Streamlined stationary phase selection facilitated by a “sample-plug retention test” in supercritical fluid extraction-supercritical fluid chromatography-mass spectroscopy (SFE-SFC-MS) method development for on-line extraction of anabolic agents
Streamlined stationary phase selection facilitated by a “sample-plug retention test” in supercritical fluid extraction-supercritical fluid chromatography-mass spectroscopy (SFE-SFC-MS) method development for on-line extraction of anabolic agents
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DOI：
10.1080/10826076.2022.2098319
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发表时间：
2021-12
影响因子：
1.3
通讯作者：
B. Berger;A. Wicker;E. Preuss;Yuka Fujito;W. Hedgepeth;Masayuki Nishimura;K. Schug
中科院分区：
文献类型：
--
作者：
B. Berger;A. Wicker;E. Preuss;Yuka Fujito;W. Hedgepeth;Masayuki Nishimura;K. Schug
摘要建立了在线超临界流体萃取-超临界流体色谱-质谱联用（SFE-SFC-MS）的方法开发（MD）方法。使用适应的固定相（SP）选择程序通过包括“分析物塞保留测试”来扩展传统的SFC-MS筛选。该测试使得能够对SP上的目标分析物塞的“捕获”能力进行早期评估。使用SFE模拟方法，通过在类似于实际在线提取的仪器条件下捕获基于SFC的注射塞来模拟基于SFE的提取塞的在线捕获。13个SP筛选使用适应的MD程序的SFC分离优化的一部分，在反兴奋剂检测中的合成代谢剂（AAS）的在线SFE-SFC-MS提取方法的发展。基于目标分析物的色谱分离潜力和高塞保留潜力，选择氰基SP进行进一步开发。选择的柱用于使用通用SFE-SFC-MS方法的“概念验证”在线提取。证明了成功的浸提液堵塞捕获。对于靶向AAS，保留时间和峰面积（4-20%RSD）具有重现性。成功的第一轮SFE-SFC-MS SP选择被证明可以避免在未来开发阶段中繁琐的重新优化和简化联用的SFE-SFC-MS MD过程。图形摘要
Abstract A novel method development (MD) approach was established to aid column selection for online supercritical fluid extraction-supercritical fluid chromatography-mass spectrometry (SFE-SFC-MS). An adapted stationary phase (SP) selection procedure was used to expand traditional SFC-MS screening by inclusion of an “Analyte-Plug Retention Test.” This test enabled an early evaluation of “trapping” capability for a plug of targeted analytes on the SP. Using an SFE-simulation method, the on-line trapping of an SFE-based extract-plug was mimicked by trapping an SFC-based injection-plug under instrument conditions similar to an actual on-line extraction. Thirteen SPs were screened using the adapted MD procedure as part of the SFC-separation optimization in the development of an on-line SFE-SFC-MS extraction method for anabolic agents (AAS) in anti-doping testing. A cyano SP was chosen for further development, based on chromatographic separation potential and high plug-retention potential for targeted analytes. The chosen column was used in “proof-of-concept” on-line extractions using a generic SFE-SFC-MS method. Successful extract-plug trapping was demonstrated. Retention times and peak areas (4–20%RSD) were reproducible for targeted AAS. Successful first round SFE-SFC-MS SP selection was demonstrated to circumvent tedious re-optimization in future development stages and streamlining of the hyphenated SFE-SFC-MS MD process. Graphical Abstract