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[采用衍生化气相色谱法测定片剂中盐酸芬氟拉明]

[Determination of fenfluramine hydrochloride in tablets by gas chromatography with derivatization].

作者信息

Tao Q F

机构信息

Zhejiang Provincial Institute for Drug Control, Hangzhou 310004, China.

出版信息

Se Pu. 2001 May;19(3):270-2.

Abstract

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.

摘要

采用衍生化气相色谱法(GC)测定片剂中盐酸芬氟拉明的含量。以5%的SE-30为固定液(2.1 m×3.2 mm内径,玻璃柱),用火焰离子化检测器(FID)检测。柱箱温度设定为125℃,进样器和FID温度为160℃。片剂中的盐酸芬氟拉明用乙酸乙酯提取,在40℃下用三氟乙酸酐衍生化30分钟,然后用GC分析。以美西律为内标进行定量测定。该方法在质量浓度范围0.1 g/L - 0.5 g/L内线性良好(r = 0.9996),检测限为8 ng。样品的平均回收率为(100.2±2.2)%(n = 6)。该方法的精密度令人满意(RSD = 1.4%)。所建立的方法已应用于片剂中盐酸芬氟拉明的测定。

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