 | 14.45 | 100.00 | 0.00 |
δ-cadinene | 100.00 | 47.86 | 28.18 | 100.00 | 7.76 | 18.19 | 13.80 | 2.18 | 99.54 | 100.00 | 85.11 | 85.11 | 100.00 | 15.13 | 100.00 | 0.00 |
Oxygenated Sesquiterpenes | ||||||||||||||||
Isospathulenol | 13.48 | 99.90 | 69.18 | 61.65 | 47.86 | 75.85 | 74.13 | 20.89 | 21.87 | 16.21 | 21.37 | 20.41 | 100.00 | 28.84 | 100.00 | 0.00 |
Diterpenes | ||||||||||||||||
Carnosic acid | 0.86 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 3.37 | 1.41 | 3.89 | 3.49 | 100.00 | 100.00 | 100.00 | 0.00 |
Triterpenes | ||||||||||||||||
Rosmarinic acid | 0.00 | 100.00 | 100.00 | 34.92 | 100.00 | 100.00 | 100.00 | 100.00 | 0.07 | 0.01 | 0.13 | 0.11 | 100.00 | 100.00 | 100.00 | 0.02 |
Flavanons | ||||||||||||||||
Naringenin | 0.00 | 100.00 | 100.00 | 76.03 | 100.00 | 100.00 | 100.00 | 100.00 | 0.07 | 0.01 | 0.12 | 0.10 | 100.00 | 100.00 | 100.00 | 0.31 |
Eriodictyol | 0.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 0.03 | 0.00 | 0.05 | 0.04 | 100.00 | 100.00 | 100.00 | 0.89 |
Flavonoids | ||||||||||||||||
Apigenin | 0.00 | 100.00 | 100.00 | 25.70 | 100.00 | 100.00 | 100.00 | 100.00 | 0.02 | 0.00 | 0.03 | 0.03 | 100.00 | 100.00 | 100.00 | 0.18 |
Luteolin | 0.00 | 100.00 | 100.00 | 54.95 | 100.00 | 100.00 | 100.00 | 100.00 | 0.01 | 0.00 | 0.02 | 0.04 | 100.00 | 100.00 | 100.00 | 0.46 |
Thymusin | 0.02 | 100.00 | 100.00 | 33.11 | 100.00 | 100.00 | 100.00 | 100.00 | 0.28 | 0.06 | 0.52 | 0.46 | 100.00 | 100.00 | 100.00 | 0.00 |
Kaempherol-3-glucuronide | 0.00 | 100.00 | 100.00 | 21.11 | 100.00 | 100.00 | 100.00 | 100.00 | 0.00 | 0.00 | 0.00 | 0.00 | 100.00 | 100.00 | 100.00 | 0.46 |
Apigenin 6.8-di-c-glucoside | 0.00 | 9.70 | 17.80 | 0.00 | 100.00 | 100.00 | 100.00 | 100.00 | 0.00 | 0.00 | 0.00 | 0.00 | 1.63 | 0.17 | 100.00 | 3.04 |
Other Oxygenated | ||||||||||||||||
Quinic acid | 0.00 | 100.00 | 100.00 | 0.21 | 100.00 | 100.00 | 100.00 | 100.00 | 0.00 | 0.00 | 0.00 | 0.00 | 80.75 | 12.09 | 100.00 | 66.50 |
Caffeic acid | 0.00 | 100.00 | 100.00 | 0.19 | 100.00 | 100.00 | 100.00 | 100.00 | 0.00 | 0.00 | 0.00 | 0.00 | 100.00 | 20.89 | 100.00 | 85.11 |
Protocatechuic acid | 0.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 0.03 | 0.01 | 0.05 | 0.04 | 100.00 | 100.00 | 100.00 | 48.04 |
p-coumaric acid | 0.00 | 100.00 | 100.00 | 13.27 | 100.00 | 100.00 | 100.00 | 100.00 | 0.02 | 0.00 | 0.03 | 0.03 | 100.00 | 100.00 | 100.00 | 2.57 |
