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目的:建立快速柱前衍生-高效液相色谱法测定人血清中丙戊酸钠(VPA)的浓度。方法:血样经酸化后用正戊烷提取,以环已烷羧酸为内标,w-溴苯乙酮为衍生化试剂,采用Agilent HC-C_(18)柱(250mm×4.6mm,5μm),流动相为甲醇-水(73:27),检测波长为262nm,流速1.0ml·min~(-1),柱温40℃。结果:血清中VPA浓度在10.12～182.16μg·ml~(-1)范围内具有良好的线性关系(r=0.9997),平均相对回收率为99.17%,日内、日间RSD均小于6%,最低定量浓度为10.12μg·ml~(-1)。结论:本法简便、快速、准确,适合临床常规血药浓度监测。
OBJECTIVE: To establish a rapid pre-column derivatization-high performance liquid chromatographic method for the determination of sodium valproate (VPA) in human serum. Methods: The blood sample was acidified and then extracted with n-pentane. Using cyclohexanecarboxylic acid as internal standard and w-bromoacetophenone as derivatization reagent, an Agilent HC-C 18 column (250 mm × 4.6 mm, 5 μm) The mobile phase was methanol-water (73:27). The detection wavelength was 262nm, the flow rate was 1.0ml · min -1 and the column temperature was 40 ℃. Results: The linear range of VPA in serum was 10.12 ~ 182.16 μg · ml ~ (-1) (r = 0.9997), the average relative recovery was 99.17%. The intra-day and inter-day RSD were all less than 6% Quantitative concentration of 10.12μg · ml ~ (-1). Conclusion: This method is simple, rapid and accurate, suitable for clinical routine blood concentration monitoring.