The newly developed experimental OPLC separation unit 100 (OSU 100) has been used for fully on-line multiple hyphenation using the one-channel flowing eluent wall (FEW) arrangement at the inlet. OSU 100-UV and OSU 100-DAD-ESI-MS with manual injector or autosampler were used to test the connected systems (OPLC-UV; OPLC-DAD-ESI-MS), using xanthine standards (caffeine, theophylline, theobromine) and green tea leaf extract as model compounds. The mobile phase chloroform-trifluoroacetic acid-acetonitrile-methanol, 76:4:6.67:13.33 (
) is suitable for rapid and selective separation, DAD, and ESI-MS of xanthines. The detection sensitivity of OPLC-UV or OPLC-DAD was increased by hyphenation with ESI-MS coupled in series. In contrast with DAD, the extracted ion chromatogram (
= 181.1 Da) after background subtraction yields readily measurable peaks from the small amounts of theophylline and theobromine in tea leaf extract. Analysis of xanthines was achieved within 10 min with less than 2 mL mobile phase. Owing to the openable adsorbent layer in OPLC the bed conditions can, moreover, be checked off-line after single or multiple fully online separations.
E. Tyihák, and G. Held
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