Vanillin | 1.07 | 100.00 | 100.00 | 20.89 | 67.61 | 50.12 | 58.88 | 54.95 | 4.90 | 2.09 | 7.59 | 7.08 | 72.44 | 91.20 | 100.00 | 0.17 |
Vanillic acid | 0.01 | 100.00 | 100.00 | 7.94 | 100.00 | 100.00 | 100.00 | 100.00 | 0.11 | 0.03 | 0.18 | 0.16 | 100.00 | 93.33 | 100.00 | 1.29 |
Vitamins (antioxidants) | ||||||||||||||||
Ascorbic acid | 0.00 | 100.00 | 100.00 | 0.50 | 100.00 | 100.00 | 100.00 | 100.00 | 0.00 | 0.00 | 0.00 | 0.00 | 100.00 | 25.91 | 100.00 | 100.00 |
α-tocopherol | 66.24 | 100.00 | 100.00 | 100.00 | 15.19 | 42.93 | 33.22 | 1.86 | 89.33 | 67.94 | 73.87 | 69.41 | 100.00 | 23.24 | 100.00 | 0.00 |
Sample | pH | Conductivity (μS/cm) | Starting Temperature (°C) | Final Temperature (°C) | Power (kW) | Zp | Extraction Type |
---|---|---|---|---|---|---|---|
3 T0 | 5.91 ± 0.20 | 621.0 ± 13.2 | 20.6 ± 0.1 | / | / | / | CE |
9 T0 | 5.77 ± 0.17 | 560.0 ± 22.3 | 20.6 ± 0.4 | / | / | / | |
3 T25 | 6.06 ± 0.29 | 319.0 ± 12.5 | 20.9 ± 0.9 | / | / | / | |
9 T25 | 6.03 ± 0.23 | 283.7 ± 2.6 | 20.9 ± 1.2 | / | / | / | |
3 T50 | 6.28 ± 0.34 | 133.8 ± 12.1 | 20.2 ± 0.3 | / | / | / | |
9 T50 | 6.28 ± 0.18 | 121.8 ± 9.1 | 20.4 ± 0.1 | / | / | / | |
TN1 | 6.13 ± 0.12 | 169.0 ± 2.3 | 23.3 ± 1.3 | 23.9 ± 1.7 | 12.0 ± 0.0 | 0.15 | HVED extraction |
TN2 | 5.82 ± 0.71 | 522.0 ± 12.1 | 24.7 ± 0.2 | 27.5 ± 0.5 | 16.0 ± 1.0 | 0.28 | |
TN3 | 5.82 ± 0.32 | 566.0 ± 20.4 | 24.7 ± 0.8 | 25.3 ± 0.4 | 14.0 ± 2.0 | 0.41 | |
TN4 | 5.83 ± 0.61 | 556.0 ± 13.2 | 25.1 ± 0.7 | 25.3 ± 1.3 | 12.0 ± 0.0 | 0.33 | |
TN5 | 6.04 ± 0.19 | 299.0 ± 12.8 | 25.0 ± 0.4 | 25.5 ± 0.5 | 22.0 ± 1.0 | 0.15 | |
TN6 | 6.02 ± 0.81 | 256.0 ± 8.1 | 23.8 ± 0.1 | 25.1 ± 0.9 | 12.0 ± 1.0 | 0.05 | |
TN7 | 6.31 ± 0.15 | 118.0 ± 11.3 | 22.4 ± 1.1 | 25.2 ± 1.5 | 11.0 ± 2.0 | 0.02 | |
TN8 | 6.22 ± 0.33 | 115.0 ± 12.7 | 22.8 ± 0.3 | 24.7 ± 0.6 | 17.0 ± 0.0 | 0.01 | |
TN9 | 6.08 ± 0.71 | 263.0 ± 20.1 | 24.2 ± 0.2 | 24.5 ± 1.3 | 17.0 ± 3.0 | 0.02 | |
TN10 | 5.77 ± 0.11 | 612.0 ± 30.4 | 24.4 ± 0.6 | 32.1 ± 2.0 | 22.0 ± 1.0 | 0.73 | |
TN11 | 6.24 ± 1.02 | 114.0 ± 12.5 | 24.6 ± 1.2 | 25.2 ± 0.6 | 20.0 ± 1.0 | 0.06 | |
TN12 | 6.15 ± 0.26 | 169.0 ± 20.1 | 24.5 ± 2.1 | 25.1 ± 1.9 | 12.0 ± 0.0 | 0.03 | |
TA1 | 6.13 ± 0.42 | 94.7 ± 11.8 | 25.0 ± 0.8 | 25.1 ± 2.2 | 8.0 ± 1.0 | 0.02 | |
TA2 | 5.39 ± 0.38 | 646.0 ± 30.1 | 25.6 ± 1.1 | 37.8 ± 1.3 | 12.0 ± 2.0 | 1.00 | |
TA3 | 5.40 ± 0.27 | 590.0 ± 13.7 | 25.3 ± 0.2 | 29.0 ± 0.9 | 9.0 ± 0.0 | 0.59 | |
