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期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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依替米星中杂质的分离纯化及结构鉴定

Separation, purification and structural identification of impurities in etimicin

作者(英文):
分类号:R917
出版年·卷·期(页码):2017,37 (11):1978-1985
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:对依替米星及其杂质进行分离纯化,并对各杂质进行结构确定。方法:采用高效液相色谱-蒸发光散射法,选用Ultimate LP C18色谱柱(250 mm×4.6 mm,5 μm),以0.2 mol·L-1三氟乙酸溶液-甲醇(84∶16)为流动相,流速0.5 mL·min-1,漂移管温度65℃,进行HPLC-ELSD分析;采用Ultimate LP-C18色谱柱(250 mm×21.2 mm,5 μm),以0.2 mol·L-1三氟乙酸水溶液-甲醇(90∶10)为流动相,流速6 mL·min-1,ELSD为检测器,进行HPLC制备分离;以甲醇-水(80∶20)为流动相,流速0.8 mL·min-1,进行MS分析;以D2O为溶剂,采用一维和二维核磁共振谱,对制备得到的杂质进行结构测定。结果:制备分离出4种微量杂质(≤0.03%),MS及NMR分析确定了它们的结构分别为1-N-乙基加洛糖胺、1-N-乙基-3',4'-二脱氧新霉胺、1-N-乙基-3″-N-脱甲基庆大霉素C1a,1-N-乙基小诺霉素。结论:通过HPLC-ELSD及其HPLC制备分离方法的联用,能迅速检测并分离纯化出微量杂质;综合运用各种一维和二维核磁共振技术对依替米星(ETM)及其杂质的结构进行对比分析,建立了一种快速、准确分析氨基糖苷类抗生素结构的方法。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: Etimicin(ETM) and its various impurities were analyzed by an HPLC-ELSD method, and the impurities were further separated and purified for the structural identification.Methods: HPLC-ELSD analysis was applied on the Ultimate LP C18 column(250 mm×4.6 mm, 5 μm), 0.2 mol·L-1 trifluoroacetic acid aqueous solution-methanol(84:16) as the mobile phase with the flow rate of 6 mL·min-1, and the drift tube temperature of 65℃.Preparative HPLC was applied, using methanol-water(80:20) as the mobile phase with the flow rate of 0.8 mL·min-1 for MS analysis.The structures of prepared impurities in etimincin were determined by 1D and 2D NMR analysis with D2O as solvent.Results: Four trace impurities(≤ 0.03%) were separated and purified.And their structures were 1-N-ethyl garamine, 1-N-ethyl-3', 4'-di-deoxy neamine, 1-N-ethyl-3″-N-demethyl gentamicin C1a and 1-N-ethyl micronomicin, respectively, which were identified by MS and NMR.Conclusion: The coupling technique of HPLC-ELSD with HPLC preparation can be applied in rapid detecting, separating and purifying trace impurities.The structural characteristics of ETM and impurities have been comparatively studied in detail by means of 1D and 2D NMR technologies.Then a rapid and accurate structural analysis method for aminoglycoside antibiotics was established.

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