柱前衍生-HPLC法测定人血清中丙戊酸钠的方法改进

目的建立快速柱前衍生-HPLC法测定人血清中丙戊酸钠（VPA）。方法选择对溴苯甲酰甲基溴为衍生化试剂,壬酸为内标,HypersilBDSC18（4.6mm×200mm,5μm）为分析柱;流动相为乙腈-水（75∶25,V/V）;检测波长254nm;流速1.0ml/min;柱温40℃。结果 VPA的血清浓度在25.0～250.0mg/L范围内线性关系良好（r=0.9991）,平均回收率为（100.43±0.73）%,日内、日间RSD均〈5%;123例服用VPA的癫痫患者应用本法监测,有53.7%的患者血药浓度在有效浓度范围之内,46.3%的患者血药浓度低于或高于有效浓度。结论本法快速、简便、准确,适合临床常规监测VPA血清浓度需要。

Improvement of precolumn derivatization HPLC assay method in determination of sodium valproate in human serum

Objective To establish a rapid analysis method for the determination of sodium valproate in serum by HPLC after precolumn derivatization. Methods p-bromophenacyl bromide was selected as derivative reagent. Nonanoic acid was used as an internal standard. The analytical column was Hypersil BDS C18 （4- 6 mm × 200 mm ,5 μm）. The mobile phase consisted of acetonitrile-water（ 75：25, V/V）. The detection wavelength was 254 nm and the flow rate was 1.0 ml/min, column temperature was 40℃. Results The linear calibration curve was obtained in the concentration range of 25.0 - 250. 0 mg/L （ r = 0. 9991 ）. The mean relative recovery was （ 100. 43± 0. 73 ） %. The relative standard deviation （ RSD ） of within day and between day were all less than 5%. The method was used for monitoring serum sodium valpruate concen- tration of 123 epileptic patients, 53.7 % of the patients who had taken sodium valproate was found the serum concentration in effective level and 46. 3 % lower or higher than effective level. Conclusion This method is found to be rapid, accurate, sensitive and more suitable for the determination of the concentration of sodium valproate in serum.