TA4 | 5.55 ± 0.16 | 608.0 ± 14.6 | 25.2 ± 2.0 | 27.9 ± 1.4 | 14.0 ± 1.0 | 0.72 | |
TA5 | 5.76 ± 0.21 | 351.0 ± 13.9 | 21.3 ± 0.5 | 31.2 ± 2.3 | 16.0 ± 2.0 | 0.28 | |
TA6 | 5.50 ± 0.34 | 280.0 ± 7.1 | 25.0 ± 0.4 | 28.5 ± 0.9 | 10.0 ± 0.0 | 0.10 | |
TA7 | 5.12 ± 0.18 | 109.6 ± 9.6 | 23.6 ± 1.7 | 25.1 ± 1.1 | 9.0 ± 1.0 | 0.00 | |
TA8 | 6.12 ± 1.12 | 116.4 ± 11.5 | 20.4 ± 2.3 | 27.4 ± 0.8 | 17.0 ± 2.0 | 0.06 | |
TA9 | 5.88 ± 0.51 | 246.2 ± 12.4 | 25.1 ± 0.1 | 26.1 ± 1.2 | 14.0 ± 0.0 | 0.13 | |
TA10 | 5.60 ± 0.40 | 605.0 ± 17.4 | 23.2 ± 0.4 | 32.3 ± 0.1 | 16.0 ± 1.0 | 0.67 | |
TA11 | 6.19 ± 0.18 | 89.0 ± 6.3 | 23.6 ± 2.4 | 24.1 ± 0.2 | 12.0 ± 1.0 | 0.01 | |
TA12 | 5.91 ± 0.26 | 222.7 ± 20.3 | 23.8 ± 1.5 | 25.2 ± 0.6 | 9.0 ± 0.0 | 0.08 |
Sample | Concentration (ng/mL) | Extraction Type | |||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Apigenin | Carnosol | Diosmetin | Hydroxytyrosol | Luteolin | Oleanolic Acid | Quercetin | Rosmarinic Acid | p-Cymene | Thymol | Carvacrol | Camphor | ||
3 T0 | 12.114 | 0.101 | 31.051 | 12.543 | 101.718 | 4.920 | 0.220 | 3611.057 | 0.147 | 0.100 | 0.023 | 0.497 | CE |
9 T0 | N/D | 0.546 | N/D | 49.436 | N/D | 58.755 | N/D | 1.983 | 1.255 | 0.023 | 0.003 | 1.177 | |
3 T25 | N/D | 0.284 | 3.851 | 53.034 | 1.109 | N/D | 1.073 | 1050.120 | 0.018 | 0.857 | 0.003 | 0.145 | |
9 T25 | 45.879 | 0.273 | 32.355 | 27.798 | 226.458 | N/D | 1.794 | 6010.666 | 1.149 | 0.010 | 0.098 | 0.138 | |
3 T50 | 66.073 | 0.354 | 28.432 | 14.164 | 170.078 | 458.380 | 1.616 | 4665.132 | 0.029 | 0.041 | N/D | 10.301 | |
9 T50 | 105.846 | 3.491 | 54.155 | 33.044 | 318.747 | 810.724 | 44.725 | 5906.846 | 0.926 | 0.001 | 0.001 | 15.601 | |
TN1 | 73.998 | 1.825 | 66.335 | 33.949 | 262.150 | 345.395 | 30.299 | 5156.860 | 0.122 | 0.000 | 0.000 | 1.178 | HVED extraction |
TN2 | 21.900 | 0.116 | 35.950 | 42.139 | 233.229 | 7.658 | 2.328 | 4291.215 | 0.038 | 0.907 | 0.429 | 0.134 | |
TN3 | 16.618 | 0.083 | 35.840 | 25.589 | 157.588 | 3.713 | 1.456 | 4393.277 | 0.001 | 0.027 | 0.008 | 1.860 | |
TN4 | 23.733 | 0.122 | 39.986 | 33.498 | 225.259 | 4.512 | 1.580 | 4586.689 | 0.037 | 0.000 | 0.000 | 0.017 | |
TN5 | 38.606 | 0.242 | 32.407 | 26.316 | 211.022 | 3.339 | 1.884 | 5047.926 | 0.007 | 2.957 | 0.000 | N/D | |
TN6 | 32.662 | 0.249 | 29.816 | 22.327 | 189.079 | N/D | 1.088 | 4722.660 | 0.002 | N/D | 0.001 | 0.056 | |
TN7 | 92.601 | 3.290 | 66.702 | 31.581 | 293.050 | 559.388 | 39.952 | 5294.104 | 0.048 | 0.000 | 0.002 | 2.243 | |
