期刊
ANALYTICA CHIMICA ACTA
卷 1202, 期 -, 页码 -出版社
ELSEVIER
DOI: 10.1016/j.aca.2022.339667
关键词
Pharmaceutical analysis; Food analysis; Lipidomics; Oxylipins; LCxLC; Data -independent acquisition
资金
- Fresenius Kabi Deutschland GmbH
- Agilent Technologies [4610]
This research developed a comprehensive 2D-LC method coupled with inline DAD-UV and ESI-QTOF-MS/MS detection for separating conjugated polyunsaturated fatty acid isomers and structurally related compounds. By combining chiral and reversed-phase columns, advanced structural annotation of unknown compounds and differentiation of positional isomers of oxidized lipids can be achieved.
This research reports on the development of a comprehensive two-dimensional liquid chromatography (2D-LC) method hyphenated to inline DAD-UV and ESI-QTOF-MS/MS-detection for the separation of conjugated polyunsaturated fatty acid isomers and structurally related (saturated, unconjugated, oxidized) compounds. In pharmaceutical lipid formulations conjugated fatty acids can be found as im-purities, generated by oxidation of polyunsaturated fatty acids. Due to the structural complexity of resultant multi-component samples one dimensional liquid chromatography may be suboptimal for quality control and impurity profiling. The screened reversed-phase columns showed a lack of selectivity for the conjugated fatty acid isomers but the resolutions improved with the shape selectivity of the stationary phases (C18-< C30-< cholesteryl-ether-bonded). Further enhanced selectivity for the non-chiral conjugated FAs could be achieved with amylose/cellulose-based chiral stationary phases (CSPs) which harbor cavities for selective inclusion depending on E/Z configurations of the double bonds of the analytes. Amylose-based CSPs showed higher selectivity for conjugated fatty acids than the cellulose-based polysaccharide CSPs. Hyphenating the chiral and reversed-phase columns in a comprehensive 2D-LC-setup was favorable since they showed orthogonality and good compatibility, because both were operated under RP-conditions. The chiral dimension (1D) mainly separated the different isomers, while the reversed-phase dimension (2D) separated according to number of double bonds and degree of oxidation. Using this setup, advanced structural annotation of unknowns was possible based on UV-, MS1-and MS2-spectra. Data-independent acquisition (by SWATH) enabled differentiation of positional isomers of oxidized lipids by characteristic MS2-fragments and elucidation of co-eluted compounds by selective extracted ion chromatograms of fragment ions (MS2 EICs). (c) 2022 Elsevier B.V. All rights reserved.
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