Department of Pharmaceutical Chemistry, Medical University of Gdańsk, Hallera 107, Gdańsk, 80-416, Poland.
Department of Pharmaceutical Chemistry, Medical University of Gdańsk, Hallera 107, Gdańsk, 80-416, Poland.
Anal Chim Acta. 2019 Jan 10;1046:192-198. doi: 10.1016/j.aca.2018.09.047. Epub 2018 Sep 23.
In this study, a field amplified sample injection (FASI) and hydrophobic interaction electrokinetic chromatography (HIEKC) method has been developed for the separation of five macrolide antibiotics: spiramycin, ivermectin, tylosin, josamycin, rapamycin, and one ansamycin drug - rifamycin. By the manipulation of both the sample and separation buffer compositions, their pH values and molarity, a systematic approach has been achieved to maximize analyte differential electrophoretic mobility and signal amplification. The impact of the sample solution composition and the injection mode on the signal amplification effect of the six tested antibiotics was also investigated. Moreover, the influence of the injection of the sample and the water plug on the quantity, symmetry and height of the analyte signal was demonstrated. All the analytes were completely resolved in less than 8 min in an uncoated fused-silica capillary of 75 μm internal diameter (I.D.) x 50 cm length. The electrophoretic separations were performed in a 60% (v/v) acetonitrile and 20 mM phosphate electrolyte system (pH 7.1) with an applied voltage of 25 kV. The established method was validated and confirmed to be applicable for the determination of the active ingredients in a quality control analysis.
在这项研究中，开发了一种场放大样品进样（FASI）和疏水相互作用电动色谱（HIEKC）方法，用于分离五种大环内酯类抗生素：螺旋霉素、伊维菌素、泰乐菌素、交沙霉素、雷帕霉素和一种安莎霉素药物-利福霉素。通过操纵样品和分离缓冲液的组成、pH 值和摩尔浓度，可以实现系统的方法，以最大限度地提高分析物的差分电泳迁移率和信号放大。还研究了样品溶液组成和进样模式对六种测试抗生素信号放大效果的影响。此外，还证明了样品和水塞的注入对分析物信号的数量、对称性和高度的影响。所有分析物在 75μm 内径（I.D.）x 50cm 长度的未涂层熔硅毛细管中不到 8 分钟即可完全分离。在 60%（v/v）乙腈和 20mM 磷酸盐电解质系统（pH7.1）中，施加 25kV 的电压进行电泳分离。所建立的方法经过验证，证实适用于质量控制分析中活性成分的测定。
