[ Pobierz całość w formacie PDF ]
.M., Spraul, M., Hofmann, M., Troke, J., Sanderson,P.N., Lindon, C., Wilson, I.D.and Nicholson, J.K., Anal.Chem., 1996, 68, 106.45.Korhammer, S.A.and Bernreuther, A., Fresenius J.Anal.Chem., 1996, 354, 131.46.Pursch, M.Strohschein, S., Händel, H.and Albert, K., Anal.Chem., 1996, 68, 386.47.Albert, K., Analusis, 1996, 24, M17.48.Höltzel, A., Schlotterbeck, G., Albert, K.and Bayer, E., Chromatographia, 1996, 42,499.49.Godejohann, M., Mügge, C., Wünsch, G.and Preiss, A., Anal.Chem., 1997, 69,3832.50.Sidelmann, U.G., Braumann, U., Hofmann, M., Spraul, M., Lindon, J.C., Nichol-son, J.K.and Hansen, S.H., Anal.Chem., 1997, 69, 607.51.Lindon, J.C., Nicholson, J.K., Sidelmann, U.G.and Wilson, I.D., Drug M etab.Rev., 1997, 29, 705.52.Strohschein, S., Pursch, M., Händel, H., and Albert, K., Fresenius J.Anal.Chem.,1997, 357, 498.53.Strohschein, S., Schlotterbeck, G., Richter, J., Pursch, M., Tseng, L.-H., Händel, H.and Albert, K., J.Chromatogr., A, 1997, 765, 207.54.Godejohann, M., Mügge, C.and Preiss, A., Anal.Chem., 1998, 70, 590.55.Strohschein, S., Pursch, M., Lubda, D.and Albert, K., Anal.Chem., 1998, 70, 13.56.Albert, K., in Analytiker-Taschenbuch 20, H.Günzler, (Ed.), Springer-Verlag,Berlin, 1998, pp.107 139.57.de Koning, J.A., Hogenboom, A.C., Lacker, T., Strohschein, S., Albert, K.andBrinkman, U.A.Th., J.Chromatogr., A, 1998, 813, 55.58.Dachler, M., Kohler, K.and Albert, K., J.Chromatogr., B, 1998, 720, 211.59.Wilson, I.D., Morgan, E.D., Lafont, R., Shockcor, J.P., Lindon, J.C., Nicholson,J.K.and Wright, B., Chromatographia, 1999, 49, 375.60.Strohschein, S., Rentel, C., Lacker, T., Bayer, E.and Albert, K., Anal.Chem., 1999,71, 1780.61.Albert, K., J.Chromatogr., A, 1999, 856, 199. 22 LC NMR and Related Techniques62.Albert, K., Dachtler, M., Händel, H., Lacker, T., Schlotterbeck, G., Strohschein, S.Tseng, L.-H.and Braumann, U., J.High Resol.Chrom., 1999, 22, 135.63.Albert, K., in NM R Spectroscopy in Drug Development and Analysis, U.Holzgrabe,I.Wawer and B.Diel (Eds), Wiley-VCH, Weinheim, 1999, pp.102 118.64.Pusecker, K., Albert, K.and Bayer, E., J.Chromatogr., A, 1999, 836, 245.65.Strohschein, S., Pursch, M.and Albert, K., J.Pharm.Biomed.Anal., 1999, 21, 669.66.Dachtler, M., Glaser, T., Händel, H., Lacker, T., Tseng, L.-H.and Albert K.,in Encyclopedia of Separation Science, Vol.II, Academic Press, London, 2000, pp.747 760.67.Vilegas, W., Vilegas, J.H.Y., Dachtler, M., Glaser, T.and Albert, K., Phytochem.Anal., 2000, 11, 317.68.Santos, L.C., Dachtler, M., Andrade F.D.P., Albert, K.and Vilegas, W., FreseniusJ.Anal.Chem., 2000, 368, 540.69.Tseng, L.-H., Braumann, U., Godejohann, M., Lee, S.-S.and Albert, K., J.Chin.Chem.Soc., 2000, 47, 1231.70.Dachtler, M., Glaser, T., Kohler, K.and Albert, K., Anal.Chem., 2001, 73, 667. 2 LC NMR: AutomationULRICH BRAUMANN and MANFRED SPRAULBruker BioSpin GmbH, Rheinstetten, Germany2.1 PRACTICAL USE OF LC NMR AND LC NMR/MSThe coupling of LC (liquid chromatography) with NMR (nuclear magneticresonance) spectroscopy can be considered now to be a standard analyticaltechnique.Today, even more complex systems, which also include mass spec-trometry (MS), are used.The question arises as to how such systems are handledefficiently with an increasing cost and a decreasing availability of skilled per-sonal.LC NMR and LC NMR/MS combine the well-established techniques ofLC, NMR and MS.For each of those techniques, various automation proced-ures and software packages are available and used in analytical laboratories.However, due to the necessary interfacing of such techniques, completely newdemands occur and additional problems have to overcome.In the first section of this review the possible types of experiments and theirapplication fields will be described, while in the second section the individualsteps of those experiments and the possibility of how to perform these tasksautomatically will be discussed.2.2 DIFFERENT WORKING MODES IN LC NMRThe theoretical basics of LC NMR coupling have already been discussed in theprevious chapter.Except for one type of experiment, the connection of thechromatographic system and the NMR detection cell via a capillary is notsufficient.Most of the experiments require a special interface with switchingvalves under software control for reliable and reproducible results.The level ofequipment and the application field depends on the types of experiment whichare being conducted and will be discussed in the following.The working modes can be first of all differentiated by the status of the sampleduring the measurement.First, it can be measured while the chromatographicseparation is continuing
[ Pobierz całość w formacie PDF ]