Supramolecular Solvent-Based Microextraction of Selected Anticonvulsant and Nonsteroidal Anti-Inflammatory Drugs from Sediment Samples
Abstract
:1. Introduction
2. Results and Discussion
2.1. Development of Chromatographic Conditions
2.2. SUPRAS Microextraction
2.2.1. Composition of Supramolecular Solvent
2.2.2. Volume of the Supramolecular Solvent
2.2.3. Sample Weight
2.2.4. Extraction Time
2.2.5. Centrifugation Time and Speed
2.2.6. SUPRAS Microextraction Procedure
2.3. Speedisk Solid-Phase Extraction
2.4. Method Validation
2.4.1. Linearity and Sensitivity
2.4.2. Accuracy and Precision
2.5. Comparison of Proposed SUPRAS-UHPLC-UV and Speedisk-UHPLC-UV Methods with Other Reported Methods
2.6. Study of the Sorption Efficiency of Selected Drugs on Soil
3. Materials and Methods
3.1. Standards, Chemicals, and Materials
3.2. Preparation of Standard Solutions
3.3. UHPLC-UV Conditions
3.4. Preparation of Supramolecular Solvent and Determination of Its Volume
3.5. Preparation of Bottom Sediment Samples–SUPRAS Microextraction
3.6. Preparation of Water Samples–Speedisk Technique
3.7. Preparation of Blank Samples
3.8. Method Validation
3.9. Study of Sorption Efficiency of Selected Drugs on Sediment
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Conflicts of Interest
References
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Sample Availability: Samples of the compounds are available from the authors. |
Compound | Concentration (µg g−1)/(µg L−1) | Recovery (%) | RSD (%) |
---|---|---|---|
SUPRAS procedure | |||
CBZ | 1.25 | 115 | 7.2 |
10 | 96.3 | 4.1 | |
20 | 98.8 | 7.3 | |
DIC | 1.25 | 97.0 | 8.2 |
10 | 88.5 | 3.5 | |
20 | 90.8 | 1.6 | |
IBU | 1.25 | 112 | 2.8 |
10 | 103 | 0.3 | |
20 | 98.4 | 3.2 | |
Speedisk solid phase extraction procedure | |||
CBZ | 0.5 | 100 | 1.1 |
2 | 97.8 | 2.4 | |
4 | 97.3 | 0.6 | |
DIC | 0.5 | 103 | 2.6 |
2 | 106 | 2.0 | |
4 | 103 | 1.8 | |
IBU | 0.5 | 81.0 | 2.9 |
2 | 98.5 | 1.8 | |
4 | 102 | 5.6 |
Compound | Linear Range | Calibration Curve Equation | Sxy | Sa | Sb | R2 a | LOQ b | LOD c |
---|---|---|---|---|---|---|---|---|
Bottom sediment samples | ||||||||
CBZ | 0.5–25.0 µg g−1 | y = 0.4853x + 0.1092 | 0.4635 | 0.0204 | 0.2619 | 0.9912 | 1.25 µg g−1 | 0.42 µg g−1 |
DIC | y = 0.1196x + 0.0517 | 0.0605 | 0.0027 | 0.0342 | 0.9975 | |||
IBU | y = 0.0786x + 0.0849 | 0.0413 | 0.0018 | 0.0233 | 0.9973 | |||
Water samples | ||||||||
CBZ | 0.05–5.0 µg L−1 | y = 0.6159x − 0.0264 | 0.0191 | 0.0042 | 0.0118 | 0.9998 | 0.05 µg L−1 | 0.017 µg L−1 |
DIC | y = 0.1571x − 0.0004 | 0.0132 | 0.0029 | 0.0081 | 0.9983 | |||
IBU | y = 0.2503x + 0.0217 | 0.0317 | 0.0070 | 0.0196 | 0.9961 |
Method | Detection | Compound | LOD/LOQ | Linear Range | Recovery (%) | Volume of Extractant | Extraction/Analysis Time | Ref. |
---|---|---|---|---|---|---|---|---|
PLE/SPE-LC | MS/MS | ibuprofen diclofenac carbamazepine | LOD 3.0–30.0 ng g−1 | 0.05–10 µg g−1 | 35–135 | 1 mL | 11 min + SPE/45 min | [9] |
SLE/SPE-UPLC | MS/MS | ibuprofen diclofenac | - | – | 85–106.5 | 1 mL | 210 min + SPE/– | [10] |
PLE/SPE-HPLC | MS/MS | diclofenac carbamazepine | LOQ 0.2–2.0 ng g−1 | – | – | 1 mL | 15 min + SPE/– | [11] |
PLE-HPLC | MS | ibuprofen diclofenac carbamazepine | LOQ 14.0–29.0 ng g−1 | 10–100 µg L−1 | 68–112 | 40 mL | 40 min/25–30 min | [12] |
USE-SPE-HPLC | DAD | ibuprofen diclofenac carbamazepine | LOQ 1.1–187.0 ng g−1 | – | 85.8–102 | 150 µL | 35.5 min + SPE/– | [13] |
