HPLC法测定人血清中卡马西平及环氧化卡马西平的浓度

目的建立测定人血清中卡马西平和环氧化卡马西平浓度的高效液相色谱法。方法色谱柱为Dia-mond C18(200 mm×4.6 mm,5μm);流动相为:甲醇-水(65∶35)(0 min)→甲醇-水(55∶45)(10 min)→甲醇-水(55∶45)(12 min)→甲醇-水(65∶35)(18 min),流速1.0 mL.min-1,柱温25℃;检测波长215 nm。以艾司唑仑为内标。结果卡马西平和环氧化卡马西平的线性范围分别为1.08~21.60μg.mL-1(r=0.9958)和0.20~5.00μg.mL-1(r=0.9952);高、中、低浓度卡马西平平均回收率为(98.5±5.1)%,(103.6±4.8)%,(100.0±4.9)%;高、中、低浓度环氧化卡马西平平均回收率为(95.8±3.6)%,(99.7±2.9)%,(93.0±5.7)%;日内及日间精密度均小于10%,最低检测浓度都为0.10μg.mL-1。结论本法简单、快速、准确,是一种有效的检测人血清中卡马西平和环氧化卡马西平的方法。

Determination of carbamazepine and carbamazepine-10,11-epoxide in human serum with HPLC

Objective To develop a method of HPLC to determine carbamazepine and carbamazepine-10,11-epoxide in human serum. Methods Samples were separated on Diamond C_(18)(200 mm×4.6 mm,5 μm). Different ratios of methanol-water were used as the gradient eluent, and flow rate was 1.0 mL·min~(-1).The column temperature was 25 ℃ and detection wavelength was 215 nm. Intern standard was estazolam. Results The calibration curves were linear in the ranges of 1.08～21.60 μg·mL~(-1)(r=0.9958)and 0.20～5.00 μg·mL~(-1)(r=0.9952) for carbamazepine and carbamazepine-10,11-epoxide respectively;the lowest limits of assay were both 0.10 μg·mL~(-1).The average recoveries at three concentrations of carbamazepine were (98.5±5.1)%,(103.6±4.8)%,(100.0±4.9)%, and those of carbamazepine-10,11-epoxide were (95.8±3.6%),(99.7±2.9)%,(93.0±5.7)% respectively;RSD of the intra-day and inter-day were less than 10%. Conclusion The method is rapid,sensitive and suitable for determination of carbamazepine and carbamazepine-10,11-epoxide in human serum.