柱前衍生高效液相色谱法测定人血清中丙戊酸钠浓度

目的建立人血清丙戊酸钠浓度的测定方法.方法将血清酸化,用乙醚提取,α-溴苯乙酮衍生,环己烷羧酸为内标,采用高效液相色谱法测定丙戊酸钠的浓度.色谱柱:Shimadzu VP-ODS(150mm×4.6mm,5μm),流动相:甲醇-水(75∶25),检测波长为248nm.结果血清内丙戊酸钠浓度在11.24～180.96μg?mL-1范围内,丙戊酸衍生物和内标衍生物的峰面积比与浓度呈现良好线性关系,平均回收率为101.00%,日内和日间RSD均<3.77%.结论该方法快速、简便、准确,适合于临床丙戊酸钠的血浓度监测.

Determination of sodium valprate in serum of precolumn derivatization by HPLC

OBJECTIVE To establish an analysis method for the determination of sodium valprate in serum. METHODS To acidify serum and extract with ether. Determination was performed by HPLC,a-phenacyl bromide as the deriving agent and cyclohexanecarboxylic acid as the interal standard. The analytical column was Shimadzu VP-ODS（ 150mm× 4. 6mm, 5μm）,methanol ： water （75 ： 25） as the mobile phase and detected wave length was 248nm. RESULTS The linear rang of sodium valprate was 11.24-180. 96μg ·mL^-1, the peak area ratio and density of valproic acid derivatives and internal standard derivatives had good linear correlation. The average recovery was 101.00 %. The RSD both within day and between day was less than 3. 77~. CONCLUSION This method was rapid,accurate,sensitive and suitable for clinical therapeutic drug monitoring of sodium valprate.