Assessment of the Presence of Pharmaceutical Compounds in Seawater Samples from Coastal Area of Gran Canaria Island (Spain)
Abstract
:1. Introduction
2. Experimental
2.1. Chemicals and Reagents
Compound | Use | Structure | pKa [17,18] | Kow * |
---|---|---|---|---|
Atenolol | Antihypertensive | 9.2 | 0.16 | |
Acetaminophen | Analgesic | 9.9 | 0.46 | |
Norfloxacin | Antibiotic | 6.4 | 0.46 | |
Ciprofloxacin | Antibiotic | 6.4 | 0.28 | |
Carbamazepine | Antiepileptic | 13.9 | 2.45 | |
Ketoprofen | Anti-inflammatory | 4.4 | 4.23 | |
Diclofenac | Anti-inflammatory | 4.2 | 4.51 |
2.2. Sample Collection
2.3. Chromatographic Conditions
Compound | Precursor ion (m/z) | Cone voltage (V) | Fragment ions (collision potential) | Ion mode |
---|---|---|---|---|
Atenolol | 267.0 | 52 | 145 (23.5) *, 190 (16.5) | ESI + |
Acetaminophen | 152.0 | 56 | 109.9 (13), 92.8 (20) | ESI + |
Norfloxacin | 320.1 | 56 | 301.9 (19), 230.8 (37) | ESI + |
Ciprofloxacin | 332.1 | 52 | 313.9 (19), 230.8 (36) | ESI + |
Carbamazepine | 237.1 | 40 | 194 (13.5), 179.2 (29.5) | ESI + |
Ketoprofen | 255.1 | 52 | 209 (10), 104.9 (18.5) | ESI + |
Diclofenac | 295.9 | 32 | 214.0 (30), 250.0 (11) | ESI − |
2.4. Solid-Phase Extraction
3. Results and Discussion
3.1. Optimisation of Solid-Phase Extraction
3.2. Analytical Parameters
LOD a (ng·L−1) | LOQ b (ng·L−1) | RSD (%) | Recovery (%) | LDR c (µg·L−1) | r2 | |
---|---|---|---|---|---|---|
Atenolol | 0.1 | 0.3 | 6.5 | 78.3 | 0.5–600 | 0.9986 |
Acetaminophen | 0.6 | 2.0 | 6.4 | 95.7 | 0.5–600 | 0.9906 |
Norfloxacin | 2.8 | 9.3 | 11.8 | 80.2 | 0.5–600 | 0.9964 |
Ciprofloxacin | 1.0 | 3.4 | 10.7 | 81.4 | 0.5–600 | 0.9935 |
Carbamazepine | 0.9 | 2.9 | 6.0 | 96.0 | 0.5–600 | 0.9926 |
Ketoprofen | 0.1 | 0.3 | 1.7 | 94.8 | 0.5–600 | 0.9962 |
Diclofenac | 1.4 | 4.6 | 9.8 | 98.2 | 0.5–600 | 0.9936 |
3.3. Evaluation of Pharmaceutical Compounds in Seawater
Outfall | Date | Acetaminophen | Norfloxacin | Ciprofloxacin | Ketoprofen | Diclofenac |
---|---|---|---|---|---|---|
Las Palmas de Gran Canaria | Jan-2011 | nd b | nd | nd | nd | nd |
Feb-2011 | nd | 3551.7 ± 315.0 | 303.6 ± 8.6 | 67.8 ± 5.3 | nd | |
Mar-2011 | 297.0 ± 26.8 | 1653.0 ± 141.2 | 123.3 ± 5.4 | nd | nd | |
Apr-2011 | nd | 77.9 ± 0.5 | nd | nd | nd | |
May-2011 | nd | nd | nd | nd | nd | |
Jun-2011 | nd | 1248.8 ± 62.3 | 95.3 ± 0.4 | nd | nd | |
Jul-2011 | nd | nd | 40.1 ± 4.9 | nd | nd | |
Aug-2011 | nd | 325.5 ± 44.9 | 18.9 ± 0.2 | nd | nd | |
Sep-2011 | nd | nd | 29.64 ± 3.1 | nd | 47.9 ± 3.5 | |
Oct-2011 | nd | 1380.74 ± 197.2 | 65.9 ± 9.2 | nd | 28.4 ± 4.0 | |
Nov-2011 | 29.7 ± 1.4 | 69.4 ± 10.3 | 60.4 ± 7.9 | nd | nd | |
Dic-2011 | nd | nd | nd | 41.6 ± 5.0 | nd | |
Jan-2012 | 21.5 ± 2.0 | 11.3 ± 0.7 | nd | 49.0 ± 3.8 | nd | |
Jinámar | Jan-2011 | nd | nd | 17.4 ± 1.6 | nd | nd |
Feb-2011 | nd | 3179.1 ± 106.2 | 303.4 ± 12.0 | 106.3 ± 6.4 | nd | |
