摘要
目的采用电喷雾离子阱质谱(ESI-MSn)法研究8种氨基糖苷类抗生素2,4-二硝基氟苯(FDNB)衍生化产物的质谱裂解规律及色谱行为。方法分别取氨基糖苷类抗生素FDNB衍生化产物溶液,将其直接导入ESI离子源进行分析。结果在正离子检测方式下,各化合物在二级质谱分析时,均可发生A环与B环之间的糖苷键断裂,生成脱去A环的碎片离子;在三级质谱分析时,进一步发生B环与C环之间的糖苷键断裂,生成脱去B环或C环的碎片离子。新霉素B由4个环组成,在三级质谱分析时,其衍生化产物发生B环与C环之间的糖苷键断裂,主要生成脱去B环的碎片离子;在四级质谱分析中,进一步生成脱去C环或D环的碎片离子。结论通过LC-MS/MS和HPLC-UV分析获得了氨基糖苷类抗生素FDNB衍生化产物的色谱行为信息,为该类药物分析方法(HPLC-UV和LC-MS/MS)的建立和结构解析提供依据。
OBJECTIVE To study the dissociation pathways and chromatographic behavior of FDNB-derivatized products of eight aminoglycoside antibiotics. METHODS The solution of FDNB-derivatized products of eight aminoglyeoside antibiotics was injected onto the electrospray ion resource to elucidate their structurs. RESULTS The FDNB-derivatized products of eight aminoglycoside an- tibiotics except neomycin B produced prominent fragmentation ions by loss of A-ring in MS2 full scan mode. In MS3 full scan mode, the abundant fragmentation ions were produced from the two-stage fragmentation ions by loss of C-ring or B-ring, separately. The FDNB-derivatized product of neomycin B demonstrated a prominent fragmentation ion at m/z 643 by loss of B-ring from the ion at m/z 1 119 in MS3 full scan mode. In MS4 full scan mode, the abundant fragmentation ions at m/z 493 and m/z 151 were formed from the fragmentation ion at rrt/z 643 by loss of C-ring or D-ring, separately. The chromatographic behaviors of the FDNB-derivatized products of eight aminoglycoside antibiotics were investigated by LC-MS/MS and HPLC-UV. CONCLUSION The structural information of the FDNB- derivatized products of aminoglycoside antibiotics was obtained via collision-activated dissociation, which provided a sound basis for the structural elucidation of the FDNB-derivatized products of aminoglycoside antibiotics and development of analytical methods （ LC-MS/ MS and HPLC-UV） of aminoglycoside compounds.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2011年第6期458-462,共5页
Chinese Pharmaceutical Journal
关键词
电喷雾离子阱质谱法
氨基糖苷类抗生素
FDNB衍生化产物
结构解析
electrospray ion trap mass spectrometry
aminoglycoside antibiotics
the FDNB-derivatized products
structural elucidation
