Liquid chromatography-tandem mass spectrometry assay for simultaneous quantification of catecholamines and metabolites in human plasma and cerebrospinal fluid

Catecholamines (CAs) and their metabolites in human cerebrospinal fluid (CSF) and plasma are potential biomarkers of Alzheimer's disease (AD) and facilitate early diagnosis. Liquid chromatography-tandem mass spectrometry is the gold standard method for analyzing CAs. The objective of this study...

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Main Authors: Yuting Wang, Quan Li, Yuhang Deng, Wenqing Wu, Cuiping Zhang, Yichi Zheng, Ming Guan, Haoqin Jiang
Format: Article
Language:English
Published: Elsevier 2025-07-01
Series:Practical Laboratory Medicine
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Online Access:http://www.sciencedirect.com/science/article/pii/S2352551725000241
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author Yuting Wang
Quan Li
Yuhang Deng
Wenqing Wu
Cuiping Zhang
Yichi Zheng
Ming Guan
Haoqin Jiang
author_facet Yuting Wang
Quan Li
Yuhang Deng
Wenqing Wu
Cuiping Zhang
Yichi Zheng
Ming Guan
Haoqin Jiang
author_sort Yuting Wang
collection DOAJ
description Catecholamines (CAs) and their metabolites in human cerebrospinal fluid (CSF) and plasma are potential biomarkers of Alzheimer's disease (AD) and facilitate early diagnosis. Liquid chromatography-tandem mass spectrometry is the gold standard method for analyzing CAs. The objective of this study was to develop and validate a liquid chromatography-tandem mass spectrometry assay capable of simultaneously quantifying dopamine (DA), epinephrine (E), norepinephrine (NE), metanephrine (MN), normetanephrine (NMN), and 3-methoxytyramine (3-MT) in both human CSF and plasma. Samples were processed by solid-phase extraction with a weak cation exchange adsorbent and then separated using an ultra-performance reversed-phase chromatography column. Analyte detection was performed using a triple quadrupole mass spectrometer operated in positive-ion multiple reaction monitoring mode. The developed assay was validated according to standard guidelines. The linearity, specificity, precision, accuracy, carryover and stability were assessed to ensure compliance with specified criteria. The lower limits of quantification for DA, E, NE, MN, NMN, and 3-MT were 4.5, 2.5, 4.5, 2.5, 2, and 0.3 pg mL−1, respectively. The total runtime for a single sample was 6.5 min. These results demonstrated that the method was sensitive, rapid, and reliable for the simultaneous quantification of DA, E, NE, MN, NMN, and 3-MT in clinical practice. We successfully detected CAs and their metabolites in plasma and CSF samples from patients with normal cognition and AD. This study demonstrates an efficient laboratory workflow for high-throughput analysis of CAs and their metabolites and lays a foundation for further studies on AD biomarkers.
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spelling doaj-art-e75451449cbc46f79f37e21970dbe5712025-08-20T03:46:49ZengElsevierPractical Laboratory Medicine2352-55172025-07-0145e0047110.1016/j.plabm.2025.e00471Liquid chromatography-tandem mass spectrometry assay for simultaneous quantification of catecholamines and metabolites in human plasma and cerebrospinal fluidYuting Wang0Quan Li1Yuhang Deng2Wenqing Wu3Cuiping Zhang4Yichi Zheng5Ming Guan6Haoqin Jiang7Department of Laboratory Medicine, Huashan Hospital, Fudan University, Shanghai, 200040, ChinaDepartment of Laboratory Medicine, Huashan Hospital, Fudan University, Shanghai, 200040, ChinaDepartment of Laboratory Medicine, Huashan Hospital, Fudan University, Shanghai, 200040, ChinaDepartment of Laboratory Medicine, Huashan Hospital, Fudan University, Shanghai, 200040, ChinaDepartment of Laboratory Medicine, Huashan Hospital, Fudan University, Shanghai, 200040, ChinaDepartment of Laboratory Medicine, Huashan Hospital, Fudan University, Shanghai, 200040, ChinaDepartment of Laboratory Medicine, Huashan Hospital, Fudan University, Shanghai, 200040, China; Huashan CSF