Improvement of the Ultrasound-Assisted Extraction of Polyphenols from Welsh Onion (Allium fistulosum) Leaves Using Response Surface Methodology
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Sample Preparation
2.3. Ultrasound-Assisted Extraction
2.4. Total Polyphenols Content
2.5. Antioxidant Activity
2.5.1. DPPH Assay
2.5.2. ABTS Assay
2.5.3. FRAP Assay
2.6. UHPLC-ESI+-Orbitrap-MS Analysis
2.7. Experimental Design
2.8. Scanning Electron Microscopy (SEM)
2.9. Fourier Transform Infrared Spectroscopy (FTIR)
2.10. Statistical Analysis
3. Results and Discussion
3.1. Effect of the UAE Conditions on Total Polyphenols Content
3.2. Effect of the UAE Conditions on the DPPH Radical Scavenging Activity
3.3. Simultaneous Multi-Response Optimization
3.4. Antioxidant Activity by ABTS and FRAP
3.5. Phenolic Composition for the Extracts at the Optimal UAE Conditions Obtained by UHPLC-ESI+-Orbitrap-MS Analysis
3.6. Chemical Conformation of the Extract Obtained at the Optimal UAE Conditions
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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n | Ethanol Concentration (% v/v) | Extraction Time (min) | Temperature (°C) | TPC a,* (mg GAE/100 g) | DPPH b,* (mg Trolox/100 g) |
---|---|---|---|---|---|
1 | 35.0 | 10.0 | 30.0 | 16.87 (±1.66) | 13.09 (±1.38) |
2 | 0.0 | 10.0 | 30.0 | 25.32 (±1.56) | 16.69 (±0.69) |
3 | 70.0 | 30.0 | 30.0 | 40.35 (±1.97) | 20.54 (±0.46) |
4 | 0.0 | 30.0 | 30.0 | 41.14 (±0.43) | 18.00 (±0.32) |
5 | 0.0 | 20.0 | 30.0 | 38.95 (±0.58) | 19.09 (±1.65) |
6 | 35.0 | 20.0 | 60.0 | 45.05 (±2.68) | 20.56 (±3.21) |
7 | 0.0 | 10.0 | 45.0 | 41.03 (±0.47) | 26.49 (±3.60) |
8 | 35.0 | 30.0 | 60.0 | 42.32 (±1.29) | 28.61 (±1.13) |
9 | 0.0 | 30.0 | 60.0 | 40.43 (±2.07) | 29.90 (±0.81) |
10 | 70.0 | 20.0 | 45.0 | 20.56 (±4.12) | 16.13 (±1.99) |
11 | 70.0 | 30.0 | 45.0 | 27.85 (±1.75) | 22.34 (±0.82) |
12 | 70.0 | 30.0 | 60.0 | 42.88 (±4.28) | 22.21 (±2.77) |
13 | 35.0 | 20.0 | 45.0 | 47.47 (±4.17) | 25.42 (±1.71) |
14 | 35.0 | 10.0 | 60.0 | 44.06 (±2.79) | 24.19 (±1.62) |
15 | 0.0 | 20.0 | 45.0 | 46.29 (±1.71) | 25.61 (±1.62) |
16 | 70.0 | 20.0 | 60.0 | 46.52 (±4.21) | 32.59 (±0.94) |
17 | 0.0 | 10.0 | 60.0 | 44.89 (±1.15) | 30.81 (±2.50) |
18 | 70.0 | 20.0 | 30.0 | 45.76 (±0.54) | 30.93 (±0.55) |
19 | 70.0 | 10.0 | 30.0 | 36.30 (±1.10) | 22.26 (±1.25) |
20 | 35.0 | 20.0 | 30.0 | 40.05 (±0.59) | 24.63 (±2.77) |
21 | 70.0 | 10.0 | 45.0 | 46.33 (±1.46) | 25.93 (±0.74) |
22 | 0.0 | 20.0 | 60.0 | 39.93 (±2.44) | 23.52 (±4.10) |
23 | 35.0 | 30.0 | 45.0 | 43.53 (±0.95) | 25.33 (±0.44) |
24 | 35.0 | 10.0 | 45.0 | 43.15 (±2.40) | 22.57 (±2.26) |
25 | 0.0 | 30.0 | 45.0 | 50.99 (±1.59) | 33.78 (±1.80) |
