Separation and characterization of clindamycin and related impurities in bulk drug by high-performance liquid chromatography-electrospray tandem mass spectrometry.
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.
Zhou
Hui
H
Zhejiang University, College of Pharmaceutical Sciences, Hangzhou 310031, PR China.
Zheng
Zhiguo
Z
Wu
Shihua
S
Tai
Yuanpo
Y
Cao
Xiaoji
X
Pan
Yuanjiang
Y
D000900:Anti-Bacterial Agents / Q000032:analysis* / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D002981:Clindamycin / Q000032:analysis* / Q000737:chemistry; D004340:Drug Contamination; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
D000900:Anti-Bacterial Agents; D002981:Clindamycin