Laboratory, Huashan Hospital, Fudan University, Shanghai, 200040, China; Corresponding author. Department of Laboratory Medicine, Huashan Hospital, Fudan University, Shanghai, 200040, China.Department of Laboratory Medicine, Huashan Hospital, Fudan University, Shanghai, 200040, China; Huashan CSF Laboratory, Huashan Hospital, Fudan University, Shanghai, 200040, China; Corresponding author. Department of Laboratory Medicine, Huashan Hospital, Fudan University, Shanghai, 200040, China.Catecholamines (CAs) and their metabolites in human cerebrospinal fluid (CSF) and plasma are potential biomarkers of Alzheimer's disease (AD) and facilitate early diagnosis. Liquid chromatography-tandem mass spectrometry is the gold standard method for analyzing CAs. The objective of this study was to develop and validate a liquid chromatography-tandem mass spectrometry assay capable of simultaneously quantifying dopamine (DA), epinephrine (E), norepinephrine (NE), metanephrine (MN), normetanephrine (NMN), and 3-methoxytyramine (3-MT) in both human CSF and plasma. Samples were processed by solid-phase extraction with a weak cation exchange adsorbent and then separated using an ultra-performance reversed-phase chromatography column. Analyte detection was performed using a triple quadrupole mass spectrometer operated in positive-ion multiple reaction monitoring mode. The developed assay was validated according to standard guidelines. The linearity, specificity, precision, accuracy, carryover and stability were assessed to ensure compliance with specified criteria. The lower limits of quantification for DA, E, NE, MN, NMN, and 3-MT were 4.5, 2.5, 4.5, 2.5, 2, and 0.3 pg mL−1, respectively. The total runtime for a single sample was 6.5 min. These results demonstrated that the method was sensitive, rapid, and reliable for the simultaneous quantification of DA, E, NE, MN, NMN, and 3-MT in clinical practice. We successfully detected CAs and their metabolites in plasma and CSF samples from patients with normal cognition and AD. This study demonstrates an efficient laboratory workflow for high-throughput analysis of CAs and their metabolites and lays a foundation for further studies on AD biomarkers.http://www.sciencedirect.com/science/article/pii/S2352551725000241CatecholamineMetanephrinePlasmaCerebrospinal fluidLiquid chromatography-tandem mass spectrometry
spellingShingle Yuting Wang
Quan Li
Yuhang Deng
Wenqing Wu
Cuiping Zhang
Yichi Zheng
Ming Guan
Haoqin Jiang
Liquid chromatography-tandem mass spectrometry assay for simultaneous quantification of catecholamines and metabolites in human plasma and cerebrospinal fluid
Practical Laboratory Medicine
Catecholamine
Metanephrine
Plasma
Cerebrospinal fluid
Liquid chromatography-tandem mass spectrometry
title Liquid chromatography-tandem mass spectrometry assay for simultaneous quantification of catecholamines and metabolites in human plasma and cerebrospinal fluid
title_full Liquid chromatography-tandem mass spectrometry assay for simultaneous quantification of catecholamines and metabolites in human plasma and cerebrospinal fluid
title_fullStr Liquid chromatography-tandem mass spectrometry assay for simultaneous quantification of catecholamines and metabolites in human plasma and cerebrospinal fluid
title_full_unstemmed Liquid chromatography-tandem mass spectrometry assay for simultaneous quantification of catecholamines and metabolites in human plasma and cerebrospinal fluid
title_short Liquid chromatography-tandem mass spectrometry assay for simultaneous quantification of catecholamines and metabolites in human plasma and cerebrospinal fluid
title_sort liquid chromatography tandem mass spectrometry assay for simultaneous quantification of catecholamines and metabolites in human plasma and cerebrospinal fluid
topic Catecholamine
Metanephrine
Plasma
Cerebrospinal fluid
Liquid chromatography-tandem mass spectrometry
url http://www.sciencedirect.com/science/article/pii/S2352551725000241
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