HPTLC-PCA Complementary to HRMS-PCA in the Case Study of Arbutus unedo Antioxidant Phenolic Profiling
Abstract
:1. Introduction
2. Materials and Methods
2.1. Reagents and Chemicals
2.2. Sampling Sites and Extraction
2.3. HPTLC Analyses
2.4. LC–ESI–Orbitrap–MS Analysis
2.5. PCA
2.6. Antiradical Activity by Diphenyl-1-Picarylhydrazyl (DPPH) and TEAC Assays
2.7. Determination of Total Phenols
2.8. Statistical Analysis
3. Results and Discussion
3.1. HPTLC–PCA Analysis
3.2. LC–ESI–Orbitrap–MS Analysis and PCA
3.3. Antioxidant Activity
4. Conclusions
Author Contributions
Funding
Conflicts of Interest
References
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No. | RT | [M − H]− | Molecular Formula | Δ PPM | MS/MS | Identity | LMFG | LMFR | LML | SSFG | SSFR | SSL |
---|---|---|---|---|---|---|---|---|---|---|---|---|
1 | 1.08 | 271.0814 | C12H15O7 | 0.6 | 139.08 | arbutin | x | x | x | nd | x | x |
2 | 4.3 | 343.0658 | C14H15O10 | −0.6 | 283.8/191.1 | galloyl quinic acid | x | x | x | x | x | x |
3 | 5.4 | 289.0708 | C27H21O18 | −1.5 | 275.9/245.1/205.1/144.2 | catechin/epicatechin | x | x | x | x | x | x |
4 | 5.5 | 353.0857 | C16H17O9 | −2.8 | 262.8/191.01/171.7 | chlorogenic acid | nd | nd | x | nd | nd | x |
5 | 5.8 | 633.0712 | C27H21O18 | −1.5 | 463.06/300.9 | strictinin ellagitannin | nd | x | x | x | nd | x |
6 | 5.9 | 289.0706 | C27H21O18 | −1.5 | 275.9/245.1/205.1/144.2 | catechin/epicatechin | x | x | x | x | x | x |
7 | 7.6 | 633.0709 | C27H21O18 | −1.5 | 463.06/300.9 | strictinin ellagitannin | nd | x | x | x | nd | x |
8 | 8.0 | 477.0656 | C21H17O13 | 0.2 | 462.0/366.07/325.05/191.03/164.7 | digalloylquinic shikimic acid | x | x | x | x | nd | x |
9 | 10.9 | 479.0815 | C21H19O13 | −1.43 | 451.2/354.7/316.02/297.6/165.8/145.5 | myricetin glucoside | nd | nd | x | nd | nd | x |
10 | 13.0 | 449.0705 | C20H17O12 | −1.7 | 317.02/183.3/149.5 | myricetin pentoside | nd | x | x | nd | nd | x |
11 | 13.3 | 615.0967 | C28H23O16 | 1.8 | 463.08/301.03 | quercetin galloylhexoside isomer | x | x | x | x | x | x |
12 | 14.2 | 463.0862 | C21H19O12 | −1.5 | 316.02/284.8/183.5 | myricetin rhamnoside | nd | x | x | x | nd | x |
13 | 17.1 | 433.0758 | C20H17O11 | −1.12 | 355.3/312.7/301.03/283.8/216.2 | quercetin pentoside | x | x | x | x | x | x |
14 | 17.2 | 615.0960 | C28H23O16 | 1.02 | 463.08/301.03/265.3/241.08 | quercetin galloylhexoside isomer | x | x | x | x | x | x |
15 | 17.7 | 433.0758 | C20H17O11 | −1.1 | 301.03/265.8/247.7/219.2/181.9/134.9 | quercetin pentoside | x | x | x | x | x | x |
16 | 19.5 | 463.0860 | C21H19O12 | 0.8 | 404.3/316.02/301.04/282; 2 | isoquercitrin | nd | x | x | x | nd | x |
17 | 19.7 | 447,0913 | C21H19O11 | −1.2 | 301.03/287.9/178.9 | quercitrin | x | x | x | x | x | x |
18 | 22.4 | 417.0810 | C20H17O10 | −0.9 | 374.9/285.04/175.6 | kaempferol pentoside | nd | x | x | x | x | x |
19 | 24.7 | 431.0965 | C21H19O10 | −1.09 | 285.03/235.2/195.9 | Kaempferol-rhamnoside (afzelin) | x | x | x | nd | x | x |
DPPH IC50 | ABTS IC50 | |||||
---|---|---|---|---|---|---|
0 min | 30 min | p Value | 0 min | 50 min | p Value | |
Trolox (µg/mL) | 13.50 | 6.15 | 3.34 | 3.28 | ||
