Zhou Hui, Zheng Zhiguo, Wu Shihua, Tai Yuanpo, Cao Xiaoji, Pan Yuanjiang
Zhejiang University, College of Pharmaceutical Sciences, Hangzhou 310031, PR China.
J Pharm Biomed Anal. 2006 Jun 16;41(4):1116-23. doi: 10.1016/j.jpba.2006.02.014. Epub 2006 Apr 17.
A simple high-performance liquid-electrospray ionization tandem mass spectrometric (HPLC-ESI-MSn) method has been developed for the rapid identification of clindamycin and its related minor impurities in bulk drug. The ESI-MSn results obtained allowed us to propose plausible schemes for their fragmentations, which were confirmed further by electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (ESI-FTICR-MS) using collision-induced dissociation (CID) method at high mass resolution. The positive ESI-MS/MS of clindamycin and its derivative compounds showed some diagnostic fragments, such as the neutral losses of H2O, HCl, methanethiol and 2-methylthio-ethenol, and the residue of 3-propyl-N-methylpyrrolidine and 3-ethyl-N-methylpyrrolidine, which are specific and useful for the identification of the lincosamide antibiotics and related impurities. According to the fragmentation mechanism of mass spectrometry and HPLC-UV-ESI-MSn data, six impurities of clindamycin have been identified on-line. Additionally, the positive ion mode extracted ion current (EIC) method has been used to separate and identify these lincosamide compounds.
已开发出一种简单的高效液相-电喷雾电离串联质谱（HPLC-ESI-MSn）方法，用于快速鉴定原料药中克林霉素及其相关微量杂质。所获得的ESI-MSn结果使我们能够提出其碎片化的合理方案，通过使用高质量分辨率的碰撞诱导解离（CID）方法的电喷雾电离傅里叶变换离子回旋共振质谱（ESI-FTICR-MS）进一步证实了这些方案。克林霉素及其衍生物化合物的正ESI-MS/MS显示出一些诊断性碎片，例如H2O、HCl、甲硫醇和2-甲硫基乙烯醇的中性丢失，以及3-丙基-N-甲基吡咯烷和3-乙基-N-甲基吡咯烷的残基，这些对于林可酰胺类抗生素及其相关杂质的鉴定具有特异性且有用。根据质谱的碎片化机制和HPLC-UV-ESI-MSn数据，在线鉴定了克林霉素的六种杂质。此外，正离子模式提取离子流（EIC）方法已用于分离和鉴定这些林可酰胺类化合物。
