胶束电动毛细管色谱法快速分析人血浆中的抗癫痫药物

目的建立胶束电动毛细管色谱(MECC)法分析人血浆中的多种抗癫痫药物的方法。方法运行缓冲液为50 mmol·L^-1 SDS-8 mmol·L^-1 Na₂HPO₄-3 mmol·L^-1 Na₂B₄O₇ (pH 8.0)-乙腈(18%)。毛细管总长50 cm，有效长度45.5 cm，内径50 μm。操作电压25 kV，运行温度30 ℃。检测波长210 nm。考察了各种因素对MECC分离的影响。结果线性范围：扑米酮1.0～40.0 μg·mL^-1，苯巴比妥1.0～60.0 μg·mL^-1，苯妥英1.0～60.0 μg·mL^-1，卡马西平1.0～40.0 μg·mL^-1，氯硝西泮0.2～8.0 μg·mL^-1，线性良好，相关系数均大于0.999 1；精密度良好，日内、日间RSD均小于15.0%；提取回收率80.0%～100.0%，RSD均小于10.0%。结论胶束电动毛细管色谱法可同时检测人血浆内多种抗癫痫药物的含量，方法成本低、操作简便、快速准确、干扰因素少。

Rapid analysis of antiepileptic drugs in human plasma by micellar electrokinetic capillary chromatography

AIM: To develop a rapid and feasible method based on micellar electrokinetic capillary chromatography (MECC) for the simultaneous determination of antiepileptic drugs (AEDs)--phenytoin (PHT), phenobarbital (PB), carbamazepine (CBZ), primidone (PRM) and clonazepam (CZP) in human plasma. METHODS: Several factors that impact the separation of AEDs with MECC were investigated, such as concentration of sodium dodecyl sulfate (SDS), buffer compositions, pH, organic modifier, internal diameter and temperature, and an optimized MECC running condition was obtained the running buffer consisted of 8 mmol x L(-1) phosphate, 3 mmol x L(-1) sodium tetraborate, and 50 mmol x L(-1) sodium dodecylsulfate (SDS) (pH 8.0), containing acetonitrile (ACN) (18%) as organic modifier. Detection at 210 nm, run at 25 kV at 30 degrees C in a untreated fused silica capillary (50/45.5 cm length, 50 microm ID). RESULTS: The reproducibility of both migration time and relative peak area with MECC analysis were appropriate for the intra- and inter-assay coefficients. The evaluated drugs concentration intervals of PRM 1.0-40.0 microg x mL(-1), PB 1.0-60.0 microg x mL(-1), PHT 1.0-40.0 microg x mL(-1), CBZ 1.0-40.0 microg x mL(-1), CZP 0.2-8.0 microg x mL(-1) were linear with correlation coefficients higher than 0.999 1, and coefficients of the variation of the points of the calibration curve lower than 10%. The recoveries of AEDs varied from 80.0% to 100.0%, depending on the drug, with coefficients of the variation lower than 10.0%. CONCLUSION: The MECC technique is showed to be rapid, simple, efficient and low cost when applied to monitoring therapeutic drugs in patient treated with a combination of PHT and other AEDs such as hepatic enzyme-inducing agents.