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- W2069581904 abstract "A semipreparative HPLC setup was evaluated for automated fractionation with both photometric- and mass spectrometric trigger. The goals of the work were to systematically study and optimize the flow-splitting setup for mass-directed purifications by mathematical modeling and experimental verification. The system comprised a passive splitting device with make-up flow capability, which directed a small fraction of the column effluent to the mass spectrometer and the remainder to the fraction collector. Tubing lengths and diameters of the splitter as well as make-up flow rates were varied in order to address and optimize peak dispersion, delay times between mass detector and fraction collector, and mass spectrometric signal quality. A paraben standard mixture was analyzed and purified on both microparticulate and monolithic columns with 10 mm inner diameter and at typical flow rates of 5–10 mL/min. Fraction purities and recoveries close to 100% were achieved. The system allowed mass-triggered fractionations on a 1 mg scale at flow rates of 10 mL/min in combination with monolithic columns in less than 2 min. Finally, the system was successfully applied to the fully automated isolation of milligram quantities of degradation products in a pharmaceutical preparation to successfully allow for structure elucidation with NMR spectroscopy." @default.
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- W2069581904 date "2007-07-01" @default.
- W2069581904 modified "2023-09-25" @default.
- W2069581904 title "Automated semipreparative purification with mass spectrometric fraction collection trigger: Modeling and experimental evaluation of a setup employing passive splitting" @default.
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- W2069581904 doi "https://doi.org/10.1002/jssc.200700059" @default.
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