TN8 | 98.111 | 11.187 | 63.431 | 37.787 | 306.348 | 1044.092 | 65.791 | 5510.994 | 0.078 | 0.000 | 0.000 | 2.328 | |
TN9 | 36.492 | 0.291 | 33.546 | 28.701 | 207.496 | 5.163 | 2.020 | 5231.490 | 0.001 | 0.000 | 0.000 | 0.067 | |
TN10 | N/D | 0.025 | 0.088 | 0.036 | 0.871 | 1.106 | N/D | 42.969 | 0.028 | 0.000 | 0.000 | 0.628 | |
TN11 | 91.870 | 4.083 | 64.151 | 31.035 | 285.800 | 561.813 | 43.709 | 5319.695 | 0.000 | 0.000 | 0.000 | 0.045 | |
TN12 | 56.268 | 0.452 | 39.586 | 25.776 | 218.796 | 19.802 | 3.778 | 4843.199 | 0.009 | 0.000 | 0.000 | 0.016 | |
TA1 | 82.733 | 6.732 | 59.872 | 31.115 | 260.344 | 869.002 | 60.758 | 5367.013 | 0.054 | 1.011 | 2.110 | 1.519 | |
TA2 | 21.497 | 0.162 | 128.078 | 285.617 | 227.339 | 5.090 | 2.631 | 4342.936 | 0.057 | 0.000 | 0.000 | N/D | |
TA3 | 22.760 | 0.239 | 39.428 | 33.397 | 183.656 | 5.541 | 2.097 | 4649.884 | 0.009 | 0.000 | 0.000 | 0.010 | |
TA4 | 23.128 | 0.118 | 44.780 | 33.985 | 216.383 | 12.748 | 2.016 | 4701.504 | 0.001 | 0.000 | 0.000 | N/D | |
TA5 | 33.864 | 0.220 | 30.660 | 27.678 | 209.574 | 3.946 | 1.579 | 4711.450 | 0.006 | 0.000 | 0.001 | N/D | |
TA6 | 48.515 | 0.443 | 43.000 | 32.625 | 306.700 | 3.738 | 1.772 | 4890.886 | 0.131 | 0.000 | 0.000 | 0.025 | |
TA7 | 88.655 | 13.187 | 55.124 | 32.586 | 262.343 | 699.078 | 37.623 | 5314.026 | 0.102 | 0.000 | 0.000 | 0.041 | |
TA8 | 86.062 | 7.819 | 58.728 | 28.403 | 290.954 | 755.546 | 50.080 | 5199.188 | N/D | 0.000 | 0.000 | 0.023 | |
TA9 | 32.634 | 0.322 | 26.486 | 25.103 | 167.677 | 4.245 | 2.197 | 4882.020 | N/D | 0.000 | 0.001 | 0.218 | |
TA10 | 40.040 | 0.107 | 74.451 | 145.722 | 431.039 | 10.132 | 38.575 | 4767.469 | 0.099 | 0.146 | 0.000 | 1.458 | |
TA11 | 98.464 | 4.025 | 52.703 | 28.518 | 254.466 | 818.490 | 50.960 | 5097.063 | 0.060 | 0.000 | 0.000 | 0.038 | |
TA12 | 29.757 | 0.159 | 27.226 | 20.202 | 177.483 | 3.595 | 1.150 | 4825.154 | 0.045 | 0.001 | 0.002 | 0.356 |
Sample | Area (%) | Extraction Type | |||
---|---|---|---|---|---|
1,8-Cineole (RI = 1038) | Linalool (RI = 1103) | Thymol (RI = 1302) | Carvacrol (RI = 1310) | ||
3 T0 | 1.40 | 14.97 | 9.12 | 14.78 | CE |
9 T0 | / | 0.21 | 0.48 | 0.47 | |
3 T25 | / | / | / | / | |
9 T25 | 1.72 | 15.03 | 9.43 | 15.20 | |
3 T50 | / | 0.30 | 0.76 | 1.21 | |
9 T50 | / | / | / | / | |
TN1 | / | / | / | / | HVED extraction |
TN2 | 1.41 | 11.36 | 9.21 | 15.30 | |
TN3 | 2.30 | 13.28 | 10.52 | 17.52 | |