PLE-SPE-LC USE-SPE-LC | MS/MS | ibuprofen diclofenac carbamazepine | - | – | 40–130 | 1 mL | 15–35 min + SPE/– | [14] |
USE-SPE-LC | MS/MS | ibuprofen diclofenac carbamazepine | LOQ 20.0 ng g−1 | 10 ng g−1–20 µg g−1 | 44–81 | 200 µL | 10 min + SPE/28 min | [15] |
PLE-SPE-LC | MS/MS | ibuprofen dikolfenak carbamazepine | MQL 0.78–163.7 ng g−1 | 10 ng g−1–2 µg g−1 | 60–82 | 1 mL | 31 min + SPE/– | [16] |
SBSE-HF-LPME-LC | MS | ibuprofen diclofenac | - | 0.5–8 mg L−1 | 57–62 | 10 µL | 20–22 h/– | [17] |
PLE-HF-LPME-LC | MS | ibuprofen diclofenac | MLD 0.4–1.4 ng g−1 | 3.9–4000 ng mL−1 | 101–109 | 25 µL | 176 min/26 min | [18] |
SUPRAS-UHPLC | UV | ibuprofen diclofenac carbamazepine | LOD 0.42 µg g−1 | 0.5–25 µg g−1 | 88.5–115 | 700 µL | 30 min/7 min | this work |
Method | Detection | Compound | LOD/LOQ | Linear Range | Recovery (%) | Volume of Extractant | Extraction/Analysis Time | Ref. |
---|---|---|---|---|---|---|---|---|
SPE-GC | MS | ibuprofen diclofenac carbamazepine | LOD: 12–32 ng L−1 | 5–50 ng L−1 | 67–80 | 200 µL | SPE/62 min | [35] |
SPE-GC | MS | ibuprofen diclofenac carbamazepine | LOQ: 0.07–0.09 ng L−1 | – | 70–100 | 50 µL | SPE/38 min | [36] |
SPE-LC | MS | ibuprofen diclofenac carbamazepine | – | – | 46–97 | 2 mL | SPE/40 min | [37] |
SPE-LC | MS/MS | ibuprofen diclofenac | LOD: 20 ng L−1 | – | 62–117 | – | – | [38] |
SPE-GC | MS | ibuprofen diclofenac carbamazepine | LOQ: 2–8 ng L−1 | 0.1–10 ng µL−1 | 77–93 | 100 µL | SPE/32 min | [39] |
SPE-GC | MS | ibuprofen diclofenac | LOD: 36–38 ng L−1 | 10–2000 ng L−1 | 67–76 | 100 µL | SPE/50.5 min | [40] |
SPE-HPLC | MS/MS | ibuprofen diclofenac | LOD: 0.14–0.52 µg L−1 | 1–250 µg L−1 | 56–77 | 300 µL | SPE/20–43 min | [41] |
SPE-GC | MS | ibuprofen dikolfenak carbamazepine | LOQ: 5–10 ng L−1 | 10 ng g−1–2 µg g−1 | 50–99 | 0.5 mL | SPE/– | [42] |
SPE-GC | MS | ibuprofen diclofenac | ILD: 20–32 µg L−1 | 0.02–25 mg mL−1 | 84–157 | 130 µL | SPE/56 min | [43] |
SPE-GC | MS | ibuprofen diclofenac carbamazepine | LOD: 0.01–0.02 ng L−1 | 0.06–400 ng L−1 | 92–102 | 105 µL | SPE/– | [44] |
Speedisk-UHPLC | UV | ibuprofen diclofenac carbamazepine | LOD: 0.17 µg L−1 | 0.05–10 µg L−1 | 81–106 | 500 µL | 60 min/7 min | this work |
Time (min) | Solvent A (%) a | Solvent B (%) a | Flow Rate (mL min−1) |
---|---|---|---|
0.0 | 40 | 60 | 0.2 |
1.0 | 45 | 55 | 0.7 |
2.0 | 45 | 55 | 0.6 |
3.0 | 45 | 55 | 0.5 |
3.5 | 80 | 20 | 0.7 |
4.0 | 80 | 20 | 0.7 |
4.5 | 85 | 15 | 0.4 |
4.9 | 85 | 15 | 0.3 |
5.0 | 100 | 0 | 0.7 |
7.0 | 100 | 0 | 0.7 |
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Bajkacz, S.; Adamczewska, P.; Kokoszka, K.; Kycia-Słocka, E.; Sochacki, A.; Felis, E. Supramolecular Solvent-Based Microextraction of Selected Anticonvulsant and Nonsteroidal Anti-Inflammatory Drugs from Sediment Samples. Molecules 2020, 25, 5671. https://doi.org/10.3390/molecules25235671
Bajkacz S, Adamczewska P, Kokoszka K, Kycia-Słocka E, Sochacki A, Felis E. Supramolecular Solvent-Based Microextraction of Selected Anticonvulsant and Nonsteroidal Anti-Inflammatory Drugs from Sediment Samples. Molecules. 2020; 25(23):5671. https://doi.org/10.3390/molecules25235671
Chicago/Turabian StyleBajkacz, Sylwia, Paulina Adamczewska, Klaudia Kokoszka, Elżbieta Kycia-Słocka, Adam Sochacki, and Ewa Felis. 2020. "Supramolecular Solvent-Based Microextraction of Selected Anticonvulsant and Nonsteroidal Anti-Inflammatory Drugs from Sediment Samples" Molecules 25, no. 23: 5671. https://doi.org/10.3390/molecules25235671