Vermeij T A C, Edelbroek P M
Epilepsy Institute of the Netherlands (SEIN), Heemstede, The Netherlands.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Sep 15;857(1):40-6. doi: 10.1016/j.jchromb.2007.06.023. Epub 2007 Jun 30.
A rapid, simple and robust method is presented for the simultaneous determination of seven antiepileptic drugs (AEDs), including primidone, phenobarbital, phenytoin, carbamazepine with its two major metabolites carbamazepine-10,11-epoxide and carbamazepine-10,11-(trans)-dihydrodiol and the new AEDs lamotrigine, hydroxycarbazepine (active metabolite of oxcarbazepine) and zonisamide in serum by high performance liquid chromatography (HPLC)-diode array detector (DAD). After solid-phase extraction, separation is achieved on an Alltima 3C18 analytical column using isocratic elution with a mixture of acetonitrile, methanol and phosphate buffer at 45 degrees C. The method is exhaustively validated, including experimental design in combination with statistical evaluation (ANOVA) to study the robustness of chromatography and sample preparation. Commonly co-administered antiepileptic drugs do not interfere with the method. Intra-day precision (RSD<1.9%), linearity, lower limit of quantitation (LOQ<0.065 mg/l) and robustness make the method suitable for daily therapeutic drug monitoring and pharmacokinetic studies.
本文介绍了一种快速、简单且稳健的方法,用于同时测定血清中的七种抗癫痫药物(AEDs),包括扑米酮、苯巴比妥、苯妥英、卡马西平及其两种主要代谢产物卡马西平-10,11-环氧化物和卡马西平-10,11-(反式)-二氢二醇,以及新型AEDs拉莫三嗪、羟卡马西平(奥卡西平的活性代谢产物)和唑尼沙胺,采用高效液相色谱(HPLC)-二极管阵列检测器(DAD)进行检测。经过固相萃取后,在Alltima 3C18分析柱上进行分离,使用乙腈、甲醇和磷酸盐缓冲液的混合物在45℃下等度洗脱。该方法经过全面验证,包括结合统计评估(方差分析)的实验设计,以研究色谱法和样品制备的稳健性。常用的联合使用的抗癫痫药物不会干扰该方法。日内精密度(RSD<1.9%)、线性、定量下限(LOQ<0.065 mg/l)和稳健性使该方法适用于日常治疗药物监测和药代动力学研究。