A High-Performance Liquid Chromatography–Electrospray–Tandem Mass Spectrometry Analysis of Cortisol and Metabolites in Placental Perfusate

Dodds, Helen M.; Taylor, Paul J.; Cannell, G. R.; Pond, Susan M.

doi:10.1006/abio.1997.2074

Cited by 33 publications

(17 citation statements)

References 22 publications

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“…Hydrocortisone has been used as internal standard by several investigators [17; 18]. In this work, we confirmed hydrocortisone molecular fragmentation at different collision induced dissociation energies.…”

Section: Resultssupporting

confidence: 84%

Hydrogen sulfide measurement using sulfide dibimane: Critical evaluation with electrospray ion trap mass spectrometry

et al. 2014

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Accurate measurement of hydrogen sulfide bioavailability remains a technical challenge due to numerous issues involving sample processing, detection methods used, and actual biochemical products measured. Our group and others have reported that reverse phase HPLC detection of sulfide dibimane (SDB) product from the reaction of H2S/HS− with monobromobimane allows for analytical detection of hydrogen sulfide bioavailability in free and other biochemical forms. However, it remains unclear whether possible interfering contaminants may contribute to HPLC SDB peak readings that may result in inaccurate measurements of bioavailable sulfide. In this study, we critically compared hydrogen sulfide dependent SDB detection using reverse phase HPLC (RP-HPLC) versus quantitative SRM electrospray ionization mass spectrometry (ESI/MS) to obtain greater clarity into the validity of the reverse phase HPLC method for analytical measurement of hydrogen sulfide. Using an LCQ-deca ion-trap mass spectrometer, SDB was identified by ESI/MS positive ion mode, and quantified by selected reaction monitoring (SRM) using hydrocortisone as an internal standard. Collision induced dissociation (CID) parameters were optimized at MS2 level for SDB and hydrocortisone. ESI/MS detection of SDB standard was found to be a log order more sensitive than RP-HPLC with a lower limit of 0.25 nM. Direct comparison of tissue and plasma SDB levels using RP-HPLC and ESI/MS methods revealed comparable sulfide levels in plasma, aorta, heart, lung and brain. Together, these data confirm the use of SDB as valid indicator of H2S bioavailability and highlights differences between analytical detection methods.

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Section: Resultssupporting

confidence: 84%

Hydrogen sulfide measurement using sulfide dibimane: Critical evaluation with electrospray ion trap mass spectrometry

et al. 2014

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“…It can also be useful for compounds, which are less amenable for separation by GC [14]. Several ionization techniques for LC-MS operating at atmospheric pressure (API) have been used for steroids including electrospray ionization (ESI-MS) [17][18][19], atmospheric pressure chemical ionization (APCI) [15,[20][21][22] and most recently atmospheric pressure photoionization (APPI) [23]. The choice of ionization technique is both compound-and instrument-dependent.…”

Section: Introductionmentioning

confidence: 99%

Determination of corticosteroids in tissue samples by liquid chromatography–tandem mass spectrometry

Rönquist-Nii

Edlund

2005

Journal of Pharmaceutical and Biomedical Analysis

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“…To date, >99% of more than 300 samples we analyzed for a variety of clinical research studies fell within the range 1.5-10% cortisol-d 3 , confirming this range is adequate for measuring CPR in diverse patient populations (data not shown). Initial isolation of cortisol by SPE with methanol elution [1, 13] demonstrated large variation for analyte signal recovery. A comparison of SPE with methanol or ethyl acetate elution [14], liquid-liquid extraction using methyl- tert -butyl ether [7], dichloromethane [12, 15], or ethyl acetate [14] found the most consistent signal recovery for cortisol was obtained with liquid-liquid extraction using ethyl acetate (data not shown).…”

Section: Resultsmentioning

confidence: 99%

Determination of cortisol production rates with contemporary liquid chromatography–mass spectrometry to measure cortisol-d3 dilution after infusion of deuterated tracer

Klopfenstein

Purnell

Brandon

et al. 2011

Clinical Biochemistry

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Objectives Measurement of 24-hour cortisol production rate (CPR) using steady-state infusion of deuterated cortisol and analysis of stable-isotope dilution by MS is a valuable tool to examine hypothalamic-pituitary-adrenal axis activity in humans. We have developed and validated an improved method for measuring cortisol dilution with contemporary LC-MS technology. Design and Methods Plasma samples and calibrators were extracted with ethylacetate. LC-MS was performed with a Surveyor HPLC and TSQ Quantum triple-quadrupole mass spectrometer equipped with an atmospheric pressure chemical ionization (APCI) source. Results Selectivity was improved over previous methods via elimination of an interferent identified as 20β-dihydrocortisol. The LLOQ for cortisol-d3 was 2.73 nmol/L and LOD 1.37 nmol/L. Plasma calibrators were linear over the concentration range 1.5%-10% cortisol-d3, with correlation coefficients >0.995. Conclusions This APCI LC-MS method offers simplified sample work-up and analysis and enables selective detection of the low concentration of cortisol-d3 infused for determination of 24-hour CPR.

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A High-Performance Liquid Chromatography–Electrospray–Tandem Mass Spectrometry Analysis of Cortisol and Metabolites in Placental Perfusate

Cited by 33 publications

References 22 publications

Hydrogen sulfide measurement using sulfide dibimane: Critical evaluation with electrospray ion trap mass spectrometry

Hydrogen sulfide measurement using sulfide dibimane: Critical evaluation with electrospray ion trap mass spectrometry

Determination of corticosteroids in tissue samples by liquid chromatography–tandem mass spectrometry

Determination of cortisol production rates with contemporary liquid chromatography–mass spectrometry to measure cortisol-d3 dilution after infusion of deuterated tracer

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