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To establish and validate a high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method for simultaneously determining the serum concentration of lamotrigine(LTG), levetiracetam(LEV), oxcarbazepine(OXC) and monohydroxycarbazepine(MHD), which is applied for clinical blood concentration detection.
A simple one-step precipitation method was used for the serum sample pretreatment, and stable isotopes of two antiepileptic drugs (OXC-D4, LEV-D6) as the internal standard. The mobile phases were aqueous solution of 0.1% formic acid and 5 mM ammonium acetate(A) and methyl alcohol(B), and the gradient elution was performed at the speed of 0.6 mL·min-1 for 6 min on Phenomenex C18(100.0 mm×4.6 mm, 3.0 μm). The column temperature was 40 ℃. Positive ion scan analysis was carried out in multi-reaction monitoring mode, using electrospray ion source. The specificity, standard curve and lower limit of quantification (LLOQ), accuracy and precision, extraction recovery, matrix effect and stability were evaluated. The patients treated with LRG, LEV or OXC in hospital were included as the research object. Blood samples were collected after the blood concentration reached a steady state and the serum concentration was detected by the method developed in this study.
The method demonstrated good specificity. For LTG, LEV, OXC and MHD, outstanding linearity was observed in the ranges of (0.20-25.00), (0.39-50.00), (0.04-5.00), (0.31-40.00) μg·mL-1, respectively. The linear equation of LTG was y=0.99x+0.02 (r=0.999 2), LEV was y=0.55x+0.01 (r=0.999 4), OXC was y=4.35x+0.04 (r=0.998 9), and MHD was y=0.56x+0.01 (r=0.998 7). The LLOQs were 0.20, 0.39, 0.04, 0.31 μg·mL-1, respectively. Acceptable accuracy as well as intra-batch and inter-batch precision were achieved; relative error (RE) and relative standard deviation (RSD) were all <15.00%. The extraction recoveries reached the standard (88.56%~112.18%, RSD<15.00%), without significant matrix effects and carryover effects. The serum samples of LTG, LEV, OXC, and MHD exhibited stability under the following conditions: storage at -20 ℃ for 14 days, three freeze-thaw cycles (-20 ℃ to room temperature), room temperature exposure for 3 hours, and post-treatment storage in the autosampler (4 ℃) for 24 hours, with all RSDs ≤10.72%. The analysis of 145 clinical samples showed that the linear range could meet the clinical needs.
This study successfully established a HPLC-MS/MS method to simultaneously quantify the serum concentration of LTG, LEV, OXC and MHD. The method is simple, economical accurate and efficient, which has promotional value.
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| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |
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