HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHIC SEPARATION OF SUBCOMPONENTS OF ANTIMYCIN-A
HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHIC SEPARATION OF SUBCOMPONENTS OF ANTIMYCIN-A
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DOI：
10.1016/0021-9673(88)90007-6
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发表时间：
1988-08-05
期刊：
影响因子：
--
通讯作者：
ABIDI, SL
中科院分区：
文献类型：
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作者：
ABIDI, SL
使用反相高效液相色谱（HPLC）技术，抗霉素A的混合物被分离成八个迄今未报道的亚组分，A1 a，A1 b，A2 a，A2 b，A3 a，A3 b，A4 a和A4 b。尽管用含有醋酸盐缓冲液的移动的流动相可以很容易地实现已知的四种主要抗霉素A1、A2、A3和A4的基线分离，但新抗生素亚组分的分离对移动的条件的变化高度敏感。 有机改性剂的类型和组合物，缓冲盐的性质，以及添加的电解质的浓度对容量因子，分离因子和峰分辨率值有深远的影响。在检查的众多色谱系统中，由甲醇-水（70：30）和0.005 M四丁基磷酸铵（pH 3.0）组成的移动的相对亚组分的分离产生了最令人满意的结果。反相梯度HPLC分离的丹磺酰化或甲基化的抗生素化合物产生的上级色谱特性和添加的电解质的存在下是不是实现分离的关键因素。同源异构体和结构异构体之间的色谱结果的差异进行了解释的基础上的差分疏溶剂相互作用的理由。反相高效液相色谱法在最佳条件下，能够分离纯样品的甲基化抗霉素的子成分用于结构研究。
Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, A1a, A1b, A2a, A2b, A3a, A3b, A4a, and A4b. Although a base-line resolution of the known four major antimycins A1, A2, A3, and A4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifiers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpretated based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.