摘要
采用高效液相色谱-电喷雾-离子阱质谱法(HPLC-ESI-IT-MSn)对硫酸依替米星中有关物质结构进行推定。采用Phenomnex Gemini NX C18色谱柱,以水-氨水-冰醋酸(96∶3.6∶0.4,V/V)-甲醇(70∶30,V/V)为流动相,质谱条件:电喷雾离子源(ESI),正离子检测模式;离子源温度350℃;雾化氮气压力275.8kPa;干燥氮气流速10L/min;离子阱质谱检测器,Smart扫描模式,扫描质量范围m/z100～900。硫酸依替米星样品中共检出18种有关物质,对其中的13种物质的结构进行了推定,其余5种有关物质的结构未进行解析,只提供了分子量和二级质谱信息。
A high performance liquid chromatography-electrospray ionization-ion trap-mass spectrometry（HPLC-ESI-IT-MSn） method for the identification of related substances in etimicin was established. The analytical conditions were as follows： Phenomnex Gemini NX C18（150 mm×4.6 mm, 5 μm） column; the mobile phase：[water-ammonia-glacial acetic acid（96∶3.6∶0.4）]-methanol（70∶30）; flow rate of mobile phase： 1 mL/min; temperature of ESI ion source： 350 ℃; nebulizing pressure： 275.8 kPa; dry gas flow： 10 L/min and the analytes were detected in the positive mode. Eighteen related substances in a etimicin sample were separated and detected by HPLC-ESI-IT-MSn and thirteen related substances were deduced, they are gentamicin C1a, micronomicin and its three isomers, two etimicin′s isomers, two degradation products of etimicin, two homologues of etimicin, and two other unknown compounds, the other five related substances which MS and MS2 data were detected can not be elucidated.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2010年第6期817-822,共6页
Chinese Journal of Analytical Chemistry
关键词
硫酸依替米星
高效液相色谱-电喷雾-离子阱质谱
结构鉴定
Etimicin sulfate
High performance liquid chromatography-electrospray ionization ion trap-mass spectrometry
Characterization
