Pharmacological treatment with antiepileptic drugs (AEDs) remains a primary selection for most patients with epilepsy, while therapeutic drug monitoring is an important strategy to ensure the efficacy and safety of AEDs. The aim of this study was to optimize and develop a green high-performance liquid chromatography (HPLC) method suitable for simultaneous detection of 8 AEDs and 2 active metabolites including primidone (PRM), lamotrigine (LTG), carbamazepine (CBZ) and its active metabolite 10,11-epoxide (CBZE), oxcarbazepine (OXC) and its active metabolite 10, 11-dihydro-10-hydroxyl carbamazepine (MHD), phenobarbital (PHB), eslicarbazepine acetate (ESLA), clonazepam (CZP) and diazepam (DZP) in human serum. The results showed that using chlorzoxazone as the internal standard, ethanol as protein precipitant of serum, ZORBAX Eclipse Plus-C18 (150 × 4.6 mm, 3.5 μm) column as stationary phase, and gradient ethanol and 15 mM potassium dihydrogen phosphate water solution as green alternative mobile phase, good chromatographic separation for 10 target analytes could be obtained. The calibration curves of 10 analytes demonstrated good linearity within the test range (r > 0.996). The intra- and inter-batch precision and accuracy were all less than 15%, while extraction recoveries were in the range of 74.57-90.89 % with the relative standard deviation values less than 15%. The results of greenness assessment showed that the proposed method was ecofriendly. Finally, the validated method was successfully applied in the determination of real serum samples.
Li Yang,Bolin Yu,Jie Yuan,Rongrong Xing,Runqin Wang,Xuan Chen,Shuang Hu
In this study, a novel technique utilizing vortex-assisted dispersive liquid-liquid microextraction with magnetic deep eutectic solvents (MDESs) was established and coupled with HPLC-UV to analyze six primary aromatic amines (PAAs). A novel hydrophobic MDES prepared from trioctylphosphine oxide , octanol , and CoCl 2 was used as the extractant, which could be dispersed uniformly during extraction, then floated onto the sample surface and re-aggregated into a single drop spontaneously after the extraction. The variables influencing the efficiency of the extraction process were investigated. When performing under the optimal extraction conditions, this method exhibited excellent linearity, low limits of detection (0.2–0.9 ng mL −1 ), and high precision (RSD ≤ 8.3 %). The enrichment factors ranged from 56 to 182. Satisfactory recoveries in the range of 91.6–109.2 % with RSDs < 7.1 % were obtained from three apple juices and three environmental water samples. The greenness and practicality of the developed method were assessed by AGREE, AGREEprep, and blue applicability grade index metric tools. Overall, the established procedure demonstrated its simplicity, speediness, environmental friendliness , and effectiveness in analyzing PAAs from aqueous matrices.
危险品化学品经营许可证（带存储）