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目的:建立快速监测癫痫患者血清中卡马西平血药浓度的柱切换-高效液相色谱法。方法:通过直接进样方式,利用自制限进填料作为预处理柱,除去血清中蛋白质等大分子杂质,卡马西平保留在预处理柱上;再通过柱切换技术,使卡马西平在分析柱上得到分析检测。通过条件优化,确定切换前预处理流动相为甲醇-水(5∶95),流速为1.2 mL·min-1;切换后分析流动相为甲醇-水(70∶30),流速为1.0 mL·min-1;切换时间为3 min;柱温:25℃;检测波长:240 nm。结果:卡马西平在0.05～20μg·mL-1范围内具有良好的线性关系(r=0.9994),3个浓度水平(2、8、12μg·mL-1)的平均回收率分别为100.5%、100.8%、99.3%,日内和日间精密度均小于5%。结论:本方法快速、简便、灵敏、准确,适用于癫痫患者日常临床血药浓度监测。
OBJECTIVE: To establish a rapid method for the determination of carbamazepine in serum of patients with epilepsy by high performance liquid chromatography (HPLC). Methods: By means of direct injection, homemade restricted fillers were used as pretreatment column to remove the macromolecular impurities such as protein in serum. Carbamazepine was retained on the pretreatment column. After the column was switched, carbamazepine was separated on the analytical column On the analysis and testing. The mobile phase was methanol-water (5:95) and the flow rate was 1.2 mL · min-1 after the preconditioning. The mobile phase was methanol-water (70:30) after switching and the flow rate was 1.0 mL · min-1; Switching time 3 min; Column temperature: 25 ℃; Detection wavelength: 240 nm. Results: Carbamazepine had a good linear relationship (r = 0.9994) in the range of 0.05 ~ 20μg · mL-1, the average recoveries of three concentrations (2,8,12μg · mL- 100.8%, 99.3%, the intra-day and inter-day precision are less than 5%. Conclusion: The method is rapid, simple, sensitive and accurate and suitable for the monitoring of daily clinical blood concentration in patients with epilepsy.