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NMR Spectroscopy Lab Report

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NMR spectroscopy is a very good tool for structure elucidation of natural siderophores after purification. This experiment depend on the quantum mechanical property of a nucleus the spin. 1H, 13C, and 15N nuclei have two different spin states (energy low and high states with a half spin numbers). 1H is resonate at a four times higher frequency than 13C, and ten times higher than 15N nuclei. Therefore the nuclei are represented by characteristic resonance frequencies in an NMR spectrum. Metals are usually removed from the sample prior to record NMR, because paramagnetic iron (III) causes the line broadening of the NMR signals. The diamagnetic Al3+ or Ga3+ are used for in case of siderophore in the metal complexed form. 2D NMR technique is a very powerful tool where the 1D NMR …show more content…

Various two dimensional pulse sequences has been created providing both increased resolution and correlations that are easy to analyze the siderophore. A resonance in the 2D-NMR spectrum represents a pair of nuclei that interact with each other either scalar or through bond. The skeletal structures of siderophores can be deduced by number of 2D NMR experiments. 1H-1H homonuclear correlation spectrum combined with one-bond and 13C-1H correlation spectrum allow determining the fragments. Furthermore, the long-range 13C-1H correlation links those fragments to build the planar structure of the molecule under study. The homonuclear 2D 1H-1H COSY (correlation spectroscopy) experiment is used to identify the protons which are directly coupled to each other. The basic COSY-90 is the most widely used experiment while its minor variant COSY-45 sequence is acquired in order to distinguish geminal and vicinal proton pairs with less sensitivity than the previous one. Another significantly used experiment DEPT is to detect the proton

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