Abstract

A simple system for on-line sample extraction following reversed-phase high-performance liquid chromatographic ( HPLC) analysis is presented. The system can be used to prepare samples for direct probe insertion mass spectrometry ( MS), infrared analysis or other techniques. The extraction cell has also been used for continuous on-line HPLC-MS. The system is based on post-column chloroform extraction of the eluted compounds from polar mobile phases consisting of methanol or acetonitrile-0.1 M potassium dihydrogen orthophosphate buffer or water. The organic solvent is mixed with the column effluent using a commercially available post-column reaction device. The non-polar phase is separated by pressurized filtration through a Teflon membrane, which acts as a barrier to the aqueous portion of the eluent. The extracted solutes are detected using an ultraviolet spectrophotometer. A portion of the organic solvent that contains the eluted component can be collected easily, examined by other analytical techniques or, as will be shown, the solvent can be applied to a moving belt interface for introduction into a mass spectrometer. The system has been used for the extraction and detection of four model compounds (dimethyl, diethyl, diisobutyl and diamyl phthalate esters). The linear range of detection by on-line mass spectrometry was shown to extend to at least 1.2 μg of each ester.

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