Department of Pharmaceutical Sciences, Laboratory of Pharmaco-Toxicological Analysis, Faculty of Pharmacy, University of Bologna, Via Belmeloro 6, I-40126 Bologna, Italy.
Anal Chim Acta. 2010 Feb 28;661(2):222-8. doi: 10.1016/j.aca.2009.12.030. Epub 2009 Dec 29.
A rapid and reliable analytical method suitable for the simultaneous determination of the antiepileptic drug, oxcarbazepine and its metabolites in human plasma and saliva by means of liquid chromatography with diode array detection (DAD) has been developed. Oxcarbazepine and its metabolites (10,11-dihydro-10-hydroxycarbamazepine, trans-10,11-dihydro-10,11-dihydroxycarbamazepine and 3-hydroxycarbamazepine) were baseline separated within 6.5 min on a reversed-phase C18 column with a phosphate buffer-acetonitrile-triethylamine mixture as the mobile phase. The DAD detector was set at 240 nm. A sample preparation method for biological samples using a microextraction by packed sorbent technique has been implemented, employing a C18 sorbent inserted into a microvolume syringe and using only a small volume (25 microL) of plasma or saliva. The extraction yield values were satisfactory for all analytes (>86.5%) as well as the precision data, which were always in the low percentage of relative standard deviation values (<4.6%). The method was successfully applied to both plasma and saliva samples drawn from psychiatric and neurological patients undergoing treatment with oxcarbazepine (Tolep) tablets.
已开发出一种快速可靠的分析方法，适用于通过二极管阵列检测（DAD）液相色谱法同时测定人血浆和唾液中的抗癫痫药物奥卡西平和其代谢物。在反相 C18 柱上，以磷酸盐缓冲液-乙腈-三乙胺混合物为流动相，可在 6.5 分钟内基线分离奥卡西平和其代谢物（10,11-二氢-10-羟基卡马西平、反式 10,11-二氢-10,11-二羟基卡马西平和 3-羟基卡马西平）。DAD 检测器设置在 240nm。采用微萃取填充固相萃取技术的生物样品前处理方法，在微体积注射器中插入 C18 固相，仅使用小体积（25μL）的血浆或唾液。所有分析物（>86.5%）的提取回收率值和精密度数据均令人满意，相对标准偏差值（<4.6%）始终处于低百分比。该方法成功应用于接受奥卡西平（Tolep）片治疗的精神科和神经科患者的血浆和唾液样本。
