依替米星有关物质的9-芴甲氧羰酰氯柱前衍生化高效液相色谱法检查与液质联用鉴定

孙晶,, 杭太俊, 袁耀佐*, 谭力, 赵恂, 赵卫

中国药学杂志 ›› 2014, Vol. 49 ›› Issue (7) : 596-603.

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中国药学杂志 ›› 2014, Vol. 49 ›› Issue (7) : 596-603. DOI: 10.11669/cpj.2014.07.021
论 著

依替米星有关物质的9-芴甲氧羰酰氯柱前衍生化高效液相色谱法检查与液质联用鉴定

  • 孙晶1,2, 杭太俊2, 袁耀佐1*, 谭力1, 赵恂1, 赵卫1
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Determination and Identification of Related Substances of Etimicin Sulfate by HPLC and Liquid Chromatography Tandem Mass Spectrometry Using Pre-Column Derivatization with 9-Fluorenylmethyloxycarbonyl Chloride

  • SUN Jing1,2, HANG Tai-jun2, YUAN Yao-zuo1*, TAN Li1, ZHAO Xun1, ZHAO Wei1
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摘要

目的 采用9-芴甲氧羰酰氯(Fmoc-Cl)为柱前衍生化试剂,建立了Fmoc-Cl柱前衍生化反相高效液相色谱法用于检查并鉴定硫酸依替米星的有关物质。方法 采用Lichrospher-C18色谱柱(4.6 mm×250 mm, 5 μm),流动相为乙腈-0.1%的甲酸溶液,等度洗脱,流速1.0 mL·min-1,检测波长265 nm,并采用电喷雾正离子化监测的LC-TOF/MS和LC-MS/MS鉴定主要有关物质。结果 该法比现有文献报道方法灵敏度和准确性更好,衍生化反应完全,衍生物稳定,依替米星及其有关物质衍生物色谱分离度良好,共测得并鉴定了硫酸依替米星中的25个有关物质,其中8个为第一次报道。结论 方法专属性高、准确度和耐用性好,适用于硫酸依替米星的含量测定及有关物质检测。

Abstract

OBJECTIVE To identify the related substances in etimicin sulfate by hyphenated techniques using pre-column derivatization with 9-fluorenylmethyloxycarbonyl chloride. METHODS The analysis was carried out on a Lichrospher-C18 column (4.6 mm×250 mm,5 μm)by using acetonitrile-0.1% formic acid solution as the mobile phase with isocratic elution mode at a flow rate of 1.0 mL·min-1, and the detection was performed at 265 nm. LC-TOF and LC-MS/MS methods were employed for the identification of the major related substances. RESULTS It was proved that the reaction was complete and the derivatives were stable. Good retention and separations were achieved. Twenty-five impurities were proposed based on comparison of their fragmentation patterns including 8 newly identified, and their formation mechanisms were also speculated. CONCLUSION The established method is specific and accurate with very good ruggedness and thus is suitable for the determination of etimicin sulfate and its related substances.

关键词

依替米星 / 庆大霉素C1a / 奈替米星 / 9-芴甲氧羰酰氯 / 衍生化

Key words

etimicin / gentamicic C1a / netilmicin / 9-fluorenylmethyloxycarbonyl chloride / derivatization

引用本文

导出引用
孙晶,, 杭太俊, 袁耀佐*, 谭力, 赵恂, 赵卫. 依替米星有关物质的9-芴甲氧羰酰氯柱前衍生化高效液相色谱法检查与液质联用鉴定[J]. 中国药学杂志, 2014, 49(7): 596-603 https://doi.org/10.11669/cpj.2014.07.021
SUN Jing,, HANG Tai-jun, YUAN Yao-zuo*, TAN Li, ZHAO Xun, ZHAO Wei. Determination and Identification of Related Substances of Etimicin Sulfate by HPLC and Liquid Chromatography Tandem Mass Spectrometry Using Pre-Column Derivatization with 9-Fluorenylmethyloxycarbonyl Chloride[J]. Chinese Pharmaceutical Journal, 2014, 49(7): 596-603 https://doi.org/10.11669/cpj.2014.07.021
中图分类号: R917   

参考文献

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