A. unedo Sassari Red fruits (µg/mL) | 229.09 ± 81.75 | 103.59 ± 45.97 | Time 0 min LSS vs. FR SS p < 0.05 LSS vs. FG SS p < 0.05 | 52.71 ± 16.13 | 21.43 ± 7.34 | Time 0 min LSS vs. FR SS p < 0.01 LSS vs. FG SS p < 0.05 |
A. unedo Sassari Yellow fruits (µg/mL) | 300.92 ± 107.31 | 131.53 ± 44.61 | 101.11 ± 53.44 | 40.33 ± 21.95 | ||
A. unedo Sassari leaves (µg/mL) | 29.37 ± 5.87 | 15.18 ± 4.11 | Time 30 min LSS vs. FR SS p < 0.05 LSS vs. FG SS p < 0.01 | 7.63 ± 1.38 | 2.35 ± 0.06 | Time 50 min LSS vs. FR SS p < 0.01 LSS vs. FG SS p < 0.05 |
A. unedo La Maddalena Red fruits (µg/mL) | 235.67 ± 43.72 | 116.84 ± 16.54 | Time 0 min L LM vs. FR LM p < 0.01 L LM vs. FG LM p < 0.01 | 79.36 ± 46.09 | 34.91 ± 23.07 | Time 0 min L LM vs. FG LM p < 0.05 |
A. unedo La Maddalena Yellow fruits (µg/mL) | 380.14 ± 90.72 | 180.30 ± 75.48 | 96.09 ± 40.98 | 49.89 ± 17.62 | ||
A. unedo La Maddalena leaves (µg/mL) | 23.35 ± 4.25 | 8.85 ± 7.79 | Time 30 min L LM vs. FR LM p < 0.01 L LM vs. FG LM p < 0.05 | 6.73 ± 2.14 | 2.72 ± 1.68 | Time 50 min L LM vs. FG LM p < 0.01 |
Extract Concent Ration (µg/mL) | GAE A. Unedo Sassari Red Fruits (µg GAE) | GAE A. Unedo Sassari Yellow Fruits (µg GAE) | GAE A. Unedo Sassari Leaves (µg GAE) | GAE A. Unedo La Maddalena Red Fruits (µg GAE) | GAE A. Unedo La Maddalena Yellow Fruits (µg GAE) | GAE A. Unedo La Maddalena Leaves(µg GAE) | Pearson Product Moment Correlation |
---|---|---|---|---|---|---|---|
100 | 67.10 ± 17.14 *† | 43.62 ± 11.85 *† | 347.56 ± 126.05 | 53.16 ± 35.75 *† | 50.62 ± 20.64 *† | 327.90 ± 126.75 | * vs. DPPH p < 0.01 † vs. ABTS p < 0.05 |
50 | 35.33 ± 9.37 *† | 22.72 ± 6.41 *† | 179.52 ± 70.68 | 26.42 ± 11.73 *† | 26.42 ± 8.04 *† | 181.55 ± 84.65 | |
25 | 23.67 ± 4.29 *† | 16.13 ± 9.12 *† | 116.46 ± 36.12 | 21.11 ± 11.83 *† | 18.10 ± 5.64 *† | 143.84 ± 67.03 | |
10 | 10.15 ± 3.27 *† | 6.78 ± 2.43 *† | 51.50 ± 15.93 | 9.53 ± 3.44 *† | 8.30 ± 2.42 *† | 64.56 ± 33.28 | |
5 | 6.63 ± 1.16 *† | 4.24 ± 0.55 *† | 29.01 ± 4.24 | 6.17 ± 3.36 *† | 5.04 ± 3.89 *† | 38.12 ± 17.86 | |
1 | 3.17 ± 1.66 *† | 2.40 ± 0.70 *† | 10.04 ± 1.54 | 4.91 ± 1.69 *† | 2.52 ± 1.17 *† | 18.54 ± 14.44 |
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Maldini, M.; D’Urso, G.; Pagliuca, G.; Petretto, G.L.; Foddai, M.; Gallo, F.R.; Multari, G.; Caruso, D.; Montoro, P.; Pintore, G. HPTLC-PCA Complementary to HRMS-PCA in the Case Study of Arbutus unedo Antioxidant Phenolic Profiling. Foods 2019, 8, 294. https://doi.org/10.3390/foods8080294
Maldini M, D’Urso G, Pagliuca G, Petretto GL, Foddai M, Gallo FR, Multari G, Caruso D, Montoro P, Pintore G. HPTLC-PCA Complementary to HRMS-PCA in the Case Study of Arbutus unedo Antioxidant Phenolic Profiling. Foods. 2019; 8(8):294. https://doi.org/10.3390/foods8080294
Chicago/Turabian StyleMaldini, Mariateresa, Gilda D’Urso, Giordana Pagliuca, Giacomo Luigi Petretto, Marzia Foddai, Francesca Romana Gallo, Giuseppina Multari, Donatella Caruso, Paola Montoro, and Giorgio Pintore. 2019. "HPTLC-PCA Complementary to HRMS-PCA in the Case Study of Arbutus unedo Antioxidant Phenolic Profiling" Foods 8, no. 8: 294. https://doi.org/10.3390/foods8080294