Alves Gilberto, Figueiredo Isabel, Castel-Branco Margarida, Loureiro Ana, Falcão Amílcar, Caramona Margarida
Laboratory of Pharmacology, Faculty of Pharmacy, Coimbra University, 3000-141 Coimbra, Portugal.
Anal Chim Acta. 2007 Jul 16;596(1):132-40. doi: 10.1016/j.aca.2007.05.056. Epub 2007 Jun 3.
Herein is reported, for the first time, a simple and reliable chiral reversed-phase liquid chromatographic method coupled to ultraviolet (UV) detection for simultaneous determination of eslicarbazepine acetate (ESL) and its metabolites, S-licarbazepine (S-LC), R-licarbazepine (R-LC) and oxcarbazepine (OXC), in mouse plasma and brain, liver and kidney tissue homogenates. All analytes and the internal standard were extracted from plasma and tissue homogenates by a solid-phase extraction procedure using Waters Oasis hydrophilic-lipophilic balance cartridges. The chromatographic separation was performed by isocratic elution with water/methanol (88:12, v/v), pumped at a flow rate of 0.7 mL min(-1), on a LichroCART 250-4 ChiraDex (beta-cyclodextrin, 5 microm) column at 30 degrees C. The UV detector was set at 225 nm. Calibration curves were linear (r2 > or = 0.996) in the ranges 0.4-8 microg mL(-1), 0.1-1.5 microg mL(-1) and 0.1-2 microg mL(-1) for ESL and OXC and in the ranges 0.4-80 microg mL(-1), 0.1-15 microg mL(-1) and 0.1-20 microg mL(-1) for R-LC and S-LC in plasma, brain and liver/kidney homogenates, respectively. The overall precision not exceeded 11.6% (%CV) and the accuracy ranged from -3.79 to 3.84% (%bias), considering all analytes in all matrices. Hence, this method will be a useful tool to characterize the pharmacokinetic disposition of ESL in mice.
本文首次报道了一种简单可靠的手性反相液相色谱法,该方法结合紫外(UV)检测,可同时测定小鼠血浆、脑、肝和肾组织匀浆中的醋酸艾司卡巴喷丁(ESL)及其代谢物S-卡马西平(S-LC)、R-卡马西平(R-LC)和奥卡西平(OXC)。所有分析物和内标均通过使用沃特世Oasis亲水亲脂平衡柱的固相萃取程序从血浆和组织匀浆中提取。色谱分离采用水/甲醇(88:12,v/v)等度洗脱,流速为0.7 mL min⁻¹,在LichroCART 250 - 4 ChiraDex(β-环糊精,5 µm)柱上于30℃进行。紫外检测器设定在225 nm。血浆、脑和肝/肾匀浆中ESL和OXC的校准曲线在0.4 - 8 µg mL⁻¹、0.1 - 1.5 µg mL⁻¹和0.1 - 2 µg mL⁻¹范围内呈线性(r²≥0.996),R-LC和S-LC的校准曲线在血浆、脑和肝/肾匀浆中分别在0.4 - 80 µg mL⁻¹、0.