Torres-Cartas S, Martín-Biosca Y, Sagrado S, Villanueva-Camañas R M, Medina-Hernández M J
Departmento de Quimica Analita, Facultad de Farmacia, Universidad de Valencia, Valencia, Spain.
Biomed Chromatogr. 2007 Jan;21(1):21-8. doi: 10.1002/bmc.710.
The determination of highly hydrophobic basic compounds by means of conventional reversed-phase liquid chromatographic methods has several drawbacks. Owing to the characteristics of micellar liquid chromatography (MLC) and capillary electrophoresis (CE), these techniques could be advantageous alternatives to reversed-phase chromatographic methods for the determination of these kinds of compounds. The objective of this study was to develop and compare MLC and CE methods for the determination of antipsychotic basic drugs (amitryptiline, haloperidol, perphenazine and thioridazine) in pharmaceutical preparations. The chromatographic determination of the analytes was performed on a Kromasil C(18) analytical column; the mobile phase was 0.04 m cetyltrimethylammonium bromide (CTAB), at pH 3, containing 5% 1-butanol, at a flow rate of 1 mL/min. The CE separation was performed in a fused-silica capillary with a 50 mm tris-(hydroxymethyl)-aminomethane buffer, pH 7, at an applied voltage of 20 kV, using barbital as internal stardard. The proposed methods are suitable for a reliable quantitation of these compounds in the commercial tablets and drops in terms of accuracy and precision and require a very simple pre-treatment of the samples. By comparing the performance characteristics and experimental details of the MLC and CE methods we conclude that CE seems to be slightly better than MLC in the determination of highly hydrophobic compounds in pharmaceuticals in terms of resolution and economy, taking into account that the limits of detection are not a handicap in pharmaceutical samples.
采用传统反相液相色谱法测定高疏水性碱性化合物存在若干缺点。由于胶束液相色谱法(MLC)和毛细管电泳法(CE)的特性,这些技术可能是反相色谱法测定这类化合物的有利替代方法。本研究的目的是开发并比较MLC和CE方法,用于测定药物制剂中的抗精神病碱性药物(阿米替林、氟哌啶醇、奋乃静和硫利达嗪)。分析物的色谱测定在Kromasil C(18)分析柱上进行;流动相为0.04 m十六烷基三甲基溴化铵(CTAB),pH值为3,含有5%的正丁醇,流速为1 mL/min。CE分离在熔融石英毛细管中进行,使用50 mm三(羟甲基)氨基甲烷缓冲液,pH值为7,施加电压为20 kV,以巴比妥为内标。所提出的方法在准确性和精密度方面适用于可靠定量商业片剂和滴剂中的这些化合物,并且样品预处理非常简单。通过比较MLC和CE方法的性能特征和实验细节,我们得出结论,考虑到检测限在药物样品中并非障碍,就分辨率和经济性而言,CE在测定药物中的高疏水性化合物方面似乎略优于MLC。