液相色谱-发光散射-电喷雾离子阱质谱法测定硫酸依替米星及其有关物质.doc

液相色谱-蒸发光散射-电喷雾离子阱质谱法 测定硫酸依替米星及其有关物质 袁耀佐 张玫* 钱文谭力（江苏省药品检验所南京 210008 ）（南京 21000 ）摘要：目的 建立HPLC-ESI-MSn）对硫酸依替米星成品中的有关物质进行鉴定。方法Gemini NX C18(4.6mm×150mm, 5μm)色谱柱，以[水-氨水-冰醋酸（96：3.6：0.4）]-甲醇（70：30）为流动相，℃，载气流量2.6L/min；质谱条件：ESI离子源离子源温度350℃雾化室压力0 psi，干燥气流速10 L /min正离子检测方式。0.05086~1.0173g/L范围内呈较好的线性（r=0.999），重复性实验RSD=1.8%,检出限为10μg/ml。用新建立的方法，从硫酸依替米星结论 为质量控制和研究提供了可靠的分析手段Analysis of Etimicin Sulfate and Its Related Substances by High Performance Liquid Chromatography Using Evaporative LightScattering Detection and Electrospray Ion Trap Mass Spectrometry Yuan Yao-zuo1, Zhang Mei1*, Qian Wen1,Tan Li1, Yan Fei and Zhang Zheng-xing2 Jiangsu Institute for food and drug control, Nanjing 210008） Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing 210009) Abstract Objectives To establish a HPLC-ELS method for the determination of etimicinsulfate and its related substances, to identify the related substances in etimicinsulfate by using HPLC-ESI-MSn. Methods the column is Gemini NX C18(4.6mm×150mm, 5μm), the mobile phase is [H2O-ammonia-glacial acetic acid(96：3.6：0.4）)-methanol(70:30), the flow rate of mobile phase is 1ml/min, the drift tube temperature was 105℃, the flow rate of nebulizing gas is 2.6L/min. the temperature of ESI ion source is 350℃, nebulizing pressure is 40 psi, dry gas flow is 10 L /min. some related substances in etimicinsulfate were elucidatedd by analyzing their MS and MS2 fragmentation with the help of a rule summarized from the elucidation of MS2 fragmentation of etimicin. Results Good separation of etimicin and main related substances could be achieved. The standard curve was rectilinear in the range of 0.05086~1.0173g/L ( r = 0.9998). The RSD of repeatability was1.8%. The limit of detection was 10 mg/L. Eighteen related substances in etimicinsulfate were separated and detected. by HPLC-ESI-MSn ,fourteen related substances were elucidated, they are gentamicin C1a, micronomicin and three of its isomers, three of etimicin’s isome