Diana J, Visky D, Hoogmartens J, Van Schepdael A, Adams E
Katholieke Universiteit Leuven, Faculteit Farmaceutische Wetenschappen, Laboratorium voor Farmaceutische Chemie en Analyse van Geneesmiddelen, O & N2, PB 923, Herestraat 49, B-3000 Leuven, Belgium.
Rapid Commun Mass Spectrom. 2006;20(4):685-93. doi: 10.1002/rcm.2364.
Liquid chromatography (LC) methods compatible with mass spectrometry (MS) that are suitable for impurity profiling of vancomycin mixtures have not been described in the literature. The mobile phases of the existing methods contain non-volatile additives and/or solvents that give problems in combination with MS. In this paper, a reversed-phase LC/tandem mass spectrometry method is described for the investigation of vancomycin and related substances. The LC method uses a Zorbax Extend C18 column (250 x 4.6 mm i.d.), 5 microm, and a mobile phase consisting of methanol, water and ammonium acetate solution (pH 9.0). This method allows us to separate vancomycin and its impurities. Mass spectral data are acquired on an LCQ ion trap mass spectrometer equipped with an electrospray interface operated in the positive and negative ion modes. The LCQ is ideally suited for identification of impurities and related substances because it provides on-line LC/MSn capability, which allows efficient identification without time-consuming isolation and purification procedures. Using this method, the fragmentation of vancomycin and known derivatives was studied and the structures of six substances occurring in commercial samples were elucidated.
文献中尚未描述适用于万古霉素混合物杂质剖析的与质谱（MS）兼容的液相色谱（LC）方法。现有方法的流动相含有非挥发性添加剂和/或溶剂，与质谱联用会产生问题。本文描述了一种反相LC/串联质谱法用于研究万古霉素及相关物质。该LC方法使用Zorbax Extend C18柱（内径250×4.6 mm，5μm），流动相由甲醇、水和醋酸铵溶液（pH 9.0）组成。该方法使我们能够分离万古霉素及其杂质。在配备电喷雾接口的LCQ离子阱质谱仪上以正离子和负离子模式采集质谱数据。LCQ非常适合鉴定杂质和相关物质，因为它具有在线LC/MSn功能，无需耗时的分离和纯化程序即可高效鉴定。使用该方法，研究了万古霉素和已知衍生物的裂解情况，并阐明了市售样品中出现的六种物质的结构。
