头孢拉定一种杂质的分离与结构解析
Isolation and structural elucidation of an impurity of cefradine.
作者信息
Zhu Y, Hendrix C, Busson R, Janssen G, Roets E, Hoogmartens J
机构信息
Katholieke Universiteit Leuven, Laboratorium voor Farmaceutische Chemie, Instituut voor Farmaceutische Wetenschappen, Belgium.
出版信息
J Pharm Biomed Anal. 1994 Sep;12(9):1137-40. doi: 10.1016/0731-7085(94)00042-5.
An impurity of unknown identity was isolated from commercial cefradine by liquid chromatography on poly (styrene-divinylbenzene) with HOAc (0.01 M)-CH3CN (94:6, v/v) as the mobile phase. The structure was elucidated as 4',5'-dihydrocefradine using nuclear magnetic resonance spectroscopy (NMR) and mass spectrometry (MS). The structure was confirmed by comparison with the chromatographic retention characteristics and photodiode-array detected ultraviolet spectrum of the synthetic compound and with its infrared, NMR and MS spectra. The presence of 4',5'-dihydrocefradine in cefradine has not been described previously.
采用聚（苯乙烯-二乙烯基苯）液相色谱法，以醋酸（0.01 M）-乙腈（94:6，v/v）为流动相，从市售头孢拉定中分离出一种身份不明的杂质。通过核磁共振光谱（NMR）和质谱（MS）确定其结构为4',5'-二氢头孢拉定。通过与合成化合物的色谱保留特性、光电二极管阵列检测的紫外光谱及其红外、NMR和MS光谱进行比较，证实了该结构。头孢拉定中4',5'-二氢头孢拉定的存在此前尚未见报道。
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