Splitless hyphenation of SFC with MS by APCI, APPI, and ESI exemplified by steroids as model compounds

Parr, Maria Kristina; Wüst, Bernhard; Teubel, Juliane; Joseph, Jan Felix

doi:10.1016/j.jchromb.2018.05.017

Cited by 36 publications

(20 citation statements)

References 64 publications

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“…In the most recent publication, Parr et al . reported the analysis of 32 underivatised steroids with an analysis time of 21 min and LODs ranging from 1 to 50 ng/mL 18 . In comparison, our method is fast (5 min) with LODs less than 0.05 ng/mL for most of the steroids that we measured.…”

Section: Resultsmentioning

confidence: 99%

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A Novel Targeted Analysis of Peripheral Steroids by Ultra-Performance Supercritical Fluid Chromatography Hyphenated to Tandem Mass Spectrometry

Kock

Acharya

Ubhayasekera

et al. 2018

Sci Rep

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Ultra-performance supercritical fluid chromatography–tandem mass spectrometry (UPSFC–MS/MS) is an alternative method for steroid analysis. Continuous development of analytical methodologies for steroid profiling is of major importance in the clinical environment to provide useful and more comprehensive data. The aim of this study was to identify and quantify a large number of endogenous steroids from the four major classes (estrogens, androgens, progestogens and corticosteroids) simultaneously within a short analytical time. This novel UPSFC–MS/MS method with electrospray in positive ionisation (ESI+) mode is robust, selective and present sufficiently high sensitivity to profile nineteen steroids in 50 µL human plasma. Under optimised conditions, nineteen different steroids were separated with high efficiency in the multiple reaction monitoring (MRM) mode. The linearity of the method was good with correlation coefficients (R2) in the range of 0.9983–0.9999 and with calibration range from 0.05–500 ng/mL in human plasma. The intraday and interday precision of the method, as RSD, was less than 15%. The accuracy of the nineteen analytes varied between 80 to 116%. Finally, the novel method was successfully applied for the determination of nineteen steroids within 5 minutes providing the possibility to use it for research as well as routine healthcare practice.

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Section: Resultsmentioning

confidence: 99%

“…UPSFC has been connected to ESI, APCI and atmospheric pressure photoionisation (APPI) as ionisation sources for MS detection 15 , 18 . Parr et al .…”

Section: Resultsmentioning

confidence: 99%

A Novel Targeted Analysis of Peripheral Steroids by Ultra-Performance Supercritical Fluid Chromatography Hyphenated to Tandem Mass Spectrometry

Kock

Acharya

Ubhayasekera

et al. 2018

Sci Rep

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“…The recent introduction of modern and reliable UHPSFC-MS systems allowed to experimentally prove some of the potential benefits of SFC over LC. Indeed, as shown in [28,[47][48][49][50], excellent values for LODs and LOQs were met, with LOD values often down to below 1 ppb [28]. However, SFC-MS does not systematically provide a clear advantage over LC-MS in terms of sensitivity.…”

Section: Achievable Sensitivity In Sfc-ms Vs Lc-msmentioning

confidence: 99%

“…This means that users have the possibility to modify the mobile phase composition before entering MS detection, so that the ionization process can be enhanced, especially in ESI mode. Some authors have recently demonstrated how the addition of either small quantities of water or the use of additives/buffers in the make-up pump, increased the MS signals, thus improving sensitivity [28,48]. Using a wide range of endogenous steroids, the authors screened different buffers/additives in the make-up solvent, finding that either pure ammonium fluoride or ammonium fluoride mixed with formic acid in the solvent, can greatly improve ionization efficiency in ESI mode for steroids.…”

Section: Accepted Manuscriptmentioning

confidence: 99%

“…Indeed, the delivery of a methanol-rich solvent strongly limits the precipitation of polar compounds, without sacrificing too much SFC and MS performance. The addition of a make-up solvent, however, may lead to the insurgence of another potential problem: a dilution factor can appear which could negatively affect MS sensitivity, especially on concentrationdependent ionization sources such as ESI [25,[27][28][29]. Contrary to what could be expected, the dilution factor remains always reasonable, whatever the mobile phase and make-up conditions, thanks to the use of the active BPR [27,30].…”

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confidence: 97%

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Supercritical fluid chromatography – Mass spectrometry: Recent evolution and current trends

Losacco

Veuthey

Guillarme

2019

TrAC Trends in Analytical Chemistry

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• A detailed summary on SFC-MS interfaces is given, with emphasis on current issues and potential solutions. • Differences between LC-MS and SFC-MS in terms of matrix effects generated are highlighted. • Sensitivity under SFC-MS has been demonstrated to be comparable to what it can be reached in LC-MS conditions. • Applications for SFC-MS are shifting towards the analysis of compounds with increasing polarity and analytes available in complex matrices.

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Assessment of ammonium fluoride as a mobile phase additive for sensitivity gains in electrospray ionization

McFadden,

Ames

2023

Analytical Science Advances

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Ammonium fluoride has been shown to improve sensitivity when using electrospray ionization (ESI) coupled with mass spectrometry (MS). Recent internal investigation furthered that claim, through the observation of improved sensitivity when analyzing steroid molecules. This work focuses on extending those observations to other small molecules to understand the impact ammonium fluoride has on detection sensitivity with optimized instrument conditions. Using conventional liquid chromatography ESI‐MS we investigated sensitivity differences between ammonium fluoride, formic acid, or ammonium hydroxide as mobile phase additives. Full source optimization was performed for nine compounds at three different organic concentrations (30%, 60%, or 90%) with formic acid, ammonium fluoride, and ammonium hydroxide adjustment. Optimization results were compiled to generate individual methods by compound, polarity, mobile phase, and organic concentration. Flow injection analysis was performed with fully optimized methods to compare compounds across different solvent systems under optimal conditions. Negative ESI data showed 2–22‐fold sensitivity improvements for all compounds with ammonium fluoride. Positive ESI data showed > 1–11‐fold improvement in sensitivity for four of seven compounds and no change for three of seven compounds with ammonium fluoride. Ammonium fluoride improved ESI− sensitivity for all compounds studied when using optimized source conditions. Investigation with ESI+ analyses showed mixed results, with four of seven compounds showing improvement and others showing equivalency or slight loss in sensitivity, suggesting potential sensitivity gains for some analogs with ESI+.

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Splitless hyphenation of SFC with MS by APCI, APPI, and ESI exemplified by steroids as model compounds

Cited by 36 publications

References 64 publications

A Novel Targeted Analysis of Peripheral Steroids by Ultra-Performance Supercritical Fluid Chromatography Hyphenated to Tandem Mass Spectrometry

A Novel Targeted Analysis of Peripheral Steroids by Ultra-Performance Supercritical Fluid Chromatography Hyphenated to Tandem Mass Spectrometry

Supercritical fluid chromatography – Mass spectrometry: Recent evolution and current trends

Assessment of ammonium fluoride as a mobile phase additive for sensitivity gains in electrospray ionization

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