Impurity profiling of acetylspiramycin by liquid chromatography-ion trap mass spectrometry.
Investigation of acetylspiramycin (ASPM) and its related substances was carried out using a reversed-phase liquid chromatography/tandem mass spectrometry method. The identification of impurities in the ASPM complex was performed with a quadrupole ion trap mass spectrometer, with an electrospray ionization (ESI) source in the positive ion mode which provides MS(n) capability. A total of 83 compounds were characterized in commercial samples, among which 31 impurities that had never been reported and 31 partially characterized impurities were deduced using the collision-induced dissociation (CID) spectra of major ASPM components as templates. Most of the major impurities arise from the starting materials and the synthesis process. This work provides very useful information for quality control of ASPM and evaluation of its synthesis process.
Wang
Ming-juan
MJ
National Institute for Control of Pharmaceutical and Biological Products, Beijing 100050, China.
Pendela
Murali
M
Hu
Chang-qin
CQ
Jin
Shao-hong
SH
Hoogmartens
Jos
J
Van Schepdael
Ann
A
Adams
Erwin
E
D000107:Acetylation; D056148:Chromatography, Reverse-Phase / Q000379:methods*; D004340:Drug Contamination; D015572:Spiramycin / Q000031:analogs & derivatives* / Q000737:chemistry / Q000592:standards; D053719:Tandem Mass Spectrometry / Q000379:methods*
C033163:acetylspiramycin; D015572:Spiramycin