Vera-Candioti Luciana, Culzoni María J, Olivieri Alejandro C, Goicoechea Héctor C
Laboratorio de Desarrollo Analítico y Quimiometría, Facultad de Bioquímica y Ciencias Biológicas, Universidad Nacional del Litoral, Ciudad Universitaria, Santa Fe, Argentina.
Electrophoresis. 2008 Nov;29(22):4527-37. doi: 10.1002/elps.200800400.
Drug monitoring in serum samples was performed using second-order data generated by CE-DAD, processed with a suitable chemometric strategy. Carbamazepine could be accurately quantitated in the presence of its main metabolite (carbamazepine epoxide), other therapeutic drugs (lamotrigine, phenobarbital, phenytoin, phenylephrine, ibuprofen, acetaminophen, theophylline, caffeine, acetyl salicylic acid), and additional serum endogenous components. The analytical strategy consisted of the following steps: (i) serum sample clean-up to remove matrix interferences, (ii) data pre-processing, in order to reduce the background and to correct for electrophoretic time shifts, and (iii) resolution of fully overlapped CE peaks (corresponding to carbamazepine, its metabolite, lamotrigine and unexpected serum components) by the well-known multivariate curve resolution-alternating least squares algorithm, which extracts quantitative information that can be uniquely ascribed to the analyte of interest. The analyte concentration in serum samples ranged from 2.00 to 8.00 mg/L. Mean recoveries were 102.6% (s=7.7) for binary samples, and 94.8% (s=13.5) for spiked serum samples, while CV (%)=4.0 was computed for five replicate, indicative of the acceptable accuracy and precision of the proposed method.
使用CE-DAD生成的二阶数据对血清样本进行药物监测，并采用合适的化学计量学策略进行处理。在卡马西平的主要代谢物（卡马西平环氧化物）、其他治疗药物（拉莫三嗪、苯巴比妥、苯妥英、去氧肾上腺素、布洛芬、对乙酰氨基酚、茶碱、咖啡因、乙酰水杨酸）以及其他血清内源性成分存在的情况下，仍可准确测定卡马西平。分析策略包括以下步骤：（i）血清样本净化以去除基质干扰；（ii）数据预处理，以降低背景并校正电泳时间偏移；（iii）通过著名的多元曲线分辨交替最小二乘法解析完全重叠的CE峰（对应卡马西平、其代谢物、拉莫三嗪和意外的血清成分），该算法提取可唯一归因于目标分析物的定量信息。血清样本中分析物浓度范围为2.00至8.00 mg/L。二元样本的平均回收率为102.6%（s = 7.7），加标血清样本的平均回收率为94.8%（s = 13.5），同时对五次重复计算得出CV（%）= 4.0，表明所提出方法的准确度和精密度均可接受。