TN4 | 3.46 | 13.99 | 10.08 | 17.70 | |
TN5 | / | / | 1.37 | 2.71 | |
TN6 | / | / | 1.14 | 2.44 | |
TN7 | / | / | / | / | |
TN8 | / | / | / | / | |
TN9 | / | / | 1.49 | 2.49 | |
TN10 | 0.96 | 13.00 | 11.50 | 21.86 | |
TN11 | / | / | / | / | |
TN12 | / | / | / | / | |
TA1 | / | / | / | / | |
TA2 | 1.48 | 6.01 | 9.87 | 17.49 | |
TA3 | 1.59 | 9.90 | 10.06 | 17.09 | |
TA4 | 1.22 | 11.44 | 10.41 | 17.88 | |
TA5 | / | 0.92 | 2.76 | 4.33 | |
TA6 | / | 0.61 | 1.86 | 2.85 | |
TA7 | / | / | / | / | |
TA8 | / | / | / | / | |
TA9 | / | / | 1.03 | 1.71 | |
TA10 | 1.27 | 14.42 | 11.50 | 20.55 | |
TA11 | / | / | / | / | |
TA12 | / | / | / | / |
p-Value* | ||||
---|---|---|---|---|
Main Effect | Treatment Time | Voltage | Ethanol Content | Treatment Type |
pH | 0.709 | 0.092 | <0.0001 | 0.183 |
Conductivity | 0.447 | 0.426 | <0.0001 | 0.158 |
Temperature difference | 0.000 | 0.371 | 0.017 | 0.014 |
Power | 0.015 | <0.0001 | 0.290 | 0.110 |
Zp | 0.374 | 0.619 | <0.0001 | 0.142 |
TPC | 0.125 | 0.324 | 0.017 | 0.735 |
DPPH | 0.023 | 0.904 | 0.623 | 0.463 |
FRAP | 0.358 | 0.423 | 0.030 | 0.531 |
Yield | 0.125 | 0.324 | 0.017 | 0.735 |
Sum UPLC-MS/MS | 0.549 | 0.977 | 0.000 | 0.427 |
Sum GC-MS | <0.0001 | 0.006 | <0.0001 | 0.332 |
Pesticides | MRL (mg/kg) | Content (mg/kg) |
---|---|---|
Alachlor | 0.02 | <0.005 |
Aldrin and dieldrin (aldrin and dieldrin combined expressed as dieldrin) | 0.01 | <0.002 |
Captan (sum of captan and THPI, expressed as captan) | 0.06 | <0.020 |
DDT (sum of p,p′-DDT, o,p′-DDT, p-p′-DDE and p,p′-TDE (DDD) expressed as DDT) | 0.05 | <0.004 |
Endosulfan (sum of α- and β-isomers and endosulfan-sulphate expressed as endosulfan) | 0.05 | <0.002 |
Endrin | 0.01 | <0.004 |
Heptachlor (sum of heptachlor and heptachlor epoxide expressed as heptachlor) | 0.01 | <0.002 |
Hexachlorobenzene | 0.01 | <0.002 |
Hexachlorocyclohexane, α-isomer | 0.01 | <0.002 |
Hexachlorocyclohexane, β-isomer | 0.01 | <0.002 |
Iprodione | 20.00 | <0.010 |
Lindane (γ-isomer of hexachlorocyclohexane ) | 0.01 | <0.002 |
Methoxychlor | 0.01 | <0.010 |
Tolylfluanid (sum of tolylfluanid and dimethylaminosulfotoluidide expressed as tolylfluanid) | 0.05 | <0.020 |
Vinclozolin | 0.02 | <0.002 |
Metals | MRL (mg/kg) | Dried Wild Thyme (mg/kg) | Extract (mg/kg) |
---|---|---|---|
Lead (Pb) | 3.000 | <0.050 | / |
Cadmium (Cd) | 1.000 | 0.120 | / |
Mercury (Hg) | 0.100 | 0.019 | / |
Chromium (Cr) | / | 12.000 | 56.550 |
