HPLC-DAD-MS法对酮咯酸氨丁三醇及其注射液有关物质的分析

发布时间：2018-04-14 14:18

  本文选题：酮咯酸氨丁三醇 + 非甾体抗炎药　； 参考：《药物分析杂志》2017年08期

【摘要】：目的:对国内各厂家生产的酮咯酸氨丁三醇及注射液的有关物质现状进行考察,为标准提高提供依据。方法:建立液相色谱-二极管阵列检测器-质谱联用法,采用C_(18)(100 mm×4.6 mm,3μm)色谱柱,以0.05 mol·L~(-1)乙酸铵溶液(甲酸调节pH至2.5)-乙腈(60∶40)为流动相,对酮咯酸氨丁三醇及注射液中有关物质进行分离,采用二极管阵列检测器及ESI/Q/TOF高分辨质谱检测器进行检测,对检测到的有关物质进行结构解析,并将有关物质检测结果与现行标准方法检测结果进行对比。结果:在所建立的液质条件下,酮咯酸氨丁三醇及其有关物质分离良好,可以检测到酮咯酸氨丁三醇合成副产物及降解产物共22个,推断了有关物质1、4、6、10、13、15、21和22的结构。现有酮咯酸氨丁三醇原料药及注射液产品中实际存在的有关物质有13个。现行标准方法对酮咯酸氨丁三醇及注射液中的有关物质没有漏检。结论:液质联用技术能有效地分离鉴定酮咯酸氨丁三醇及注射液中的有关物质,液质分析结果为酮咯酸氨丁三醇及注射液的质量控制提供了参考。
[Abstract]:Objective: to investigate the current situation of ketocloroic acid aminobutanol and related substances in injection produced by domestic manufacturers, and to provide basis for improving the standard.Methods: a liquid chromatography-diode array detector / mass spectrometry method was developed. The chromatographic column was CSTP 18mm 脳 4.6mm ~ (-3) 渭 m, and the mobile phase was 0.05 mol / L ~ (-1) ammonium acetate solution (pH adjusted by formic acid to pH (2.5) -acetonitrile (60: 40)).The related substances in ketocloroic acid aminobutanol and its injection were separated and detected by diode array detector and ESI/Q/TOF high resolution mass spectrometry.The results were compared with those of the current standard method.Results: under the established liquid quality conditions, the separation of ketoclalic acid aminobutanol and its related substances was good. 22 by-products and degradation products of ketocloroic acid aminobutanol could be detected.There are 13 related substances in raw materials and injection products of ketocloroic acid aminobutanol.The current standard method has not missed the detection of related substances in ketocloroic acid aminobutanol and its injection.Conclusion: the liquid-mass spectrometry can effectively separate and identify the related substances in ketocloroic acid aminobutanol and its injection. The result of liquid quality analysis provides a reference for the quality control of ketololac aminobutanol and its injection.
【作者单位】： 江苏省食品药品监督检验研究院;中国药科大学药学院;中国食品药品检定研究院;
【基金】：国家“重大新药创制”科技重大专项(2015ZX09303001)
【分类号】：O657.63;R927.1
，

本文编号：1749686