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目的采用气相色谱法测定丙戊酸钠片的含量。方法样品先用水溶解、稀硫酸酸化、二氯甲烷萃取;采用HP-FFAP气相色谱柱(30 m×0.53 mm,1.00μm),柱温150℃,氢火焰离子化检测器(FID),分流比为1∶1;用正二十烷为内标物,按内标法以峰面积计算含量。结果 0.05~0.5 mg·m L-1丙戊酸钠与内标峰面积呈良好的线性关系(r=0.9999,n=6),最低检出限3.4 ng,平均回收率为99.8%(n=9);样品含量的平均值为96.3%,RSD=0.3%(n=6)。结论所用方法准确、专属性强、精密度高,可用于丙戊酸钠片的含量测定。
Objective To determine the content of sodium valproate tablets by gas chromatography. Methods The samples were dissolved in water, acidified with dilute sulfuric acid and extracted with dichloromethane. The chromatographic separation was performed on a HP-FFAP column (30 m × 0.53 mm, 1.00 μm) with a column temperature of 150 ° C, a FID, 1: 1; n-eicosane as internal standard, according to internal standard method to calculate the peak area. Results The peak area of 0.05 ~ 0.5 mg · mL-1 valproate was linear with the internal standard peak area (r = 0.9999, n = 6) and the lowest detection limit was 3.4 ng with an average recovery of 99.8% (n = 9); the average sample content was 96.3%, RSD = 0.3% (n = 6). Conclusion The method used is accurate, specific and precise, and can be used for the determination of sodium valproate tablets.