Generation of urinary steroid profiles in patients with adrenal incidentaloma using gas chromatography–mass spectrometry

Великанова, Л И; Стрельникова, Е. Г.; Объедкова, Е В; Krivokhizhina, N. S.; Shafigullina, Z R; Grigoryan, Karine; Поваров, В. Г.; Москвин, А. Л.

doi:10.1134/s1061934816070169

Cited by 9 publications

(2 citation statements)

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“…Процедура пробоподготовки состояла из 3 этапов: проведение гидролиза конъюгатов стероидов с помощью фермента сульфатазы, полученной от Helix pomatia, жидкостная экстракция аналитов и их последующая дериватизация. Метоксиамина гидрохлорид и 1-(триметилсилил)имидазол использовали в качестве дериватизирующих агентов [13].…”

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Study of urine steroid profiles by gas chromatography-mass spectrometry in patients with adrenocortical cancer in the course of treatment

et al. 2021

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Background: Adrenocortical carcinoma (ACC) is a rare and aggressive disease. There are only few studies evaluating the diagnostic value of gas chromatography-mass spectrometry (GC-MS) for detection of ACC recurrence after surgery. It is necessary to conduct an in-depth study to search for the most informative markers of the disease relapse.Aim: To study urine steroid metabolism by GC-MS during treatment to identify early signs of metastatic disease and relapse.Materials and methods: Thirty nine (39) ACC patients were examined before and after surgery, in the early postoperative period (< 1 year) and late postoperative period (at 2 to 5 years). Ten (10) patients were disease-free at less than 1 year after surgery. Twenty nine (29) patients had metastases in lungs and other organs: 14, within 1 year after surgery, and 15, at 2 to 5 years. The control group included 25 patients with nonfunctioning adrenocortical adenomas (NAA) without malignant characteristics at histological examination. Urine steroid profiles were assessed with a gas chromatograph-mass spectrometer Shimadzu GCMS-QP2020.Results: As assessed by GC-MS, 16 major ACC biomarkers were found before surgery, including etiocholanolone, dehydroepiandrosterone (DHEA) and its metabolites, pregnanediol, pregnanetriol, 5-ene-pregnenes, and tetrahydro-11-deoxycortisol (THS). Their urine excretion was increased compared to that in the patients with NAA (р < 0.002). A non-classic 5-ene-pregnene, 3β,16,20-pregnenetriol (3β,16,20-dP3), was identified, with its urine excretion of > 500 mcg/day that was typical for ACC patients. After surgery, decreased urinary excretion of THS (р < 0.0001) and 3β,16,20-dP3 (р < 0.0001), increased 3α,16,20-dP3/3β,16,20-dP3 ratio (р = 0.003), compared to those before surgery, were indicative of the absence of any metastases. No difference of urine THS excretion and 3α,16,20-dP3/3β,16,20-dP3 ratio from the corresponding values before surgery (p > 0.05) is a sign of metastatic diseases in the ACC patients at less than 1 year after the surgery, of the disease relapse at 2 to 5 years, and of the disease relapse after chemotherapy. In addition, in the ACC patients with metastatic disease within 1 year after surgery, increased progestogen urine excretion was found. Urine excretion of DHEA and its metabolites in the patients with the disease relapse after chemotherapy was not different from those in the ACC patients before surgery (p > 0.05).Conclusion: Determination of urine excretion of THS, DHEA and its metabolites, etiocholanolone, 5-ene-pregnenes, 3β,16,20-dP3, and 3α,16,20-dP3/3β,16,20-dP3 ratio by GC-MS is of utmost importance in the monitoring of treatment for ACC and early diagnosis of the disease progression.

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Study of urine steroid profiles by gas chromatography-mass spectrometry in patients with adrenocortical cancer in the course of treatment

et al. 2021

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“…Nevertheless, LC-MS(/MS) also has disadvantages such as limited chromatographic resolution and detection by electrospray ionization (ESI) mass spectra, that contain limited structural information due to low fragmentation rates [13,18]. In these aspects GC-MS cannot be replaced by LC-MS, since its high chromatographic resolution and the option for recording information-rich electron ionization (EI) mass spectra makes GC-MS a powerful tool for untargeted analyses and steroid profiling [13,[16][17][18][19]. In particular, EI mass spectra of derivatives like sterol trimethylsilyl (TMS) ethers and methyloxime-trimethylsilyl (MO-TMS) ethers provide considerable structural information which can help to identify unknown steroidal analytes and can be used for suspected-target screening [18,20,21].…”

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Comparison of Strategies for the Determination of Sterol Sulfates via GC-MS Leading to a Novel Deconjugation-Derivatization Protocol

et al. 2019

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Sulfoconjugates of sterols play important roles as neurosteroids, neurotransmitters, and ion channel ligands in health and disease. In most cases, sterol conjugate analysis is performed with liquid chromatography-mass spectrometry. This is a valuable tool for routine analytics with the advantage of direct sterol sulfates analysis without previous cleavage and/or derivatization. The complementary technique gas chromatography-mass spectrometry (GC-MS) is a preeminent discovery tool in the field of sterolomics, but the analysis of sterol sulfates is hampered by mandatory deconjugation and derivatization. Despite the difficulties in sample workup, GC-MS is an indispensable tool for untargeted analysis and steroid profiling. There are no general sample preparation protocols for sterol sulfate analysis using GC-MS. In this study we present a reinvestigation and evaluation of different deconjugation and derivatization procedures with a set of representative sterol sulfates. The advantages and disadvantages of trimethylsilyl (TMS), methyloxime-trimethylsilyl (MO-TMS), and trifluoroacetyl (TFA) derivatives were examined. Different published procedures of sterol sulfate deconjugation, including enzymatic and chemical cleavage, were reinvestigated and examined for diverse sterol sulfates. Finally, we present a new protocol for the chemical cleavage of sterol sulfates, allowing for simultaneous deconjugation and derivatization, simplifying GC-MS based sterol sulfate analysis.

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Gas Chromatography–Mass Spectrometry Analysis of Urinary Steroid Metabolomics for Detection of Early Signs of Adrenal Neoplasm Malignancy in Patients with Cushing’s Syndrome

et al. 2019

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Generation of urinary steroid profiles in patients with adrenal incidentaloma using gas chromatography–mass spectrometry

Cited by 9 publications

References 9 publications

Study of urine steroid profiles by gas chromatography-mass spectrometry in patients with adrenocortical cancer in the course of treatment

Study of urine steroid profiles by gas chromatography-mass spectrometry in patients with adrenocortical cancer in the course of treatment

Comparison of Strategies for the Determination of Sterol Sulfates via GC-MS Leading to a Novel Deconjugation-Derivatization Protocol

Gas Chromatography–Mass Spectrometry Analysis of Urinary Steroid Metabolomics for Detection of Early Signs of Adrenal Neoplasm Malignancy in Patients with Cushing’s Syndrome

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