26 | 35.0 | 30.0 | 30.0 | 53.83 (±2.36) | 33.00 (±0.60) |
27 | 70.0 | 10.0 | 60.0 | 50.08 (±2.11) | 32.09 (±2.73) |
Source | Sum of Squares | Degrees Freedom | Mean Square | Error | F-Value | p-Value |
---|---|---|---|---|---|---|
x1: Concentration | 882.013 | 1 | 882.013 | 0.92113 | 77.00 | 0.0000 |
x2: time | 590.346 | 1 | 590.346 | 0.92113 | 51.54 | 0.0000 |
x3: temperature | 2374.35 | 1 | 2374.35 | 0.92113 | 207.28 | 0.0000 |
x2x3 | 844.309 | 1 | 844.309 | 1.12815 | 73.71 | 0.0000 |
x32 | 247.87 | 1 | 247.870 | 1.59545 | 21.64 | 0.0014 |
Lack of fit | 1070.07 | 21 | 50.956 | 4.45 | 0.0000 | |
Pure error | 618.548 | 54 | 11.455 | |||
Total | 6627.51 | 80 |
Source | Sum of Squares | Degrees Freedom | Mean Square | Error | F-Value | p-Value |
---|---|---|---|---|---|---|
x1: Concentration | 418.964 | 1 | 418.964 | 0.52780 | 111.40 | 0.0000 |
x2: time | 60.3885 | 1 | 60.3885 | 0.52780 | 16.06 | 0.0002 |
x3: temperature | 1484.14 | 1 | 1484.14 | 0.52780 | 394.64 | 0.0000 |
x2x3 | 73.4735 | 1 | 73.4735 | 0.64642 | 19.54 | 0.0000 |
x32 | 158.717 | 1 | 158.717 | 0.91418 | 42.20 | 0.0026 |
Lack of fit | 204.384 | 21 | 9.73256 | 2.59 | ||
Pure error | 203.081 | 54 | 3.76077 | |||
Total | 2603.14 | 80 |
Optimal Conditions | Results | |||
---|---|---|---|---|
a [Et] (% v/v) | b time (min) | c T (°C) | d TPC (mg GAE/100 g) | e DPPH (mg Trolox/100 g) |
Experimental values | ||||
70 | 10 | 60 | 51.33 (±2.54) * | 32.35 (±1.47) * |
Predicted values | ||||
70 | 10 | 60 | 51.78 | 34.07 |
Phenolic Compounds | tR (min) | Concentration (mg kg−1) |
---|---|---|
p-Coumaric acid | 3.6 | 0.70 (±0.01) |
Ferulic acid | 3.7 | 1.85 (±0.21) |
Quercetin | 4.5 | 0.55 (±0.21) |
Cyanidin | 3.8 | 6.00 (±0.56) |
Kaempferol | 4.9 | 0.30 (±0.14) |
Quercetin-3-glucoside | 3.6 | 4.40 (±0.28) |
Kaempferol-3-glucoside | 3.5 | 1.20 (±0.14) |
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Medina-Jaramillo, C.; Gomez-Delgado, E.; López-Córdoba, A. Improvement of the Ultrasound-Assisted Extraction of Polyphenols from Welsh Onion (Allium fistulosum) Leaves Using Response Surface Methodology. Foods 2022, 11, 2425. https://doi.org/10.3390/foods11162425
Medina-Jaramillo C, Gomez-Delgado E, López-Córdoba A. Improvement of the Ultrasound-Assisted Extraction of Polyphenols from Welsh Onion (Allium fistulosum) Leaves Using Response Surface Methodology. Foods. 2022; 11(16):2425. https://doi.org/10.3390/foods11162425
Chicago/Turabian StyleMedina-Jaramillo, Carolina, Edward Gomez-Delgado, and Alex López-Córdoba. 2022. "Improvement of the Ultrasound-Assisted Extraction of Polyphenols from Welsh Onion (Allium fistulosum) Leaves Using Response Surface Methodology" Foods 11, no. 16: 2425. https://doi.org/10.3390/foods11162425