五氮杂二十五烷五盐酸盐的衍生化及高效液相色谱分析
Derivatization and high-performance liquid chromatographic analysis of pentaazapentacosane pentahydrochloride.
作者信息
Heimbecher S, Lee Y C, Tabibi S E, Yalkowsky S H
机构信息
Department of Pharmaceutical Sciences, College of Pharmacy, University of Arizona, Tucson 85721, USA.
出版信息
J Chromatogr B Biomed Sci Appl. 1997 Mar 28;691(1):173-8. doi: 10.1016/s0378-4347(96)00452-5.
A rapid high-performance liquid chromatographic method for determination of the dansyl derivative of pentaazapen-tacosane (PAPC) pentahydrochloride has been developed. The chromatographic system uses a reversed-phase C8 column, a mobile phase of acetic acid buffer and acetonitrile and UV detection. The dansylation conditions were optimized with a pH of 11.0 and a 20-fold dansyl chloride excess. The yield of dansyl PAPC increased 10-fold as the reaction pH was changed from 9.5 to 10.5. Under derivatization conditions of pH 8.5-11.0 and 1-30-fold excess dansyl chloride only perdansyl PAPC was found.
已开发出一种快速高效液相色谱法，用于测定五氮杂二十五烷（PAPC）五盐酸盐的丹磺酰衍生物。该色谱系统使用反相C8柱、乙酸缓冲液和乙腈的流动相以及紫外检测。丹磺酰化条件在pH值为11.0且丹磺酰氯过量20倍的情况下进行了优化。当反应pH值从9.5变为10.5时，丹磺酰PAPC的产率提高了10倍。在pH值为8.5 - 11.0且丹磺酰氯过量1 - 30倍的衍生化条件下，仅发现了单丹磺酰PAPC。
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