A New Method for the Determination of Amisulpride in a Small Volume (200 μL) of Human Saliva Using LC-DAD Supported by SPE
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemicals and Solvents
2.2. LC-DAD Conditions
2.3. Preparation of Quality Control (QC) and Standard Samples
2.4. Collection of Saliva Samples
2.5. Extraction of Amisulpride from Saliva Samples
2.6. Validation
2.6.1. Linearity
2.6.2. Intra and Inter-Day Precision
2.6.3. Limit of Detection (LOD) and Lower Limit of Quantification (LLOQ)
2.6.4. Selectivity
2.6.5. Extraction and Absolute Recovery
2.6.6. Stability
2.7. Clinical Application
3. Results
3.1. Chromatographic Analysis
3.2. Solid Phase Extraction
3.3. Method Validation
3.3.1. Extraction and Absolute Recovery
3.3.2. Stability
3.4. Clinical Application
4. Discussion
5. Conclusions
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
References
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Procedure | Dilution Solvent | Washing Solvent | Elution Solvent |
---|---|---|---|
1. | methanol:water (1:1) | water | methanol |
2. | acetonitrile | ||
3. |
| methanol | |
4. | acetonitrile | ||
5. | 2% formic acid | 5% ammonium in methanol | |
6. | 5% ammonium in acetonitrile | ||
7. |
| 5% ammonium in methanol | |
8. | 5% ammonium in acetonitrile | ||
9. | 0.1 M K2HPO4 | methanol:water (10:90, v/v) | methanol |
Calibration Curve y = ax + b (n = 4) | |
---|---|
Range (ng/mL) | 5–5000 |
Determination coefficient (R2) | 0.9978 ± 0.0021 |
Slope a ± Δa | 0.0005 ± 0.00005 |
Intercept b ± Δb | −0.0147 ± 0.00700 |
LOD (ng/mL) | 3.0 |
LLOQ (ng/mL) | 5.0 |
QC (ng/mL) | Intra-Day (CV%) | Inter-Day (CV%) | Extraction Recovery (%) | Absolute Recovery (%) | Stability (Difference %) | |
---|---|---|---|---|---|---|
8 °C | −21 °C | |||||
25 | 4.79 | 8.84 | 101.22 | 61.03 | −2.50 | −0.50 |
400 | 4.41 | 4.72 | 91.81 | 83.10 | −2.81 | −1.24 |
2500 | 5.05 | 7.44 | 92.82 | 80.69 | −2.63 | −1.65 |
4000 | 1.79 | 4.95 | 96.02 | 79.91 | −3.89 | −2.49 |
Patient | Age | Dose (mg/Day) | Amisulpride (ng/mL) |
---|---|---|---|
1 | 58 | 400 | 2852.9 |
2 | 62 | 400 | 4713.1 |
3 | 56 | 400 | 4707.6 |
4 | 40 | 200 | 216.3 |
5 | 38 | 200 | 543.3 |
6 | 43 | 200 | 104.8 |
Biological Matrices | Volume of the Sample (µL) | Isolation | Separation and Detection | LOQ (ng/mL) | Linearity (ng/mL) | R2 | Concentration (ng/mL) | References |
---|---|---|---|---|---|---|---|---|
Plasma | 1000 | LLE | HPLC-UV | 20 | 100–1000 | 0.985 | 107–14,824 | [8] |
1000 | SPE | HPLC-FL | 2 | 2–800 | >0.99 | 424.4 ± 292.8 | [10] | |
50 | LLE | LC-MS/MS | 0.5 | 0.5–500.52 | =0.9999 | 522.58 | [11] | |
100 | LLE | LC-MS/MS | 0.1 | 0.1–100 | >0.99 | - | [12] | |
100 | LLE | HPLC-MS/MS | 2 | 2–2500 | >0.99 | 947.9 1093.4 | [14] | |
1500 | SPE | LC-FL | 10 | 10–1000 | =0.9979 | 501 ± 216 515 ± 208 | [15] | |
20 | deproteinisation | UPLC-MS/MS | 20 | 20–2000 | >0.9977 | 21.9–773.7 | [18] | |
Plasma/breast milk | plasma 25 milk 15 | deproteinisation | LC-MS/MS | breast milk 0.6 plasma 0.5 | breast milk 0.6 to 75 plasma 0.5–360 | >0.999 | maternal plasma 95 breast milk 1131 baby’s plasma 10 | [17] |
Serum, plasma | 200 | LLE | LC-MS/MS | 0.5 | 1–400 | >0.98 | - | [13] |
100 | column-switching | HPLC-UV | 10 | 10–600 | >0.99 | - | [9] | |
Serum | 1000 | SPE | HPLC-UV | 10 | 10–1000 | >0.9995 | - | [20] |
Blood | 500 | SPE | HPLC-MS/MS | 5 | 5–500 | >0.99 | - | [7] |
Whole blood, oral fluid, serum | 200 | LLE | LC-MS/MS | 10 | 10–500 | >0.99 | - | [5] |
Plasma, oral fluid, whole blood | 500 | LLE | HPLC-MS/MS | - | - | - | plasma 193,241; oral fluid 190, 208; whole blood 243, 381 | [6] |
Plasma, serum, oral fluid | 200 | LLE | LC-MS/MS | 6 | 10–500 | >0.99 | plasma/serum 413–2348 | [16] |
Plasma, oral fluid | 500 | LLE | LC-MS/MS | 5 | 5–800 | >0.99 | plasma 40–1338 oral fluid 16–1827 | [19] |
Oral fluid | 500 | LLE | UPLC-MS/MS | 3.20 | 3.20–1920 | 0.995 | 1.04–68.66 | [21] |
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Dziurkowska, E.; Kosinska, S.; Plenis, A.; Wesolowski, M. A New Method for the Determination of Amisulpride in a Small Volume (200 μL) of Human Saliva Using LC-DAD Supported by SPE. Separations 2023, 10, 277. https://doi.org/10.3390/separations10050277
Dziurkowska E, Kosinska S, Plenis A, Wesolowski M. A New Method for the Determination of Amisulpride in a Small Volume (200 μL) of Human Saliva Using LC-DAD Supported by SPE. Separations. 2023; 10(5):277. https://doi.org/10.3390/separations10050277
Chicago/Turabian StyleDziurkowska, Ewelina, Sandra Kosinska, Alina Plenis, and Marek Wesolowski. 2023. "A New Method for the Determination of Amisulpride in a Small Volume (200 μL) of Human Saliva Using LC-DAD Supported by SPE" Separations 10, no. 5: 277. https://doi.org/10.3390/separations10050277