Semi-automated serum steroid profiling with tandem mass spectrometry

Rakete, Sophie; Schubert, Tom; Vogeser, Michael

doi:10.1016/j.jmsacl.2022.12.006

Cited by 4 publications

(3 citation statements)

References 35 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Energy‐resolved breakdown curves can be a useful tool in method development for optimization of the collision energy for ideal target ion production (and thus improved sensitivity). Previous work has been done on optimizing collision energy for SRM/MRM transitions, including for drugs in serum matrices, 23 plasma proteins, 24 and sulfonamides in fish 25 . Notably, a recent study was published that sought to provide a protocol to use breakdown curves during LC–MS/MS method development, using piperacillin and testosterone in both matrix‐free and serum matrices 26 …”

Section: Introductionmentioning

confidence: 99%

Further exploration of the collision‐induced dissociation of select beta blockers: Acebutolol, atenolol, bisoprolol, carteolol, and labetalol

Carlo,

Patrick

2023

J Mass Spectrom

View full text Add to dashboard Cite

Beta blockers are a class of drugs commonly used to treat heart‐related diseases; they are also regulated under the World Anti‐Doping Agency. Tandem mass spectrometry is often used in the pharmaceutical industry, clinical analysis laboratory, and antidoping laboratory for detection and characterization of drugs and their metabolites. A deeper chemical understanding of dissociation pathways may eventually lead to an improved ability to predict tandem mass spectra of compounds based strictly on their chemical structure (or vice versa), which is especially important for characterization of unknowns such as emerging designer drugs or novel metabolites. In addition to providing insights into dissociation pathways, the use of energy‐resolved breakdown curves can produce improved selectivity and lend insights into optimal fragmentation conditions for liquid chromatography‐tandem mass spectrometry LC–MS/MS workflows. Here, we perform energy‐resolved collision cell and multistage ion trap collision‐induced dissociation‐mass spectrometry (CID‐MS) experiments, along with complementary density functional theory calculations, on five beta blockers (acebutolol, atenolol, bisoprolol, carteolol, and labetalol), to better understand the details of the pathways giving rise to the observed MS/MS patterns. Results from this work are contextualized within previously reported literature on these compounds. New insights into the formation of the characteristic product ion m/z 116 and the pathway leading to characteristic loss of 77 u are highlighted. We also present comparisons of breakdown curves obtained via qToF, quadrupole ion trap, and in‐source CID, allowing for differences between the data to be noted and providing a step toward allowing for improved selectivity of breakdown curves to be realized on simple instruments such as single quadrupoles or ion traps.

show abstract

Section: Introductionmentioning

confidence: 99%

Further exploration of the collision‐induced dissociation of select beta blockers: Acebutolol, atenolol, bisoprolol, carteolol, and labetalol

Carlo,

Patrick

2023

J Mass Spectrom

View full text Add to dashboard Cite

show abstract

“…Multiple application notes have been published, including analysis of fat‐soluble vitamins, veterinary drugs, pesticides, and hormones, all using ammonium fluoride‐adjusted mobile phase systems 19–23,31 . Specifically, several application notes identify improved sensitivity for hormone measurement after switching to an ammonium fluoride‐based mobile phase system 21–23,32–35 . Internal efforts in developing a trace level analytical method for steroids showed an approximate 5‐10 fold improvement in sensitivity by replacing ammonium hydroxide with ammonium fluoride and making no other changes.…”

Section: Introductionmentioning

confidence: 99%

“…19 , 20 , 21 , 22 , 23 , 31 Specifically, several application notes identify improved sensitivity for hormone measurement after switching to an ammonium fluoride‐based mobile phase system. 21 , 22 , 23 , 32 , 33 , 34 , 35 Internal efforts in developing a trace level analytical method for steroids showed an approximate 5‐10 fold improvement in sensitivity by replacing ammonium hydroxide with ammonium fluoride and making no other changes. Additionally, recent publications describe sensitivity improvements by substituting ammonium fluoride as a mobile phase modifier (vs formic acid or ammonium acetate) in metabolism screening work.…”

Section: Introductionmentioning

confidence: 99%

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

McFadden,

Ames

2023

Analytical Science Advances

View full text Add to dashboard Cite

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+.

show abstract

Quantification of glucocorticoid and progestogen metabolites in bovine plasma, skimmed milk and saliva by UHPLC-HR-MS with polarity switching

Rehm,

Hankele,

Ulbrich

et al. 2024

Analytica Chimica Acta

View full text Add to dashboard Cite

Semi-automated serum steroid profiling with tandem mass spectrometry

Cited by 4 publications

References 35 publications

Further exploration of the collision‐induced dissociation of select beta blockers: Acebutolol, atenolol, bisoprolol, carteolol, and labetalol

Further exploration of the collision‐induced dissociation of select beta blockers: Acebutolol, atenolol, bisoprolol, carteolol, and labetalol

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

Quantification of glucocorticoid and progestogen metabolites in bovine plasma, skimmed milk and saliva by UHPLC-HR-MS with polarity switching

Contact Info

Product

Resources

About