丙酸增强电喷雾离子化效率液质联用法推定硫酸依替米星检出有关物质的结构

发布时间：2018-06-11 19:39

本文选题：氨基糖苷类抗生素 + 硫酸依替米星　；参考：《中国药学杂志》2015年20期

【摘要】：目的建立适用于硫酸依替米星在2015年版《中国药典》二部中第二法(2010年版条件下)检出有关物质并进行结构鉴定的LC/MSn法。方法采用Welch Ultimate LP-C18(4.6 mm×300 mm,5μm)色谱柱,以0.2 mol·L-1三氟乙酸(添加0.1%的丙酸)-甲醇(84∶16)为流动相;流速:1.0 m L·min-1;柱后分流,30%进入质谱检测,用有关物质色谱保留时间、一级、二级质谱信息推测结构。结果在2010年版《中国药典》的流动相条件中添加0.1%的丙酸,显著提高质谱检出灵敏度,且依替米星及其有关物质的保留时间无明显改变,代表性样品中检测出了28个有关物质,利用杂质对照品鉴定了9个,利用质谱碎片信息推定了14个,其余5个因质谱信息有限未进行推定。结论建立的方法可以用于2010年版《中国药典》条件下检出有关物质的结构推定,为硫酸依替米星质量提高和工艺优化提供了参考。
[Abstract]:Objective to establish an LC- / MSn method for the detection and structural identification of related substances in Etimicin Sulfate in the second part of the Chinese Pharmacopoeia in 2015 (2010 edition). Methods Welch Ultimate LP-C184.6 mm 脳 300mm ~ 5 渭 m column was used with 0.2 mol L ~ (-1) trifluoroacetic acid (0.1% propionate-methanol 84: 16) as mobile phase, flow rate: 1.0 mL 路min ~ (-1). After column separation, 30% was detected by mass spectrometry. The second order mass spectrum information conjecture structure. Results 0.1% propionic acid was added to the mobile phase of the 2010 edition of Chinese Pharmacopoeia. The sensitivity of mass spectrometry was significantly improved, and the retention time of etimicin and its related substances was not changed. 28 related substances were detected in representative samples. Nine were identified by impurity reference substance, 14 were inferred by mass spectrometry fragment information, and the other 5 were not inferred due to limited mass spectrum information. Conclusion the established method can be used to predict the structure of the related substances in the 2010 edition of Chinese Pharmacopoeia and provide a reference for improving the quality of Etimicin Sulfate and optimizing the process.
【作者单位】：江苏省食品药品监督检验研究院;中国药科大学;常州方圆制药有限公司;中国食品药品检定研究院;
【分类号】：R927.1

【共引文献】