Mar-2011 | nd | 1130.1 ± 106.6 | 140.7 ± 21.1 | nd | nd | |
Apr-2011 | nd | 92.1 ± 6.0 | nd | nd | nd | |
May-2011 | nd | nd | nd | nd | nd | |
Jun-2011 | nd | 808.6 ± 71.9 | 66.7 ± 2.0 | nd | nd | |
Jul-2011 | nd | 191.6 ± 7.1 | 70.2 ± 7.9 | nd | nd | |
Aug-2011 | nd | nd | 9.0 ± 0.2 | nd | nd | |
Sep-2011 | nd | 591.3 ± 15.8 | 52.3 ± 0.2 | nd | nd | |
Oct-2011 | nd | 1565.9 ± 210.0 | 121.6 ± 15.8 | nd | 28.4 ± 2.9 | |
Nov-2011 | nd | 2250 ± 112.5 | 119.9 ± 14.9 | nd | nd | |
Dic-2011 | nd | nd | nd | nd | nd | |
Jan-2012 | nd | 18.0 ± 1.0 | 17.7 ± 1.4 | nd | nd | |
Punta Salina | Jan-2011 | nd | nd | nd | nd | nd |
Feb-2011 | - | - | - | - | - | |
Mar-2011 | nd | nd | nd | nd | nd | |
Apr-2011 | - | - | - | - | - | |
May-2011 | nd | nd | nd | nd | nd | |
Jun-2011 | nd | nd | nd | nd | nd | |
Jul-2011 | nd | 185.3 ± 22.8 | 18.8 ± 2.6 | nd | nd | |
Aug-2011 | nd | nd | nd | nd | 56.7 ± 5.3 | |
Sep-2011 | nd | 634.5 ± 52.0 | 64.9 ± 10.3 | nd | 343.6 ± 51.1 | |
Oct-2011 | nd | 1681.5 ± 244.0 | 101.0 ± 5.7 | nd | 29.5 ± 1.4 | |
Nov-2011 | nd | 33.3 ± 2.4 | 30.8 ± 3.9 | nd | nd | |
Dic-2011 | nd | nd | nd | nd | nd | |
Jan-2012 | nd | 22.9 ± 2.1 | 26.3 ± 3.8 | nd | nd | |
Los Cochinos | Jan-2011 | nd | nd | nd | nd | nd |
Feb-2011 | - | - | - | - | - | |
Mar-2011 | nd | nd | nd | nd | nd | |
Apr-2011 | - | - | - | - | - | |
May-2011 | nd | nd | nd | nd | nd | |
Jun-2011 | nd | nd | nd | nd | nd | |
Jul-2011 | nd | 134.3 ± 15.1 | 80.1 ± 12.2 | nd | nd | |
Aug-2011 | nd | nd | nd | nd | 57.1 ± 0.8 | |
Sep-2011 | nd | 899.9 ± 130.8 | 72.0 ± 8.8 | nd | 160.0 ± 24.4 | |
Oct-2011 | nd | nd | 4.4 ± 0.5 | nd | 23.7 ± 0.4 | |
Nov-2011 | nd | 20.8 ± 3.2 | 15.8 ± 1.4 | nd | nd | |
Dic-2011 | nd | 17.4 ± 1.9 | 12.5 ± 0.2 | nd | nd | |
Jan-2012 | nd | 17.0 ± 1.3 | 13.5 ± 0.1 | nd | nd |
4. Conclusions
Acknowledgments
Conflict of Interest
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Afonso-Olivares, C.; Torres-Padrón, M.E.; Sosa-Ferrera, Z.; Santana-Rodríguez, J.J. Assessment of the Presence of Pharmaceutical Compounds in Seawater Samples from Coastal Area of Gran Canaria Island (Spain). Antibiotics 2013, 2, 274-287. https://doi.org/10.3390/antibiotics2020274
Afonso-Olivares C, Torres-Padrón ME, Sosa-Ferrera Z, Santana-Rodríguez JJ. Assessment of the Presence of Pharmaceutical Compounds in Seawater Samples from Coastal Area of Gran Canaria Island (Spain). Antibiotics. 2013; 2(2):274-287. https://doi.org/10.3390/antibiotics2020274
Chicago/Turabian StyleAfonso-Olivares, Cristina, Mª Esther Torres-Padrón, Zoraida Sosa-Ferrera, and José Juan Santana-Rodríguez. 2013. "Assessment of the Presence of Pharmaceutical Compounds in Seawater Samples from Coastal Area of Gran Canaria Island (Spain)" Antibiotics 2, no. 2: 274-287. https://doi.org/10.3390/antibiotics2020274