Nickel (Ni) | / | 20.060 | 6.450 |
Manganese (Mn) | / | 115.000 | 40.750 |
Iron (Fe) | / | 1581.000 | 25.350 |
Copper (Cu) | / | 8.400 | 5.700 |
Zinc (Zn) | / | 42.000 | 13.000 |
Sample | High Voltage Treatment Time (min) | Voltage (kV) | Ethanol Content (%) | Stirring (min) | Extraction Type |
---|---|---|---|---|---|
3 T0 | 0 | 0 | 0 | 3 | CE |
9 T0 | 0 | 0 | 0 | 9 | |
3 T25 | 0 | 0 | 25 | 3 | |
9 T25 | 0 | 0 | 25 | 9 | |
3 T50 | 0 | 0 | 50 | 3 | |
9 T50 | 0 | 0 | 50 | 9 | |
TN1 | 3 | 20 | 50 | 0 | HVED extraction |
TN2 | 9 | 20 | 0 | 0 | |
TN3 | 3 | 20 | 0 | 0 | |
TN4 | 3 | 25 | 0 | 0 | |
TN5 | 9 | 25 | 25 | 0 | |
TN6 | 9 | 20 | 25 | 0 | |
TN7 | 9 | 20 | 50 | 0 | |
TN8 | 9 | 25 | 50 | 0 | |
TN9 | 3 | 25 | 25 | 0 | |
TN10 | 9 | 25 | 0 | 0 | |
TN11 | 3 | 25 | 50 | 0 | |
TN12 | 3 | 20 | 25 | 0 | |
TA1 | 3 | 15 | 50 | 0 | |
TA2 | 9 | 15 | 0 | 0 | |
TA3 | 3 | 15 | 0 | 0 | |
TA4 | 3 | 20 | 0 | 0 | |
TA5 | 9 | 20 | 25 | 0 | |
TA6 | 9 | 15 | 25 | 0 | |
TA7 | 9 | 15 | 50 | 0 | |
TA8 | 9 | 20 | 50 | 0 | |
TA9 | 3 | 20 | 25 | 0 | |
TA10 | 9 | 20 | 0 | 0 | |
TA11 | 3 | 20 | 50 | 0 | |
TA12 | 3 | 15 | 25 | 0 |
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Nutrizio, M.; Pataro, G.; Carullo, D.; Carpentieri, S.; Mazza, L.; Ferrari, G.; Chemat, F.; Banović, M.; Režek Jambrak, A. High Voltage Electrical Discharges as an Alternative Extraction Process of Phenolic and Volatile Compounds from Wild Thyme (Thymus serpyllum L.): In Silico and Experimental Approaches for Solubility Assessment. Molecules 2020, 25, 4131. https://doi.org/10.3390/molecules25184131
Nutrizio M, Pataro G, Carullo D, Carpentieri S, Mazza L, Ferrari G, Chemat F, Banović M, Režek Jambrak A. High Voltage Electrical Discharges as an Alternative Extraction Process of Phenolic and Volatile Compounds from Wild Thyme (Thymus serpyllum L.): In Silico and Experimental Approaches for Solubility Assessment. Molecules. 2020; 25(18):4131. https://doi.org/10.3390/molecules25184131
Chicago/Turabian StyleNutrizio, Marinela, Gianpiero Pataro, Daniele Carullo, Serena Carpentieri, Luisa Mazza, Giovanna Ferrari, Farid Chemat, Mara Banović, and Anet Režek Jambrak. 2020. "High Voltage Electrical Discharges as an Alternative Extraction Process of Phenolic and Volatile Compounds from Wild Thyme (Thymus serpyllum L.): In Silico and Experimental Approaches for Solubility Assessment" Molecules 25, no. 18: 4131. https://doi.org/10.3390/molecules25184131