Objective To establish a method for the determination of 10-hydroxyl carbamazepine (MHD),which is an activity metabolite of oxcarbazepine in human serum. Methods Serum samples were detected by high performance liquid chromatography (HPLC) after being processed by methanol protein deposition.The chromatographic column was Agilent TC-C18 (4.6 mm × 250 mm, 5 μm), with the mobile phase of acetonitrile-10 mmol ? L-1 KH2 PO4 ( 33 : 67) at a flow rate of 1.0 mL?min-1 .The detection wavelength was 230 nm,and phenacetin was used as an internal standard. Results The average recovery range of low,middle and high (1.0,10.0,60.0 μg?mL-1 ) concentrations for MHD was from 100.3％ to 106.0％.The RSD of intra-day and inter-day was ≤5.8％ (n= 5) and ≤7.4％ (n= 5),respectively.The limit detection of analysis method was 0.1 μg?mL-1 .Regression equation was Y = 0.1308X+ 0.0679 ( r = 0.9966,n = 5). Serum samples remained stable at room temperature,freezing and freeze thawing condition. Conclusion This method is sensitive,accurate,simple and quick,and can be used for monitoring the oxcarbazepine metabolites MHD in serum for clinical and pharmacokinetic study.%目的 建立测定人血清奥卡西平活性代谢产物10-羟基卡马西平浓度的方法.方法 血样采用甲醇沉淀蛋白处理后,采用高效液相色谱法测定10-羟基卡马西平浓度:以Agilent TC-C18(4.6 mm×250 mm,5μm)为色谱柱,流动相:乙腈-10 mmol?L-1磷酸二氢钾(33:67),流速:1 mL?min-1,检测波长:230 nm,非那西丁为内标物.结果 奥卡西平活性代谢物10-羟基卡马西平低、中、高(1.0,10.0,60.0μg?mL-1)3种浓度平均回收率范围为100.3％～106.0％,日内精密度RSD≤5.8％(n=5),日间精密度RSD≤7.4％(n=5),分析方法的最低检测限为0.1μg?mL-1.回归方程为:Y=0.1308X+0.0679(r=0.9966,n=5),10-羟基卡马西平在0.5～80μg?mL-1浓度范围内,线性关系良好.血样在室温、冷冻、冻融的情况下稳定.结论 该方法灵敏、准确、简单、快速,适用于奥卡西平活性代谢物10-羟基卡马西平临床血药浓度监测.
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