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LC-MS法鉴定利伐沙班有关物质

刘超逸, 张戈, 杭太俊, 王磊, 张晓飞, 宋敏

刘超逸, 张戈, 杭太俊, 王磊, 张晓飞, 宋敏. LC-MS法鉴定利伐沙班有关物质[J]. 中国药科大学学报, 2015, 46(4): 450-457. DOI: 10.11665/j.issn.1000-5048.20150411
引用本文: 刘超逸, 张戈, 杭太俊, 王磊, 张晓飞, 宋敏. LC-MS法鉴定利伐沙班有关物质[J]. 中国药科大学学报, 2015, 46(4): 450-457. DOI: 10.11665/j.issn.1000-5048.20150411
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LIU Chaoyi, ZHANG Ge, HANG Taijun, WANG Lei, ZHANG Xiaofei, SONG Min. Identification of related substances in rivaroxaban by LC-MS[J]. Journal of China Pharmaceutical University, 2015, 46(4): 450-457. DOI: 10.11665/j.issn.1000-5048.20150411
Citation: LIU Chaoyi, ZHANG Ge, HANG Taijun, WANG Lei, ZHANG Xiaofei, SONG Min. Identification of related substances in rivaroxaban by LC-MS[J]. Journal of China Pharmaceutical University, 2015, 46(4): 450-457. DOI: 10.11665/j.issn.1000-5048.20150411
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LC-MS法鉴定利伐沙班有关物质

  • 1.

    中国药科大学药物分析教研室

  • 2.

    江苏嘉逸医药有限公司

Identification of related substances in rivaroxaban by LC-MS

摘要

    摘要
  • 摘要: 采用LC-MS法对利伐沙班有关物质进行结构鉴定。采用Inert Sustain C18色谱柱(250 mm×4.6 mm，5 μm)，以含0.2%甲酸的乙腈-水为流动相线性梯度洗脱，对利伐沙班及其强制降解产生的有关物质进行分离；电喷雾正离子化高分辨TOF/MS检测，结合MS/MS法和对照品对照鉴定各有关物质的结构。在所建立的条件下，利伐沙班及其有关物质分离良好，检测到15个有关物质，分别为利伐沙班合成起始原料或由起始原料引入的有关物质(3个)、合成副产物(4个)和降解产物(10个)。建立的LC-MS法能有效鉴定利伐沙班有关物质，为其工艺过程控制和质量保障提供参考依据。
    Abstract: An LC-MS method was established for the identification of the related substances in rivaroxaban. HPLC separation was carried out on an Inert Sustain C18 column(250 mm×4. 6 mm, 5 μm)with linear gradient elution using a mobile phase consisting of 0. 2% formic acid acetonitrile and 0. 2% formic acid aqueous solution. Rivaroxaban and its related substances could be completely separated under the established HPLC conditions. The structures of the related substances were identified by electrospray positive ESI high resolution TOF/MS and MS/MS spectra determination and elucidation, and further verified through reference substances. Fifteen related substances were detected and identified to be three related substances of starting materials, four synthetic by-products and ten degradation products. The established method is useful for the identification of the related substances in rivaroxaban. The results obtained are valuable for its manufacturing control and quality assurance.
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    • 参考文献(13)
  • [1] Samama MM. The mechanism of action of rivaroxaban-an oral,direct factor Xa inhibitor-compared with other anticoagulants[J].Thromb Res,2011,127(6):497-504.
    [2] Terry C,Sum L.Rivaroxaban:an oral direct factor Xa inhibitor for the prevention of thromboembolism[J].Cardiol Rev,2009,17(4):192-197.
    [3] Thomas TF,Ganetsky V,Spinler SA.Rivaroxaban:an oral factor Xa inhibitor[J].Clin Ther,2013,35(1):4-27.
    [4] Çelebier M,Reçber T,Koçak E,et al.RP-HPLC method development and validation for estimation of rivaroxaban in pharmaceutical dosage forms[J].Braz J Pharm Sci,2013,49(2):359-366.
    [5] Kasad PA. Photolytic-thermal degradation study and method development of rivaroxaban by RP-HPLC[J].Int J Pharm Tech Res,2013,5(3):1254-1263.
    [6] Rohde G.Determination of rivaroxabana novel,oral,direct factor Xa inhibitor—in human plasma by high-performance liquid chromatography-tandem mass spectrometry[J].J Chromatogr B,2008,872(1/2):43-50.
    [7] Korostelev M,Bihan K,Ferreol L,et al.Simultaneous determination of rivaroxaban and dabigatran levels in human plasma by high-performance liquid chromatography-tandem mass spectrometry[J].J Pharm Biomed Anal,2014,100:230-235.
    [8] Ramisetti NR,Kuntamukkala R.Development and validation of a stability indicating LC-PDA-MS/MS method for separation,identification and characterization of process related and stress degradation products of rivaroxaban[J].RSC Adv,2014,4(44):23155-23167.
    [9] Xu J,Hu WH,Gu DF,et al.Identification and determination of related substances in atropine sulfate with hyphenated technique[J].J China Pharm Univ(中国药科大学学报),2014,45(4):438-443.
    [10] Jin C,Wang M,Na Q,et al.Identification of chromatographic-mass spectrometric structures of related substances in terazosin hydrochloride[J].Chin J Pharm Anal(药物分析杂志),2014,34(11):107-117.
    [11] Yuan J,Huang CJ,Zhang JW,et al.Synthesis of rivaroxaban[J].Chin J New Drugs(中国新药杂志),2010,19(23):2185-2187.
    [12] Gao Y,Liang B,Ni GW,et al.Graphical synthetic routes of rivaroxaban[J].Chin J New Drugs(中国新药杂志),2012,21(4):371-374.
    [13] Cai ZY,Wen YL,Zhang SL,et al.Preparation and structural confirmation of the related substances of rivaroxaban[J].Chin J Pharm(中国医药工业杂志),2014,45(4):303-307.
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  • 刊出日期:  2015-08-24

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