Micro extraction to quantitate spermidine and spermine in human urine and blood by matrix-assisted laser desorption ionization time-of-flight mass spectrometry

• Published in: Journal of Chromatography A Vol. 1326; pp. 1 - 6
• Main Authors: Lu, Chi-Yu, Su, Huai-Hsin, Chen, Yen-Ling, Tseng, Wei-Lung
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 24.01.2014; Elsevier
• Subjects: alkalinization; Biological and medical sciences; Blood; blood sampling; desorption; Human; Humans; Indicators and Reagents; Investigative techniques, diagnostic techniques (general aspects); Ionization; Lasers; liquid chromatography; Liquid Phase Microextraction; Liquid-liquid extraction; matrix-assisted laser desorption-ionization mass spectrometry; Medical sciences; Micro extraction; Miscellaneous. Technology; Monitors; organic wastes; Pathology. Cytology. Biochemistry. Spectrometry. Miscellaneous investigative techniques; protocols; Solvents; Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization - methods; Spermidine; Spermidine - blood; Spermidine - urine; Spermine; Spermine - blood; Spermine - urine; Urine; Urine; Spermine; Micro extraction; Spermidine; Blood; Human; Biological fluid; Polyamine; Chemical analysis; Healthy subject; Matrix assisted laser desorption ionization; Derivatization; Chemical enrichment; Analysis method; Sample preparation; Biogenic amine; Clinical biology; Liquid liquid microextraction; Time-of-flight mass spectrometers; Quantitative analysis
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2013.12.037

•Development of a fast MALDI-TOF MS method for spermidine and spermine quantitation.•Use of micro liquid–liquid extraction to concentrate spermidine and spermine.•Application of the proposed method to quantitate spermidine and spermine in urine and blood. Spermidine and its derivative, spermine, are basic compounds with unique roles in physiological function. This study used matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry (MS) to monitor these analytes in human urine and blood. The MALDI-TOF MS is also suitable when a high-throughput analytical method is required. Unlike liquid chromatography (LC)–MS, MALDI-TOF MS does not require a mobile phase in sample separation and generates very little organic waste. Micro liquid–liquid extraction was also performed to minimize the use of organic solvents in this study. After alkalization step, biosamples were prepared by adding a small volume (20μL) of organic solvent to concentrate, and purify the spermidine and spermine contained in the urine and blood samples. A suitable extraction protocol was developed after optimizing various conditions associated with extraction efficiency. The proposed method was then successfully used to monitor these compounds in human urine (mean value<1μg/mL) and blood (mean value>1μg/mL).