Abstract
HPLC hyphenated instrumentations are powerful tools for separation and structure identification of non-crystalline organic compounds on an analytical scale. Prominent among these is the high performance liquid chromatography–solid phase extraction–nuclear magnetic resonance (HPLC−SPE−NMR) hyphenation, which combines the strength of analytical resolution (HPLC), multiple peak trapping and single deuterated solvent used for NMR sampling (SPE), providing definitive information for structural elucidation (NMR, 1D and 2D). Our laboratory has utilized this technique in combination with HPLC−HRESIMS and HPLC−microfractionation−bioassay to explore the bioactive natural products and metabolites of bioactive compounds successfully. It should be addressed that appropriate sample pretreatment is very helpful to facilitate the subsequent optimization of HPLC conditions for well-resolved separation, which is critical to achieve successful application of HPLC−SPE−NMR analysis. In this chapter, the application of HPLC−SPE−NMR in characterization of polyphenols from Phyllanthus reticulatus, labile acylated flavonol monorhamnosides from Machilus philippinensis, lignans from P. myrtifolius and P. uriaria, stilbenoids from Syagrus romanzoffiana, and Amaryllidaceous alkaloids from Crinum asiaticum var. sinicum is described. These studies demonstrate that HPLC−SPE−NMR is very useful for thorough chemical investigation with the advantages of saving time, plant materials, and consumables over general methods.
Published Version
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