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建立同时测定血清中卡马西平(CBZ)及10.11-环氧卡马西平(CBZE)血清浓度的反相高效液相色谱法;样本血清加入氯硝西泮(CZP)内标液,经乙腈直接沉淀蛋白,流动相为:乙腈:水=33:67,柱温30℃,经ZORBAX SB-C18(4.6×150mm,5μm),流速1.0ml.min-1,色谱柱洗脱、分离,于230nm紫外波长下检测;在一定浓度范围内(CBZ:0.4~80.0mg.L-1;CBZE:0.4~20.0mg.L-1)各CBZ及CBZE与内标峰高之比与浓度比呈良好的线性关系,回收率高于95%(95%~99%,n=5),日内和日间变异小于6%(2.37%~4.10%,2.81%~5.87%,n=5);本方法作简便、迅速,血清用量少。方法回收率高,重线性好,专属性好,可用于常规治疗药物监测,也可用于卡马西平及其代谢产物环氧卡马西平的药动学研究。
To establish a method for the simultaneous determination of carbamazepine (CBZ) and 10.11-CBZE in serum by reversed-phase high performance liquid chromatography (HPLC). Serum samples were added with CZP internal standard solution, The precipitated protein was eluted with acetonitrile: water = 33:67 and column temperature 30 ℃. The mobile phase was eluted with ZORBAX SB-C18 (4.6 × 150 mm, 5 μm) at a flow rate of 1.0 ml · min- Under UV wavelength, the ratio of CBZ and CBZE to the peak height of internal standard in a certain concentration range (CBZ: 0.4 ~ 80.0 mg.L-1; CBZE: 0.4 ~ 20.0 mg.L-1) (95% -99%, n = 5). The intra-and inter-day variability was less than 6% (2.37% -4.10%, 2.81% -5.87%, n = 5) Simple, rapid, less serum. The method has high recovery rate, good linearity and good specificity, and can be used for the monitoring of conventional therapeutic drugs. It can also be used for the pharmacokinetic study of carbamazepine and its metabolite epoxycarbamazepine.