Capillary-HPLC-NMR

The instrumental setup for capillary HPLC-NMR coupling is shown in Figure 4.6. The capillary pump is connected via 50 pm capillaries between the capillary HPLC pump, the UV detector, and the NMR flow probe. 

FIGURE 4.6 Instrumental setup for capillary HPLC-NMR coupling. (From Hentschel, P. et al., J. Chromatogr. A, 285, 2006. With permission.)... 

Hentschel, P, Krucker, M., Grynhaum, M. D., Putzhach, K., Bischoff, R., and Albert, K., Determination of regulatory phosphorylation sites in nanogram amounts of a synthetic fragment of ZAP-70 using microprohe NMR and on-hne coupled capillary HPLC-NMR, Magnetic Resonance in Chemistry 43(9), 747-754, 2005. 

The specific constraints and requirements of continuous-flow NMR will be explained in the first chapter, whereas specific applications, such as biomedical and natural product analysis, LC-NMR-MS and LC-NMR in an industrial environment, together with polymer analysis, will be discussed separately. Thus, the reader will obtain a broad overview of the application power of LC-NMR and the benefits of its use. He/She will also be introduced to the pitfalls of this technique. Special attention will be given to the exciting newer coupled techniques such as SFC-NMR and capillary HPLC-NMR. However, new emerging future developments will also be discussed thoroughly. 

Olson, D. L. Trace Analysis Using Capillary HPLC-NMR, presented at the 2nd SMASH NMR Conference, Argonne, IL, 2000. 

Practical Realization of Analytical HPLC-NMR and Capillary-HPLC-NMR... 

Fig. 2. Capillary-HPLC-NMR system with solenoidal micro flow probe (1.5 pL active detection volume).

Figure 6 depicts the contour plot of a capillary-HPLC-NMR separation of unsaturated fatty acid methyl esters. The injected sample amoimt was about 1-2 pg. As a representative example, Fig. 7 shows the capillary H NMR spectrum of eicosenic acid methyl ester. 

Fig. 6. Capillary-HPLC-NMR contour plot of four unsaturated fatty acid methyl esters ...

Behnke B, Schlotterbeck G, Tallarek U, et al. (1996) Capillary HPLC-NMR coupling high resolution NMR spectroscopy in the nanoliter scale. Analytical Chemistry 68 1110-1115. 

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