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目的建立测定人血浆中拉莫三嗪、奥卡西平及其代谢物10-羟基卡马西平浓度的高效液相色谱方法。方法以非那西汀为内标,血浆样品用乙醚萃取,用C18柱分析,流动相为乙腈-0.05 mol·L-1磷酸二氢钠水溶液(25∶75,p H 4.5),流速为1.0 m L·min-1,柱温为25℃,检测波长为220 nm。同时考察该方法的专属性、标准曲线和定量下限、精密度与回收率、稳定性。结果拉莫三嗪、10-羟基卡马西平、奥卡西平分别在0.1~20.0μg·m L-1(y=20.11×10-2c+1.31×10-2,r=0.999 0),0.5~50.0μg·m L-1(y=9.77×10-2c+0.35×10-2,r=0.999 8),0.25~25.0μg·m L-1(y=131.69×10-2c-0.59×10-2,r=0.999 1)线性关系良好。拉莫三嗪、10-羟基卡马西平、奥卡西平的方法回收率均在88.65%~100.38%,日内、日间精密度均<15%。结论该方法操作简便、准确、灵敏度高,可用于拉莫三嗪、奥卡西平及其代谢物10-羟基卡马西平血药浓度监测。
OBJECTIVE To establish a high performance liquid chromatographic method for the determination of 10-hydroxycarbamazepine in human plasma by lamotrigine, oxcarbazepine and its metabolites. Methods The phenacetin was used as the internal standard. The plasma samples were extracted with ether. The mobile phase consisted of acetonitrile-0.05 mol·L-1 aqueous sodium dihydrogen phosphate (25:75, p H 4.5) with a C18 column at a flow rate of 1.0 m L · min-1. The column temperature was 25 ℃ and the detection wavelength was 220 nm. At the same time examine the specificity of the method, the standard curve and lower limit of quantification, precision and recovery, stability. Results The values of lamotrigine, 10-hydroxycarbamazepine and oxcarbazepine were respectively in the range of 0.1-20.0 μg · m L-1 (y = 20.11 × 10-2c + 1.31 × 10-2, r = 0.999 0) 50.0 μg · m L -1 (y = 9.77 × 10 -2c + 0.35 × 10 -2, r = 0.999 8), 0.25-25.0 μg · m L -1 (y = 131.69 × 10 -2c -0.59 × 10- 2, r = 0.999 1) Linearity is good. The recoveries of lamotrigine, 10-hydroxycarbamazepine and oxcarbazepine all ranged from 88.65% to 100.38%. The intra- and inter-day precision were all <15%. Conclusion The method is simple, accurate and sensitive. It can be used to monitor the concentration of 10-hydroxy-carbamazepine in lamotrigine and oxcarbazepine and their metabolites.