GC/MS in Recent Years Has Defined the Normal and Clinically Disordered Steroidome: Will It Soon Be Surpassed by LC/Tandem MS in This Role?

Abstract

Gas chromatography/mass spectrometry (GC/MS) has been used for steroid analysis since the 1960s. The advent of protective derivatization, capillary columns, and inexpensive electron ionization bench-top single quadrupole soon made it the method of choice for studying disorders of steroid synthesis and metabolism. However, the lengthy sample workup prevented GC/MS from becoming routine for steroid hormone measurement, which was dominated by radioimmunoassay. It was the emergence of liquid chromatography/tandem MS (LC/MS/MS) that sparked a renewed interest in GC/MS for the multicomponent analysis of steroids. GC/MS is excellent at providing an integrated picture of a person's steroid metabolome, or steroidome, as we term it. We review the recent work on newly described disorders and discuss the technical advances such as GC coupling to triple quadrupole and ion trap analyzers, two-dimensional GC/MS, and alternative ionization and detection systems such as atmospheric pressure chemical ionization (APCI) and time of flight. We believe that no novel GC/MS-based technique has the power of GC(electron ionization)/MS/MS as a “discovery tool,” although APCI might provide ultimate sensitivity, which might be required in tissue steroidomics. Finally, we discuss the role of LC/MS/MS in steroidomics. This remains a challenge but offers shorter analysis times and advantages in the detection and discovery of steroids with a known structure. We describe recent advances in LC/MS steroidomics of hydrolyzed and intact steroid conjugates and suggest the technique is catching up with GC/MS in this area. However, in the end, both techniques will likely remain complementary and both should be available in advanced analytical laboratories.

Reference intervals for the urinary steroid metabolome: The impact of sex, age, day and night time on human adult steroidogenesis

“…by producing stable oxime-silyl-derivatives, and by the development of a derivative purification method based on lipophilic Sephadex in 1977 [9–11]. The long history of urinary steroid analysis and the current role of GC-MS in steroid analysis compared with other analytical techniques as LC-MS/MS were sufficiently addressed in detail elsewhere [12–15].…”

Conjugating immunoassays to mass spectrometry: Solutions to contemporary challenges in clinical diagnostics

“…Subsequent acceptance of gas chromatography-MS (GC-MS) for immunoassay validation in clinics lead to mainstream use of the more versatile liquid chromatography-MS (LC-MS) [ 17 , 18 , 20 ]. Despite its waning popularity due to the requirement for extensive sample preparation and often chemical derivatisation, GC-MS still has an important place in the clinical analysis of selected compounds such as excreted steroid metabolites [ 21 , 22 ].…”

Metabolomic Analysis Identifies Glycometabolism Pathways as Potential Targets of Qianggan Extract in Hyperglycemia Rats

“…It offers a powerful platform to investigate metabolic pathways, identify biomarkers for diagnosing and monitoring diseases, and predict therapeutic targets of drugs (Guo et al, 2018;Procopet et al, 2018). Gas chromatography-mass spectrometry (GC-MS), which possesses high resolution, sensitivity, and available database, is one of the powerful and popular tools in metabolomics studies (Shackleton et al, 2018). It has been extensively applied to assess the effects and explore metabolic mechanisms of TCM in treating diseases.…”