Development and validation of a liquid chromatography–tandem mass spectrometry method for the simultaneous analysis of androgens, estrogens, glucocorticoids and progestagens in human serum

Iannone, Michele; Dima, Anna Pia; Sciarra, Francesca; Botrè, Francesco; Isidori, Andrea M.

doi:10.1002/bmc.5344

Cited by 11 publications

(4 citation statements)

References 56 publications

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“…To circumvent the confusion deriving from the addition of atoms common to the elemental composition of the CERs lipid class and minimize misidentification errors, we evaluated the effects of adding a different eluent additive. Given to the advantages in the ionization of hydrophobic compounds with NH 4 F ammonium fluoride described in the literature 24 , we explored the effects of adding NH 4 F in our analytical conditions and compared the performance with that obtained with NH 4 COOH. To compare the two chromatographic conditions, which are detailed in the materials and methods, we studied the ionization behavior of the deuterated d31-Cer[NS]34:1 lipid reference.…”

Section: Resultsmentioning

confidence: 99%

“…We have compared NH 4 COOH, which is one of the most common modifiers in metabolomic and lipidomic analyses, with NH 4 F, due to its increasing use in LCMS workflows more recently. We have tested the concentration that of NH 4 F that is typically used for hydrophobic compounds 24 . With NH 4 COOH we observed increased complexity and ambiguities linked to the elemental composition of some CERs.…”

Section: Discussionmentioning

confidence: 99%

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Comparison between ammonium formate and ammonium fluoride in the analysis of stratum corneum lipids by reversed phase chromatography coupled with high resolution mass spectrometry

Maiellaro,

Bottillo,

Cavallo

et al. 2024

Sci Rep

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Lipids are key constituents of the barrier function in the human stratum corneum (SC), which is the outermost layer of the epidermis and amenable to non-invasive sampling by tape stripping. The three major lipid classes in the SC, i.e., ceramides, fatty acids, and cholesterol, present equimolar concentration. Liquid chromatography coupled with mass spectrometry (LCMS) is elective in profiling lipids in the SC in both positive and negative ion modes. Nevertheless, the latter one allows for the simultaneous detection of the three major epidermal components of the SC. Determination of ceramides in the SC poses analytical challenges due to their wide range of structures and concentrations especially in the case of limited sample amounts. Ammonium formate is a commonly used modifier added to the mobile phase to assist ionization. However, it introduces uncertainty in the identification of ceramides when operating in negative ion mode, even with high resolution MS. We tested the advantages of using fluoride in the lipid profiling of SC and unambiguous identification of ceramides subclasses. The use of fluoride enhanced the ionization of ceramides, regardless the specific substructure, solved misidentification issues, and was successfully applied to the simultaneous detection of all three lipid classes in the human SC.

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Section: Resultsmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

Comparison between ammonium formate and ammonium fluoride in the analysis of stratum corneum lipids by reversed phase chromatography coupled with high resolution mass spectrometry

Maiellaro,

Bottillo,

Cavallo

et al. 2024

Sci Rep

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show abstract

“…High-sensitivity measurement of testosterone, free testosterone, and dehydroepiandrosterone and its sulfate was carried out by liquid chromatography with tandem mass spectrometry (LC-MS/MS; see table S4) ( 35 ). Baseline androgen concentrations were not directly correlated with treatment-related changes in cardiac torsion or strain (table S5).…”

Section: Resultsmentioning

confidence: 99%

Sex-specific effects of daily tadalafil on diabetic heart kinetics in RECOGITO, a randomized, double-blind, placebo-controlled trial

et al. 2022

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Cyclic GMP–phosphodiesterase type 5 (PDE5) inhibition has been shown to counteract maladaptive cardiac changes triggered by diabetes in some but not all studies. We performed a single-center, 20-week, double-blind, randomized, placebo-controlled trial (NCT01803828) to assess sex differences in cardiac remodeling after PDE5 inhibition in patients with diabetic cardiomyopathy. A total of 122 men and women (45 to 80 years) with long-duration (>3 years) and well-controlled type 2 diabetes mellitus (T2DM; HbA1c < 86 mmol/mol) were selected according to echocardiographic signs of cardiac remodeling. Patients were randomly assigned (1:1) to placebo or oral tadalafil (20 mg, once daily). The primary outcome was to evaluate sex differences in cardiac torsion change. Secondary outcomes were changes in cardiovascular, metabolic, immune, and renal function. At 20 weeks, the treatment-by-sex interaction documented an improvement in cardiac torsion (−3.40°, −5.96; −0.84, P = 0.011) and fiber shortening (−1.19%, −2.24; −0.14, P = 0.027) in men but not women. The primary outcome could not be explained by differences in cGMP concentrations or tadalafil pharmacodynamics. In both sexes, tadalafil improved hsa-miR-199-5p expression, biomarkers of cardiovascular remodeling, albuminuria, renal artery resistive index, and circulating Klotho concentrations. Immune cell profiling revealed an improvement in low-grade chronic inflammation: Classic CD14 ++ CD16 − monocytes reduced, and Tie2 + monocytes increased. Nine patients (14.5%) had minor adverse reactions after tadalafil administration. Continuous PDE5 inhibition could offer a strategy to target cardiorenal complications of T2DM, with sex- and tissue-specific responses. Further studies are needed to confirm Klotho and hsa-miR-199-5p as markers for T2DM complications.

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“…Several sophisticated techniques, such as next generation sequencing, mass spectrometry, and biosensors/nanosensors, are currently used to analyze circulating microbiomes and their metabolites. Mass spectrometry-based metabolomics constitutes an innovative approach to the detection and characterization of small molecules [ 94 ] and microbiome-synthesized metabolites [ 95 ]. Furthermore, the knowledge of a specific metabolomic signature represents relevant information that allows for the identification of bacterial sources [ 96 ].…”

Section: Microbial Metabolites Identification In Diseasementioning

confidence: 99%

The Diagnostic Potential of the Human Blood Microbiome: Are We Dreaming or Awake?

Sciarra

Franceschini

Campolo

et al. 2023

IJMS

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Human blood has historically been considered a sterile environment. Recently, a thriving microbiome dominated by Firmicutes, Actinobacteria, Proteobacteria, and Bacteroidetes phyla was detected in healthy blood. The localization of these microbes is restricted to some blood cell populations, particularly the peripheral blood mononuclear cells and erythrocytes. It was hypothesized that the blood microbiome originates from the skin–oral–gut axis. In addition, many studies have evaluated the potential of blood microbiome dysbiosis as a prognostic marker in cardiovascular diseases, cirrhosis, severe liver fibrosis, severe acute pancreatitis, type 2 diabetes, and chronic kidney diseases. The present review aims to summarize current findings and most recent evidence in the field.

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Development and validation of a liquid chromatography–tandem mass spectrometry method for the simultaneous analysis of androgens, estrogens, glucocorticoids and progestagens in human serum

Cited by 11 publications

References 56 publications

Comparison between ammonium formate and ammonium fluoride in the analysis of stratum corneum lipids by reversed phase chromatography coupled with high resolution mass spectrometry

Comparison between ammonium formate and ammonium fluoride in the analysis of stratum corneum lipids by reversed phase chromatography coupled with high resolution mass spectrometry

Sex-specific effects of daily tadalafil on diabetic heart kinetics in RECOGITO, a randomized, double-blind, placebo-controlled trial

The Diagnostic Potential of the Human Blood Microbiome: Are We Dreaming or Awake?

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