【摘要】 采用高效液相色谱-电喷雾离子阱质谱(HPLC-MSn)联用,分离和鉴定6种氨基糖甙类抗生素及其中的杂质,并探讨这6种结构相似的氨基糖甙类抗生素的质谱裂解规律。采用Agilent SB-C18(250 mm×4.6mm,5μm)色谱柱,流动相为0.05mol/L三氟乙酸溶液-甲醇(90∶10)和0.05 mol/L五氟丙酸溶液-甲醇(65∶35);在正离子检测方式下,用电喷雾离子阱质谱法对阿司米星、异帕米星、大观霉素、威替米星、奈替米星、西索米星及其杂质进行多级质谱分析。异帕米星、威替米星、奈替米星、西索米星及其杂质在二级质谱分析时,均可发生B环(脱氧链霉胺)与C环(氨基葡萄糖)之间的糖苷键断裂,生成脱去C环的碎片离子,并进一步发生A环(氨基葡萄糖)与B环之间的糖苷键断裂,生成A环或B环的碎片离子。鉴定了6种氨基糖甙类抗生素中7个杂质的结构。更多还原

【Abstract】 A high performance liquid chromatogrpahy-electrospray ion trap mass spectrometric(HPLC-MSⁿ)method for the separation and structural identification of six aminoglycoside antibiotics and the impurities was developed.The column was Agilent SB-C₁₈（250 mm×4.6 mm,5 μm）.The mobile phases were 0.05（mol/L） trifluoroacetic acid-methanol（（90∶10）,（V/V））and 0.05 mol/L pentafluoropropionic acid-methanol（（65∶35）,（V/V））.In positive mode,netilmicin,sisomicin,vetilmicin,spectinomycin,isepamicin,astromicin and the impurities were elucidated by the use of electrospray ion trap mass spectrometry in the multi-stage MS full scan mode.It is demonstrated that the netilmicin,sisomicin,vetilmicin,isepamicin and the impurities gave abundant（product） ions by loss of the C-ring（amino-α-D-glycopyranose） in MS² full scan mode.The prominent fragmentation ions were formed from the fragmentation ions by loss of the B-ring（2-deoxy-D-streptamine）（furthermore）.The possible structure of seven impurities in six aminoglycoside antibiotics were deduced based on the HPLC-MSⁿdata.更多还原