高效毛细管气相色谱法测定糖浆剂中丙戊酸钠含量

Capillary Column Gas Chromatography Determination of Sodium Valproate Syrup

目的:建立高效毛细管气相色谱法测定丙戊酸钠糖浆剂的含量,为其质量控制提供依据。方法:调节 pH 至丙戊酸的pK_a 以下,丙戊酸钠转化为丙戊酸,采用乙醚萃取净化样品;高效毛细管气相色谱分离和测定丙戊酸,色谱柱为 AT SE-54高效石英毛细管色谱柱(15m×0.25mm×0.33μm),柱温180℃,分流进样;进样器温度:215℃;检测器:FID,温度:215℃。载气为 N_2,流速:18mL·min^(-1);Air 150 mL·min^(-1);H_262 mL·min^(-1);Makeup(N_2)10mL·min^(-1)。结果:丙戊酸得到基线分离,在2-20mg·mL^(-1)。浓度范围内线性关系良好(r=0.9997),重复性 RSD 小于1.7%,回收率高于99.7%。结论:本法简便、快速、准确,适用于丙戊酸钠糖浆剂的质量控制。

Objective:To establish the content determination method of sodium valproate syrup by capillary column gas chromatography.Metheds:Sodium valproate was inverted into valproic acid at pH<4.5,and was extracted and purified.Valproic acid was separated and indentified on capillary column (15 m×0.25 mm×0.33 μm)by GC.The column temperature 180℃,split injection;injector temperature 215℃;detector:FID,temperature:215℃,carrier gas N_218 mL·min^(-1);Air 150 mL·min^(-1);H_262 mL·min^(-1);makeup (N_2) 10 mL·min^(-1).Results:Valproic acid had good resolution.The linear ranges of valproic acid was 2-20 mg·mL^(-1) with the correlation coefficients 0.9997.The RSD in the reproducibility test was less than 1.7%.The average recoveries was upper 99.7%.Con- clusion:The method is simple,rapid,accurate,and is suitable for sodium valproate syrup.