Determination of drugs used in advanced breast cancer by capillary gas chromatography of pharmaceutical formulations
Determination of drugs used in advanced breast cancer by capillary gas chromatography of pharmaceutical formulations
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DOI：
10.1002/jssc.200301334
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发表时间：
2003-07-01
影响因子：
3.1
通讯作者：
Cabello, MP
中科院分区：
文献类型：
--
作者：
Berzas, JJ;Rodríguez, J;Cabello, MP
开发了火焰离子化检测（FID）毛细管气相色谱方法，用于分析药物制剂中的他莫昔芬、阿那曲唑和来曲唑，以氯米帕明作为内标，以实现定量。研究了最佳条件：柱头压力 (110 kPa)、进样器和检测器 (FID) 温度（均为 325°C）、不分流步骤的时间和温度（0.75 分钟和 70°C）、进样体积（2 µL）以及提供短于 8 分钟分析时间的柱箱温度程序。对验证方法的主要方面进行了检查和讨论。使用 Plackett-Burman 分数阶乘模型和十五个实验的矩阵对该方法的耐用性进行了测试。他莫昔芬、阿那曲唑和来曲唑的检测限分别为 17.0、9.6 和 30.6 mug L-1。该方法简单、快速、灵敏；经药物制剂分析测试，回收率在98.8%~100.3%之间。
A capillary gas chromatographic method with flame ionisation detection (FID) has been developed for the analysis of Tamoxifen, Anastrozole, and Letrozole in their pharmaceutical preparations, using Clomipramine as the internal standard in order to achieve quantification. Optimal conditions were investigated: column head pressure (110 kPa), injector and detector (FID) temperatures (both 325degreesC), time and temperature for the splitless step (0.75 min and 70degreesC), volume injected (2 muL), and an oven temperature program providing analysis times shorter than 8 minutes. The principal aspects of the validation method are examined and discussed. A test of the ruggedness of this method was carried out using the Plackett-Burman fractional factorial model with a matrix of fifteen experiments. Detection limits of 17.0, 9.6, and 30.6 mug L-1 were obtained for Tamoxifen, Anastrozole, and Letrozole, respectively. This method is simple, rapid, and sensitive; it was tested on the analysis of pharmaceutical preparations, achieving recoveries between 98.8% and 100.3%.