衍生化气相色谱法测定盐酸芬氟拉明片的纯度

 应用衍生化气相色谱法测定盐酸芬氟拉明片的纯度。样品溶解后经碱化乙酸乙酯提取 ,以盐酸美西律作内标 ,提取液用三氟乙酸酐进行酰化衍生化 ,衍生化产物在 5 %SE 30的色谱柱上分析 ,用氢火焰离子化检测器 (FID)检测。实验结果表明 ,芬氟拉明的质量浓度在 0 1g/L～ 0 5 g/L范围内线性良好 (r =0 9996 ) ;芬氟拉明与内标美西律的分离度大于 4;理论塔板数以芬氟拉明峰计大于 2 0 0 0 ;方法的精密度好 ,相对标准偏差 (RSD)为 1 4% (n=7) ;平均回收率为 (10 0 2± 2 2 ) % (n =6 ) ;检测限为 8ng。用该方法得到的结果灵敏、准确、重复性好。

Determination of Fenfluramine Hydrochloride in Tablets by Gas Chromatography with Derivatization

The contents of fenfluramine hydrochloride in tablets were determined by using gas chromatography (GC) with derivatization. Five percent SE-30 was used as stationary liquid(2.1 m x 3.2 mm i.d., glass column), and was detected with flame ionization detector (FID). The oven temperature was set at 125 degrees C, with injector and FID temperature at 160 degrees C. The fenfluramine hydrochloride in the tablets was extracted with ethyl acetate and derivatized with trifluoroacetic anhydride at 40 degrees C for 30 min, and then analyzed by GC. The quantitative determination was performed with mexiletine as the internal standard. The method showed good linearity within the mass concentration range from 0.1 g/L-0.5 g/L(r = 0.9996) and the limit of detection was 8 ng. The average recovery of the samples was (100.2 +/- 2.2)% (n = 6). The precision of the method is satisfactory(RSD = 1.4%). The method developed has been applied to the determination of fenfluramine hydrochloride in tablets.