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 mass spectrometric cleavage and chromatographic behavior of 8 aminoglycoside antibiotics 2,4-dinitrofluorobenzene (FDNB) derivatized by electrospray ion trap mass spectrometry (ESI-MSn). Methods The solutions of FDNB derivatized with aminoglycoside antibiotics were directly introduced into the ESI ion source for analysis. Results In the positive ion detection mode, the glycosidic bonds between ring A and ring B could be cleaved by each compound during secondary mass spectrometry analysis to generate the fragment ions which deprotte the A ring. The glycosidic bond between the B ring and the C ring is cleaved to generate fragment ions that de-B ring or C ring. Neomycin B is composed of four rings. During the third-order mass spectrometry analysis, the derivatization product of the neomycin B breaks the glycosidic bond between the B ring and the C ring and mainly generates the fragment ion of the B ring. In the fourth-stage mass spectrometry analysis , Further generating fragment ions off C ring or D ring. Conclusion Chromatographic behavior of the FDNB derivatisation product of aminoglycoside antibiotics was obtained by LC-MS / MS and HPLC-UV analysis. The chromatographic behavior of the FDNB derivatisation product for HPLC-UV and LC-MS / MS was provided in accordance with.