ISOLATION OF DOXYCYCLINE, 6-EPIDOXYCYCLINE AND 2-ACETYL-2-DECARBOXAMIDOMETACYCLINE FROM COMMERCIAL METACYCLINE BY PREPARATIVE COLUMN LIQUID-CHROMATOGRAPHY ON SILICA-GEL

被引：11

作者：

WENG, ND ^{[1
]}

VERRESEN, K ^{[1
]}

BUSSON, R ^{[1
]}

ROETS, E ^{[1
]}

HOOGMARTENS, J ^{[1
]}

机构：

[1] CATHOLIC UNIV LEUVEN, INST FARMACEUT WETENSCHAPPEN, FARMACEUT CHEM LAB, VAN EVENSTR 4, B-3000 LOUVAIN, BELGIUM

来源：

JOURNAL OF CHROMATOGRAPHY | 1991年 / 586卷 / 01期

关键词：

D O I：

10.1016/0021-9673(91)80026-D

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

Isolation of doxycycline, 6-epidoxycycline and 2-acetyl-2-decarboxamidometacycline from commercial metacycline was achieved by preparative column liquid chromatography on silica gel, previously impregnated with edetate (EDTA). Careful control of the pH of EDTA allowed fine tuning of the separation. The mobile phases were composed of dichloromethane. methanol and 0.1 mM EDTA at pH 9.0 or 6.0. Structures were confirmed with nuclear magnetic resonance spectroscopy. The presence of doxycycline and its 6-epimer in commercial metacycline has not previously been described. The presence of the 2-acetyl derivative was not surprising since analogous 2-acetyl derivatives have been identified in other tetracyclines.

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页码：67 / 72

页数：6

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