Reduced Graphene Oxide Aerogels Cartridges for Solid Phase Extraction of Benzotriazoles
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Synthesis and Characterization of the rGO Aerogels
2.3. Solid Phase Extraction Tests
2.4. Chromatographic Conditions
3. Results and Discussion
3.1. Properties of the rGO Aerogels
3.2. rGO Aerogels in Solid Phase Extraction
3.2.1. Recovery Test: Elution Solvent and rGO Aerogel Performance
3.2.2. Optimization of the SPE Method: Elution Time and Elution Volume
3.3. Applicability of the SPE Method
3.4. SPE-HPLC Tests with Real (River) Waters
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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Material | SBET (m2 g−1) | Vtotal (mL g−1) | Vmicro a (mL g−1) |
---|---|---|---|
GS | 203 | 0.89 | 0.08 |
GA-40% | 247 | 0.41 | 0.09 |
GA-60% | 164 | 0.49 | 0.06 |
G-GA-40% | 51 | 0.26 | 0.01 |
Material | Concentration (ng mL−1) | EFtheo | UV329 | UV234 | ||
---|---|---|---|---|---|---|
Recovery (%) | SD a (%) | Recovery (%) | SD a (%) | |||
GS | 1 | 50 | 83.6 | 10.4 | 76.7 | 5.0 |
100 | 12.5 | 91.0 | 7.8 | 79.7 | 6.8 | |
GA-60% | 1 | 50 | 70.4 | 8.7 | 84.9 | 2.7 |
5 | 12.5 | 56.6 | 5.4 | 88.1 | 4.4 | |
100 | 12.5 | 61.7 | 9.1 | 87.6 | 5.8 | |
G-GA-40% | 1 | 50 | 78.2 | 9.9 | 82.6 | 7.2 |
5 | 12.5 | 93.2 | 5.8 | 96.1 | 9.2 | |
50 | 12.5 | 80.1 | 8.1 | 83.9 | 3.2 | |
100 | 12.5 | 97.1 | 4.5 | 88.6 | 4.2 |
Material | UVP | UV329 | UV234 | |||
---|---|---|---|---|---|---|
Recovery (%) | SD a (%) | Recovery (%) | SD a (%) | Recovery (%) | SD a (%) | |
GA-60% | N.D. b | - | 9.7 | 3.2 | 5.2 | 3.9 |
G-GA-40% | N.D. b | - | N.D. b | - | 4.7 | 2.1 |
Sample | Analyte | Range (ng mL−1) | Equation | R2 | LOD a (ng mL−1) | LOQ b (ng mL−1) |
---|---|---|---|---|---|---|
GA-60% | UV329 | 3–250 | y = 0.215x + 2.329 | 0.9960 | 1.43 | 4.76 |
UV234 | 3–250 | y = 0.317x + 0.072 | 0.9948 | 1.16 | 3.88 | |
G-GA-40% | UV329 | 3–250 | y = 0.391x + 0.118 | 0.9981 | 0.95 | 3.17 |
UV234 | 3–250 | y = 0.340x + 0.338 | 0.9998 | 0.95 | 3.18 |
Method | Extractant | Performance Parameters | Ref. | |||
---|---|---|---|---|---|---|
Material | Time of Synthesis (Days) | Extraction Time (min) | Recovery (%) | EFtheo | ||
SPE-HPLC-UV | GS | 4.1 | 15 | 89–105 | 6.25 | [21] |
SBSE-HPLC-DAD | GS/Ni coated | >7 | 60 | 84–112 | 67 | [23] |
SPE-HPLC-UV | GAs | 3 | 10 | 75–97 | 12.5–50 | This work |
Material | Spiked (ng mL−1) | UV329 | UV234 | ||||
---|---|---|---|---|---|---|---|
Found (ng mL−1) | Recovery (SD a) (%) | ME b (SD a) (%) | Found (ng mL−1) | Recovery (SD a) (%) | ME b (SD a) (%) | ||
GA-60% | 0 | N.D. c | - | - | N.D. c | - | - |
25 | 20.05 | 80.0 (9.5) | 98.8 (7.1) | 21.89 | 87.6 (3.02) | 89.8 (1.95) | |
50 | 34.74 | 69.5 (8.4) | 97.8 (6.4) | 35.95 | 72.9 (2.26) | 80.8 (1.21) | |
100 | 68.55 | 68.6 (5.9) | 88.0 (5.2) | 84.61 | 84.6 (8.2) | 91.9 (8.8) | |
G-GA-40% | 0 | N.D. c | - | - | N.D. c | - | - |
25 | 20.88 | 83.5 (1.5) | 81.4 (1.5) | 21.47 | 85.9 (2.8) | 93.7 (2.6) | |
50 | 46.93 | 93.9 (4.9) | 87.4 (4.1) | 51.36 | 102.7 (3.3) | 97.6 (3.2) | |
100 | 88.31 | 88.3 (4.9) | 90.6 (4.9) | 81.45 | 81. 5 (9.7) | 83.5 (7.5) |
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Flores-López, S.L.; Arenillas, A.; Mikšík, I.; Menéndez, J.A.; Montes-Morán, M.A. Reduced Graphene Oxide Aerogels Cartridges for Solid Phase Extraction of Benzotriazoles. Materials 2023, 16, 2519. https://doi.org/10.3390/ma16062519
Flores-López SL, Arenillas A, Mikšík I, Menéndez JA, Montes-Morán MA. Reduced Graphene Oxide Aerogels Cartridges for Solid Phase Extraction of Benzotriazoles. Materials. 2023; 16(6):2519. https://doi.org/10.3390/ma16062519
Chicago/Turabian StyleFlores-López, Samantha L., Ana Arenillas, Ivan Mikšík, J. Angel Menéndez, and Miguel A. Montes-Morán. 2023. "Reduced Graphene Oxide Aerogels Cartridges for Solid Phase Extraction of Benzotriazoles" Materials 16, no. 6: 2519. https://doi.org/10.3390/ma16062519