Nikolaou Panagiota, Papoutsis Ioannis, Dona Artemisia, Spiliopoulou Chara, Athanaselis Sotiris
Department of Forensic Medicine and Toxicology, School of Medicine, National and Kapodistrian University of Athens, Greece.
Department of Forensic Medicine and Toxicology, School of Medicine, National and Kapodistrian University of Athens, Greece.
J Pharm Biomed Anal. 2015 Jan;102:25-32. doi: 10.1016/j.jpba.2014.08.034. Epub 2014 Sep 6.
A sensitive and accurate gas chromatography-mass spectrometric method was developed and validated for the simultaneous determination of levetiracetam and lamotrigine in whole blood. A solid-phase extraction (SPE) procedure using HF Bond Elut C18 columns followed by derivatization using N-methyl-N-tert-butyldimethylsilyl-trifluoroacetamide (MTBSTFA) with 1% tert-butyldimethylsilyl chloride (TBDMSCl) was used. In this assay, levetiracetam-d6 was used as internal standard. Limits of detection and quantification were 0.15 and 0.50 μg/mL, respectively, for both analytes. The method was proved to be linear within the concentration range of 0.50-50.0 μg/mL (R(2) ≥ 0.992) for both analytes. Absolute recovery was found to be at least 90.0 and 97.2% for levetiracetam and lamotrigine, respectively. Intra-day and inter-day accuracy values for both analytes were ranged from -6.5 to 4.2 and -6.6 to 3.0%, respectively, whereas their respective precision values were less than 11.4 and 8.3%. The developed method was successfully used in our laboratory for quantification of levetiracetam and lamotrigine blood concentrations during the investigation of forensic cases where these antiepileptic drugs were involved. This method could also be used for therapeutic drug monitoring purposes.
建立并验证了一种灵敏、准确的气相色谱-质谱法,用于同时测定全血中的左乙拉西坦和拉莫三嗪。采用HF Bond Elut C18柱进行固相萃取(SPE),随后使用含1%叔丁基二甲基氯硅烷(TBDMSCl)的N-甲基-N-叔丁基二甲基硅基三氟乙酰胺(MTBSTFA)进行衍生化。在该分析中,左乙拉西坦-d6用作内标。两种分析物的检测限和定量限分别为0.15和0.50μg/mL。该方法在两种分析物浓度范围为0.50 - 50.0μg/mL(R(2)≥0.992)内被证明呈线性。左乙拉西坦和拉莫三嗪的绝对回收率分别至少为90.0%和97.2%。两种分析物的日内和日间准确度值分别在-6.5%至4.2%和-6.6%至3.0%之间,而它们各自的精密度值分别小于11.4%和8.3%。所建立的方法在我们实验室已成功用于涉及这些抗癫痫药物的法医案件调查中左乙拉西坦和拉莫三嗪血药浓度的定量分析。该方法也可用于治疗药物监测目的。