Ultra sensitive measurement of endogenous epinephrine and norepinephrine in human plasma by semi-automated SPE-LC-MS/MS

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• 作者：Guodong Zhang ; Yizhong Zhang ; Chengjie Ji ; Thomas McDonald ; Justin Walton ; Elizabeth A. Groeber ; Rick C. Steenwyk ; Zhaosheng Lin ; ^{lin905@gmail.com}
• 关键词：Catecholamines ; Epinephrine ; Norepinephrine ; Alumina SPE ; Human plasma ; Biomarker ; LC&ndash ; MS/MS
• 刊名：Journal of Chromatography B ; Analytical Technologies in the Biomedical and Life Sciences
• 出版年：2012
• 期刊代码：124_15700232
• 类别：ch
• 出版时间：1 May, 2012
• 卷：895-896
• 期：Complete
• 页码：186-190
• 文件大小：473 K

摘要

Measurement of endogenous epinephrine (E) and norepinephrine (NE) in human plasma is very challenging due to lower endogenous concentrations as compared with animal plasma. An LC-MS/MS in combination with alumina-based SPE and derivatization procedure was validated for the measurement of E and NE in human plasma with acceptable intra-day and inter-day accuracy and precision. Sample was extracted with semi-automated alumina 96-well solid phase extraction (SPE) cartridge. The resulting eluent was dried and derivatized using d4-acetaldehyde. The analytes were separated on a monolithic C₁₈ column. Extraction efficiencies were >66%for E and NE. The lower limit of quantitation (LLOQ) was 5.00 pg/mL for E and 20.0 pg/mL for NE.