Coupling supercritical fluid extraction (SFE) on-line with supercritical fluid chromatography (SFC) - tandem mass spectrometry (MS/MS) provides a single platform for efficient extraction, separation, and detection in a chemical analysis. SFE-SFC-MS/MS requires consideration of many extraction and chromatographic variables to not only provide the most efficient extraction, but also to analytically transfer the extracted analytes to the column for separation. There is a fundamental lack of understanding of how the variables in SFE affect those in SFC. Typically, a univariate approach is taken in on-line SFE-SFC-MS/MS method development, but this provides little insight into the relative importance of variables and their potential interactions. Here, a multivariate approach was used to develop a better understanding of the synergistic relationship between the extraction and separation processes by focusing on the optimization of extraction parameters for target analytes with a wide range of physicochemical properties in matrices of variable retentivity. The methodology used a set of optimal on-line SFE-SFC-MS/MS extraction parameters for 18 analytes of variable physicochemical properties in three different silica gel-based sample matrices are presented.

中文翻译：

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在线超临界流体萃取的多元方法 - 超临界流体色谱 - 质谱方法开发

超临界流体萃取 (SFE) 与超临界流体色谱 (SFC)-串联质谱 (MS/MS) 在线联用为化学分析中的高效萃取、分离和检测提供了单一平台。SFE-SFC-MS/MS 需要考虑许多萃取和色谱变量，不仅要提供最有效的萃取，而且还要以分析方式将萃取的分析物转移到色谱柱进行分离。对于 SFE 中的变量如何影响 SFC 中的变量，人们根本缺乏了解。通常，在在线 SFE-SFC-MS/MS 方法开发中采用单变量方法，但这几乎无法深入了解变量的相对重要性及其潜在相互作用。这里，多变量方法用于更好地理解提取和分离过程之间的协同关系，重点是优化具有可变保留性基质中各种理化特性的目标分析物的提取参数。该方法使用了一组最佳在线 SFE-SFC-MS/MS 提取参数，对三种不同的基于硅胶的样品基质中的 18 种不同理化特性的分析物进行了介绍。