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色谱-质谱联用技术研究盐酸西那卡塞的有关物质

胡钟芳, 宋敏, 杭太俊

胡钟芳, 宋敏, 杭太俊. 色谱-质谱联用技术研究盐酸西那卡塞的有关物质[J]. 中国药科大学学报, 2016, 47(6): 719-726. DOI: 10.11665/j.issn.1000-5048.20160615
引用本文: 胡钟芳, 宋敏, 杭太俊. 色谱-质谱联用技术研究盐酸西那卡塞的有关物质[J]. 中国药科大学学报, 2016, 47(6): 719-726. DOI: 10.11665/j.issn.1000-5048.20160615
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HU Zhongfang, SONG Min, HANG Taijun. Studies on related substances in cinacalcet hydrochloride by LC-MS[J]. Journal of China Pharmaceutical University, 2016, 47(6): 719-726. DOI: 10.11665/j.issn.1000-5048.20160615
Citation: HU Zhongfang, SONG Min, HANG Taijun. Studies on related substances in cinacalcet hydrochloride by LC-MS[J]. Journal of China Pharmaceutical University, 2016, 47(6): 719-726. DOI: 10.11665/j.issn.1000-5048.20160615
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色谱-质谱联用技术研究盐酸西那卡塞的有关物质

  • 中国药科大学药物分析教研室

Studies on related substances in cinacalcet hydrochloride by LC-MS

摘要

    摘要
  • 摘要: 采用LC-MS法分离和鉴定盐酸西那卡塞有关物质。采用Hypersil C18(100 mm×4.6 mm，2.4 μm)色谱柱，以0.1%乙酸铵溶液-乙腈(93∶7)为流动相A相，乙腈为流动相B相进行线性梯度洗脱，对盐酸西那卡塞有关物质及强制降解产物进行分离。经过电喷雾正离子化-高分辨TOF/MS检测，同时结合MS/MS光谱和对照品对照，对各有关物质进行分析鉴定。在所建立的液-质联用分析条件下，盐酸西那卡塞及其有关物质得到有效的分离，共检测到10个有关物质，分别为盐酸西那卡塞合成起始原料(1个)、合成中间体(1个)、合成副产物(4个)和降解产物(5个)。建立的LC-MS法能有效鉴定盐酸西那卡塞有关物质，并为其质量控制和工艺优化研究提供参考依据。
    Abstract: To develop an LC-MS method for the separation and identification of the related substances in cinacalcet hydrochloride. The separation was carried out on a Thermo BDS Hypersil C18 column(100 mm×4. 6 mm, 2. 4 μm)with mobile phase consisting of 0. 1% ammonium acetate buffer-acetonitrile(93∶7)(A)and acetonitrile(B)by gradient elution. The related substances were identified by electrospray positive ionization high resolution TOF/MS and MS/MS, and verified further through reference substances. Cinacalcet hydrochloride and itsrelated substances were separated under the established LC-MS condition. Ten related substances were detected and identified to be one starting material, one intermediate, four synthetic by-products and five degradation products. It showed that the LC-MS method was useful for separating and identifying the related substances in cinacalcet hydrochloride. And the results obtained are valuable for cinacalcet hydrochloride manufacturing process control and quality assurance.
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    • 参考文献(14)
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  • 刊出日期:  2016-12-24

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