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首页> 外文期刊>Analytical and Bioanalytical Chemistry >An integrated method for degradation products detection and characterization using hybrid ion trap/time-of-flight mass spectrometry and data processing techniques: Application to study of the degradation products of danofloxacin under stressed conditions
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An integrated method for degradation products detection and characterization using hybrid ion trap/time-of-flight mass spectrometry and data processing techniques: Application to study of the degradation products of danofloxacin under stressed conditions

机译：一种使用混合离子阱/飞行时间质谱和数据处理技术进行降解产物检测和表征的综合方法：在研究研究条件下达氟沙星降解产物的应用

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A new strategy using hybrid ion trap/time-of-flight mass spectrometry coupled with high-performance liquid chromatography and post-acquisition data mining techniques was developed and applied to the detection and characterization of degradation products of danofloxacin. The degradation products formed under different forced conditions were separated using an ODS-C18 column with gradient elution. Accurate full-scan MS data were acquired in the first run and processed with the combination of extracted ion chromatograms and LC-UV chromatograms. These processes were able to find accurate molecular masses of possible degradation products. Then, the accurate MS/MS data acquired through data-dependent analysis mode in another run facilitated the structural elucidations of degradation products. As a result, a total of 11 degradation products of danofloxacin were detected and characterized using the developed method. Overall, this analytical strategy enables the acquisition of accurate-mass LC/MS data, search of a variety of degradation products through the post-acquisition processes, and effective structural characterization based on elemental compositions of degradation product molecules and their product ions. The ability to measure degradation products via tandem mass spectrometry coupled with accurate mass measurement, all in only two experimental runs, is one of the most attractive features of this methodology. The results demonstrate that use of the LC/MS-IT-TOF approach appears to be rapid, efficient and reliable in structural characterization of drug degradation products.
机译：提出了一种使用混合离子阱/飞行时间质谱结合高效液相色谱和采集后数据挖掘技术的新策略，并将其用于检测和表征达氟沙星降解产物。使用具有梯度洗脱的ODS-C18色谱柱分离在不同强制条件下形成的降解产物。在第一次运行中获得了准确的全扫描MS数据，并结合了提取的离子色谱图和LC-UV色谱图进行了处理。这些过程能够找到可能降解产物的准确分子质量​​。然后，在另一轮运行中通过依赖于数据的分析模式获得的准确MS / MS数据有助于降解产物的结构阐明。结果，使用开发的方法检测并鉴定了11种达氟沙星降解产物。总体而言，这种分析策略能够采集精确质量的LC / MS数据，通过后采集过程搜索各种降解产物，并基于降解产物分子及其产物离子的元素组成进行有效的结构表征。通过串联质谱分析降解产物的能力以及精确的质量测定（仅两个实验运行），是该方法最吸引人的功能之一。结果表明，在药物降解产物的结构表征中，使用LC / MS-IT-TOF方法似乎是快速，有效和可靠的。

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