Micro-UHPLC-MS/MS method for analysis of oxylipins in plasma and platelets

Cebo, Malgorzata; Fu, Xiaoqing; Gawaz, Meinrad; Chatterjee, Mainak; Lämmerhofer, Michael

doi:10.1016/j.jpba.2020.113426

Cited by 20 publications

(16 citation statements)

References 26 publications

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“…All analytes possessing a single chiral center could be readily resolved into the two enantiomers. For monohydroxides, it was observed that the (R)-enantiomer eluted earlier than the (S)-, as previously reported for this stationary phase 18 . This order of elution was inferred for analogous compounds for which enantiopure standards were not available.…”

Section: Chiral Sfc Methods Developmentsupporting

confidence: 88%

“…Initial efforts examined the Waters AMY-1 and CEL-2 columns, with the AMY-1 column evidencing superior performance for separating the octadecanoids, in agreement with earlier studies 16,18 . The AMY-1 column employs a tris(3,5-dimethylphenylcarbamate) derivative of amylose as stationary phase.…”

Section: Chiral Sfc Methods Developmentsupporting

confidence: 82%

“…Chiral RPLC methods can provide similar levels of resolution, but generally require long analysis and equilibration times 16,17 . The new generation of chiral columns, with sub-2 µm particles and higher tolerance to a range of solvents, have significantly improved chiral separation 18 . Recently, supercritical fluid chromatography (SFC) has gained popularity 19 due to improved coupling to the mass spectrometer and introduction of robust instrumentation 20 .…”

mentioning

confidence: 99%

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Development of a chiral SFC-MS/MS and reversed-phase LC-MS/MS platform for the quantitative metabolic profiling of octadecanoid oxylipins

Quaranta

Zöhrer

Revol-Cavalier

et al. 2022

Preprint

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Octadecanoids are broadly defined as oxylipins (i.e., lipid mediators) derived from 18-carbon fatty acids. In contrast to the well-studied eicosanoids, there is a lack of analytical methods for octadecanoids, hampering further investigations in the field. We developed an integrated workflow combining chiral separation by supercritical fluid chromatography (SFC) and reversed-phase liquid chromatography (LC) coupled to tandem-MS detection for quantification of a broad panel of octadecanoids. The platform included 70 custom-synthesized analytical and internal standards to extend the coverage of the octadecanoid synthetic pathways. A total of 103 octadecanoids could be separated by chiral SFC and complex enantioseparations could be performed in <13 minutes, while the achiral LC method separated 67 species in 13.5 minutes. The LC method provided a robust complementary approach with greater sensitivity relative to the SFC method. Both methods were validated in solvent and surrogate matrix in terms of linearity, lower limits of quantification (LLOQ), recovery, accuracy, precision, and matrix effects. Instrumental linearity was good for both methods (R2>0.995) and LLOQ ranged from 0.03-6.00 ng/mL for SFC and 0.01-1.25 ng/mL for LC. The average accuracy in solvent and surrogate matrix ranged from 89-109% in SFC and from 106-220% in LC, whereas coefficients of variation (CV) were <14% (at medium and high concentration) and 26% (at low concentration). Validation in surrogate matrix showed negligible matrix effects (<16% for all analytes) and average recoveries ranged from 71-83%. The combined methods provide a platform to investigate the biological activity of octadecanoids and expand our understanding of these little studied compounds.

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Section: Chiral Sfc Methods Developmentsupporting

confidence: 88%

Section: Chiral Sfc Methods Developmentsupporting

confidence: 82%

mentioning

confidence: 99%

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Development of a chiral SFC-MS/MS and reversed-phase LC-MS/MS platform for the quantitative metabolic profiling of octadecanoid oxylipins

Quaranta

Zöhrer

Revol-Cavalier

et al. 2022

Preprint

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“…Validation according to FDA guidelines showed the suitability for high-throughput analysis in a clinical routine laboratory . Cebo et al introduced a validated approach based on offline mixed-mode SPE enrichment and micro-UHPLC-ESI-triple quadruple (QqQ)-MS/MS for the quantification of 42 oxylipins in plasma and platelets at reasonable throughput (13 min per sample) . Limits of detection were between 2 and 250 fmol on column, offering comparable LODs to well established conventional LC approaches, but at significantly reduced solvent consumption.…”

Section: Navigating the Conflicting Goals Of Metabolome Coverage And ...mentioning

confidence: 99%

“…242 Cebo et al introduced a validated approach based on offline mixedmode SPE enrichment and micro-UHPLC-ESI-triple quadruple (QqQ)-MS/MS for the quantification of 42 oxylipins in plasma and platelets at reasonable throughput (13 min per sample). 243 conventional LC approaches, but at significantly reduced solvent consumption. Multidimensional Chromatography.…”

Section: ■ Harmonization and Reference Materialsmentioning

confidence: 99%

Recurrent Topics in Mass Spectrometry-Based Metabolomics and Lipidomics—Standardization, Coverage, and Throughput

et al. 2020

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Recent advances in analytical techniques for high throughput experimentation

Vervoort

Goossens

Baeten

et al. 2021

Analytical Science Advances

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High throughput experimentation is a growing and evolving field that allows to execute dozens to several thousands of experiments per day with relatively limited resources. Through miniaturization, typically a high degree of automation and the use of digital data tools, many parallel reactions or experiments at a time can be run in such workflows. High throughput experimentation also requires fast analytical techniques capable of generating critically important analytical data in line with the increased rate of experimentation. As traditional techniques usually do not deliver the speed required, some unique approaches are required to enable workflows to function as designed. This review covers the recent developments (2019‐2020) in this field and was intended to give a comprehensive overview of the current “state‐of‐the‐art.”

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Micro-UHPLC-MS/MS method for analysis of oxylipins in plasma and platelets

Cited by 20 publications

References 26 publications

Development of a chiral SFC-MS/MS and reversed-phase LC-MS/MS platform for the quantitative metabolic profiling of octadecanoid oxylipins

Development of a chiral SFC-MS/MS and reversed-phase LC-MS/MS platform for the quantitative metabolic profiling of octadecanoid oxylipins

Recurrent Topics in Mass Spectrometry-Based Metabolomics and Lipidomics—Standardization, Coverage, and Throughput

Recent advances in analytical techniques for high throughput experimentation

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