本文選題：氨基糖苷類抗生素 + 硫酸依替米星�。� 參考：《中國藥學(xué)雜志》2015年20期

【摘要】：目的建立適用于硫酸依替米星在2015年版《中國藥典》二部中第二法(2010年版條件下)檢出有關(guān)物質(zhì)并進(jìn)行結(jié)構(gòu)鑒定的LC/MSn法。方法采用Welch Ultimate LP-C18(4.6 mm×300 mm,5μm)色譜柱,以0.2 mol·L-1三氟乙酸(添加0.1%的丙酸)-甲醇(84∶16)為流動相;流速:1.0 m L·min-1;柱后分流,30%進(jìn)入質(zhì)譜檢測,用有關(guān)物質(zhì)色譜保留時間、一級、二級質(zhì)譜信息推測結(jié)構(gòu)。結(jié)果在2010年版《中國藥典》的流動相條件中添加0.1%的丙酸,顯著提高質(zhì)譜檢出靈敏度,且依替米星及其有關(guān)物質(zhì)的保留時間無明顯改變,代表性樣品中檢測出了28個有關(guān)物質(zhì),利用雜質(zhì)對照品鑒定了9個,利用質(zhì)譜碎片信息推定了14個,其余5個因質(zhì)譜信息有限未進(jìn)行推定。結(jié)論建立的方法可以用于2010年版《中國藥典》條件下檢出有關(guān)物質(zhì)的結(jié)構(gòu)推定,為硫酸依替米星質(zhì)量提高和工藝優(yōu)化提供了參考。
[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.
【作者單位】： 江蘇省食品藥品監(jiān)督檢驗(yàn)研究院;中國藥科大學(xué);常州方圓制藥有限公司;中國食品藥品檢定研究院;
【分類號】：R927.1

【共引文獻(xiàn)】

相關(guān)期刊論文 前9條

1 李曉冰;石富國;宋沁馨;丁雯;龔楚婷;錢亞芳;丁黎;;藥物分析研究進(jìn)展[J];藥學(xué)進(jìn)展;2013年08期

2 朱曉s，

本文編號：2006428