Shipkova P A, Heimark L, Bartner P L, Chen G, Pramanik B N, Ganguly A K, Cody R B, Kusai A
Schering-Plough Research Institute, 2015 Galloping Hill Road, Kenilworth, NJ 07033, USA.
J Mass Spectrom. 2000 Nov;35(11):1252-8. doi: 10.1002/1096-9888(200011)35:11<1252::AID-JMS56>3.0.CO;2-J.
High-resolution mass spectrometry has been routinely used for structural confirmation and identification; however, it has mostly been applied to relatively pure samples. Exact mass measurement of minor components such as impurities, degradation products or metabolites in complex mixtures has been difficult without prior separation and isolation. Here we report the utilization of on-line liquid chromatography in combination with high-resolution mass spectrometry for the identification of impurities and base degradation products of Sch 27899, a member of the everninomicin class of antibiotics. Nine Sch 27899-related impurities and degradation products were detected by negative ion electrospray ionization using a magnetic sector mass spectrometer. Exact mass measurements were obtained at a resolution of 5000 using polyethylene glycol (PEG) sulfates as internal standards. Corresponding elemental compositions were determined within a 2 ppm error tolerance and structures were proposed for all components.
高分辨率质谱法一直被常规用于结构确证和鉴定；然而，它大多应用于相对纯的样品。在没有事先分离和提纯的情况下，对复杂混合物中的微量成分（如杂质、降解产物或代谢物）进行精确质量测量一直很困难。在此，我们报告了联用在线液相色谱与高分辨率质谱法来鉴定依维菌素类抗生素Sch 27899的杂质和碱降解产物。使用磁扇形质谱仪通过负离子电喷雾电离检测到了9种与Sch 27899相关的杂质和降解产物。以聚乙二醇（PEG）硫酸盐作为内标，在5000的分辨率下获得了精确质量测量结果。在误差容忍度为2 ppm的范围内确定了相应的元素组成，并对所有成分提出了结构推测。
