Determination of the low concentrations (less than 10-100 pg ml-1) of melatonin in blood plasma by gas chromatography/mass spectrometry has previously required the use of negative ionization (electron capture) mass spectrometry, a technique particularly delicate to set up. We show that a general-purpose medium-resolution instrument gives adequate sensitivity in electron impact mode, when used with a capillary gas chromatographic column-switching device. A straightforward extraction procedure gives good specificity, and the limit of useful measurement is better than 10 pg per 1 ml sample.

Installation of a Commercially available capillary-to-capillary column switching system in an otherwise unmodified gas chromatographhass spectrometer instrument is described. The first column is monitored via the jet separator, the second being connected directly to the ion source. This arrangement obviates the need for an auxiliary detector. A single gas chromatographic oven is adequate for many purposes.