LC-MS based simultaneous profiling of adrenal hormones of steroids, catecholamines, and metanephrines

Metabolic changes in adrenocortical steroids and medullary catecholamines characterize adrenal tumors, but they are measured using different analytical protocols. To increase bioanalytical validity while maintaining sample homogeneity, LC-MS-based profiling of 29 cortical steroids and 6 medullary am...

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Main Authors: Jongsung Noh, Chaelin Lee, Jung Hee Kim, Seung Woon Myung, Man Ho Choi
Format: Article
Language:English
Published: Elsevier 2023-11-01
Series:Journal of Lipid Research
Subjects:
Online Access:http://www.sciencedirect.com/science/article/pii/S0022227523001268
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author Jongsung Noh
Chaelin Lee
Jung Hee Kim
Seung Woon Myung
Man Ho Choi
author_facet Jongsung Noh
Chaelin Lee
Jung Hee Kim
Seung Woon Myung
Man Ho Choi
author_sort Jongsung Noh
collection DOAJ
description Metabolic changes in adrenocortical steroids and medullary catecholamines characterize adrenal tumors, but they are measured using different analytical protocols. To increase bioanalytical validity while maintaining sample homogeneity, LC-MS-based profiling of 29 cortical steroids and 6 medullary amines, including catecholamines and metanephrines, in a single run was developed. Alkyloxycarbonylation with isobutyl chloroformate was employed together with our comprehensive steroid assay, and all adrenal hormones were separated on a reversed-phase C18 column (50 × 2.1 mm, 1.9 μm) at a flow rate of 0.3 ml/min. The lower limits of quantification for all analytes ranged from 0.1 to 2.0 ng/ml, with extraction recoveries of 58.5%–109.5%, while the imprecision and accuracy were 1.6%–14.8% and 89.2%–114.9%, respectively. The validated LC-MS assay was applied to serum samples obtained from 60 patients with adrenal Cushing syndrome, primary aldosteronism, and pheochromocytoma/paraganglioma (PPGL). In addition to the characteristic metabolic changes in glucocorticoids, mineralocorticoids, catecholamines, and metanephrine, the molecular ratios of dehydroepiandrosterone sulfate and 20α-dihydrocortisol indicated Cushing syndrome and primary aldosteronism (P < 0.01 for all compounds), respectively. Moreover, the interactive molecular ratios of 11-deoxycortisol with normetanephrine, metanephrine, norepinephrine, and epinephrine (P < 0.01 all compounds) were proposed to characterize the metabolic features of PPGL. Novel LC-MS-based quantitative profiling of steroids, catecholamines, and metanephrines in human serum was successfully established and characterized metabolic features of individual adrenal tumors that could be used for clinical purposes.
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spelling doaj.art-d3b028095c0e492dac5ece6bb37351c42023-11-17T05:24:35ZengElsevierJournal of Lipid Research0022-22752023-11-016411100453LC-MS based simultaneous profiling of adrenal hormones of steroids, catecholamines, and metanephrinesJongsung Noh0Chaelin Lee1Jung Hee Kim2Seung Woon Myung3Man Ho Choi4Center for Advanced Biomolecular Recognition, Korea Institute of Science and Technology, Seoul, Korea; Department of Chemistry, Kyonggi University, Suwon, KoreaCenter for Advanced Biomolecular Recognition, Korea Institute of Science and Technology, Seoul, KoreaDepartment of Internal Medicine, Seoul National University College of Medicine, Seoul, KoreaDepartment of Chemistry, Kyonggi University, Suwon, KoreaCenter for Advanced Biomolecular Recognition, Korea Institute of Science and Technology, Seoul, Korea; For correspondence: Man Ho ChoiMetabolic changes in adrenocortical steroids and medullary catecholamines characterize adrenal tumors, but they are measured using different analytical protocols. To increase bioanalytical validity while maintaining sample homogeneity, LC-MS-based profiling of 29 cortical steroids and 6 medullary amines, including catecholamines and metanephrines, in a single run was developed. Alkyloxycarbonylation with isobutyl chloroformate was employed together with our comprehensive steroid assay, and all adrenal hormones were separated on a reversed-phase C18 column (50 × 2.1 mm, 1.9 μm) at a flow rate of 0.3 ml/min. The lower limits of quantification for all analytes ranged from 0.1 to 2.0 ng/ml, with extraction recoveries of 58.5%–109.5%, while the imprecision and accuracy were 1.6%–14.8% and 89.2%–114.9%, respectively. The validated LC-MS assay was applied to serum samples obtained from 60 patients with adrenal Cushing syndrome, primary aldosteronism, and pheochromocytoma/paraganglioma (PPGL). In addition to the characteristic metabolic changes in glucocorticoids, mineralocorticoids, catecholamines, and metanephrine, the molecular ratios of dehydroepiandrosterone sulfate and 20α-dihydrocortisol indicated Cushing syndrome and primary aldosteronism (P < 0.01 for all compounds), respectively. Moreover, the interactive molecular ratios of 11-deoxycortisol with normetanephrine, metanephrine, norepinephrine, and epinephrine (P < 0.01 all compounds) were proposed to characterize the metabolic features of PPGL. Novel LC-MS-based quantitative profiling of steroids, catecholamines, and metanephrines in human serum was successfully established and characterized metabolic features of individual adrenal tumors that could be used for clinical purposes.http://www.sciencedirect.com/science/article/pii/S0022227523001268adrenal tumorchemical derivatizationmass spectrometryadrenal cortexadrenal medullar
spellingShingle Jongsung Noh
Chaelin Lee
Jung Hee Kim
Seung Woon Myung
Man Ho Choi
LC-MS based simultaneous profiling of adrenal hormones of steroids, catecholamines, and metanephrines
Journal of Lipid Research
adrenal tumor
chemical derivatization
mass spectrometry
adrenal cortex
adrenal medullar
title LC-MS based simultaneous profiling of adrenal hormones of steroids, catecholamines, and metanephrines
title_full LC-MS based simultaneous profiling of adrenal hormones of steroids, catecholamines, and metanephrines
title_fullStr LC-MS based simultaneous profiling of adrenal hormones of steroids, catecholamines, and metanephrines
title_full_unstemmed LC-MS based simultaneous profiling of adrenal hormones of steroids, catecholamines, and metanephrines
title_short LC-MS based simultaneous profiling of adrenal hormones of steroids, catecholamines, and metanephrines
title_sort lc ms based simultaneous profiling of adrenal hormones of steroids catecholamines and metanephrines
topic adrenal tumor
chemical derivatization
mass spectrometry
adrenal cortex
adrenal medullar
url http://www.sciencedirect.com/science/article/pii/S0022227523001268
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