Rapid Ion Mobility Separations of Bile Acid Isomers Using Cyclodextrin Adducts and Structures for Lossless Ion Manipulations.

Rapid Ion Mobility Separations of Bile Acid Isomers Using Cyclodextrin Adducts and Structures for Lossless Ion Manipulations.
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DOI:
10.1021/acs.analchem.8b02990
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发表时间:
2018-09-18
影响因子:
7.4
通讯作者:
Smith RD
Smith RD
中科院分区:
化学1区
文献类型:
--
作者:
Chouinard CD;Nagy G;Webb IK;Garimella SVB;Baker ES;Ibrahim YM;Smith RD

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胆汁酸 (BA) 是一类重要的类固醇代谢物,通常表现出与疾病状态和其他健康状况相关的变化。目前对这些结构相似的化合物的分析因缺乏灵敏度、分离时间长且异构体分辨率往往较差而受到限制。为了克服这些挑战并为 BA 异构体提供快速分析,我们利用环糊精加合物与无损离子操作 (SLIM) 结构提供的新型离子淌度 (IM) 分离功能。环糊精被发现与所研究的牛磺基和糖基 BA 异构体相互作用,形成刚性的非共价主客体包合物。如果不使用环糊精加合物,BA 异构体的各自迁移率几乎相同,因此无法进行基线解析。环糊精-胆汁酸主体-客体包合复合物的每次分离都在不到 1 秒的时间内完成,为当前基于液相色谱的分离提供了更快的替代方案。 SLIM 提供了积累较大离子群和 IM 峰压缩的功能,从而实现了所研究的 BA 异构体的更高分辨率的分离并增加了信号强度。
Bile acids (BAs) constitute an important class of steroid metabolites often displaying changes associated with disease states and other health conditions. Current analyses for these structurally similar compounds are limited by a lack of sensitivity and long separation times with often poor isomeric resolution. To overcome these challenges and provide rapid analyses for the BA isomers, we utilized cyclodextrin adducts in conjunction with novel ion mobility (IM) separation capabilities provided by structures for lossless ion manipulations (SLIM). Cyclodextrin was found to interact with both the tauro- and glyco-conjugated BA isomers studied, forming rigid noncovalent host-guest inclusion complexes. Without the use of cyclodextrin adducts, the BA isomers were found to be nearly identical in their respective mobilities and thus unable to be baseline resolved. Each separation of the cyclodextrin—bile acid host—guest inclusion complex was performed in less than 1 s, providing a much more rapid alternative to current liquid chromatography-based separations. SLIM provided capabilities for the accumulation of larger ion populations and IM peak compression that resulted in much higher resolution separations and increased signal intensities for the BA isomers studied.
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