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目的建立一种用反相高效液相色谱法同时测定人血清中苯巴比妥、苯妥英钠和卡马西平的浓度。方法以艾司唑仑为内标物,血样经氯仿-乙酸乙酯提取后,氮气吹干,用甲醇复溶10μL进样,以Agilent Eclipse XDB-C18柱(150 mm×4.6 mm,5μm)为分析柱,甲醇-水(51∶49)为流动相,检测波长238 nm,流速1.0 mL·min~(-1)。结果苯巴比妥、苯妥英钠、卡马西平线性范围分别为2~80 mg·L~(-1)(r=0.999 2)、1.006~40.24 mg·L~(-1)(r=0.999 9)和0.5~20 mg·L~(-1)(r=0.999 2);相对回收率分别为101.10%、102.16%和100.84%,提取回收率均≥95%;日内、日间RSD均<6%。结论本次建立的HPLC法具有操作简便、快速,结果准确等优点,适于临床快速检测血清中苯巴比妥、苯妥英钠和卡马西平浓度。
Objective To establish a method for the simultaneous determination of phenobarbital, phenytoin sodium and carbamazepine in human serum by reversed-phase high performance liquid chromatography. Methods Estazolam was used as an internal standard. The blood samples were extracted with chloroform - ethyl acetate and then dried under nitrogen. The samples were reconstituted with 10 μL of methanol and analyzed by Agilent Eclipse XDB - C18 column (150 mm × 4.6 mm, 5 μm) The analytical column and methanol-water (51:49) were used as the mobile phase. The detection wavelength was 238 nm and the flow rate was 1.0 mL · min -1. Results The linear ranges of phenobarbital, phenytoin and carbamazepine were 2 ~ 80 mg · L -1 (r = 0.999 2), 1.006 ~ 40.24 mg · L -1 (r = 0.999 9 ) And 0.5 ~ 20 mg · L -1 (r = 0.999 2). The relative recoveries were 101.10%, 102.16% and 100.84%, respectively. The average recoveries were both above 95% %. Conclusion The established HPLC method is simple, rapid and accurate. It is suitable for rapid detection of phenobarbital, phenytoin sodium and carbamazepine in serum.