反相高效液相色谱-柱前衍生法测定人血清中丙戊酸浓度

Determination of valproate in serum by precolumn derivatization HPLC

目的 建立人血清中丙戊酸浓度测定方法 。方法 将血清酸化,用乙醚提取,以环己烷羧酸为内标,α-溴苯乙酮为衍生化试剂,采用高效液相色谱法测定。色谱柱：Eclipse Plus C_（18）柱（150 mm×4.6 mm,5μm）,流动相：甲醇-水（70：30）,检测波长：248 nm,流速：1.0 ml/min。结果 血清中丙戊酸浓度线性范围为8.65～173μg/ml,平均回收率〉99.27%,日内和日间RSD〈5%。结论 本法快速、简便、准确,适合于临床血药浓度监测。

Objective To establish a determination method for valprate in serum. Methods Serum sample was acidified by sulfuric acid and extracted with ethyl ether, cyclohexanecarboxylic acid was selected as an internal standard, α-bromoaceto phenone as derivative reagent. Determination was performed with HPLC with methanol water （70： 30） as the mobile phase. The nalytical column was Eclipse Plus C18（150 mm×4.6 mm,5μe） ,detected at 248 nm, the flow rate was 1.0 ml/min. Re- sults The linear rang of valproate was 8.65～ 173μg/ml. The mean relative recovery was bigger than 99.27 %. Both the rela tire standard deviation （RSD） of inter-day and intra-day was less than 5%. Conclusions The method is rapid,accurate,sensi- tive and suitable for clinical therapeutic drug monitoring.