Li Bo, Van Schepdael Ann, Hoogmartens Jos, Adams Erwin
Laboratorium voor Farmaceutische Analyse, Faculteit Farmaceutische Wetenschappen, Katholieke Universiteit Leuven, O&N2, PB 923, Herestraat 49, B-3000 Leuven, Belgium.
Rapid Commun Mass Spectrom. 2007;21(11):1791-8. doi: 10.1002/rcm.3030.
The characterization of unknown impurities present in neomycin sulfate by liquid chromatography (LC) coupled with ion trap mass spectrometry (ITMS) is described. The volatile LC method was developed using an evaporative light scattering detector due to its lower investment and operating costs, easier operation and less maintenance than mass spectrometry. The method shows separation of neomycin B from seven potential related substances reported in the European Pharmacopoeia and several other unknown impurities. The unknown impurities were further investigated by coupling the developed LC method with ITMS. Their structures were deduced based on the fragmentation patterns obtained from reference substances. Four unknowns were identified as isomers of paromamine, LP-A, neamine and LP-B.
本文描述了采用液相色谱（LC）与离子阱质谱（ITMS）联用技术对硫酸新霉素中存在的未知杂质进行表征的方法。由于与质谱相比，蒸发光散射检测器投资和运行成本较低、操作更简便且维护需求更少，因此开发了一种挥发性液相色谱方法。该方法可将新霉素B与欧洲药典中报道的七种潜在相关物质以及其他几种未知杂质分离开来。通过将所开发的液相色谱方法与离子阱质谱联用，对未知杂质进行了进一步研究。根据从对照品获得的碎裂模式推断出它们的结构。四种未知物被鉴定为巴龙胺、LP - A、新霉胺和LP - B的异构体。
