Quantitative analysis of 6-hydroxymelatonin in human urine by gas chromatography-negative chemical ionization mass spectrometry

✍ Scribed by Masahiro Tetsuo; Sanford P. Markey; Robert W. Colburn; Irwin J. Kopin

• Publisher: Elsevier Science
• Year: 1981
• Tongue: English
• Weight: 653 KB
• Volume: 110
• Category: Article
• ISSN: 0003-2697
• DOI: 10.1016/0003-2697(81)90137-8

✦ Synopsis

A method for assay of urinary dhydroxymelatonin, the major metabolite of the pineal hormone melatonin is described. After addition of an internal standard of deuterated 6hydroxymelatonin sulfate, human mine was hydrolyzed enzymatically and free dhydroxymelatonin extracted, reacted to form a stable t-butyldimethylsilylpentafluoropropionyl derivative which was separated on silica gel column chromatography, and quantified using electron capture negative-ion chemical ionization mass spectrometry. Intrassay variability over an 18-h period was 5.4% [53.8 ng/3 ml urine f 2.94 (SD)] and interassay variability over a 2-week period was 2.1% 151.8 ng/3 ml urine f 1.08 (SD)].