A small cage-like molecule (2) composed of three aminomethyl pyrroles and two hexa-substituted benzenes has been prepared by reduction of its iminopyrrole analogue (1) using NaBH₄. It was revealed by ¹H NMR spectroscopic analyses that cage molecule 2 strongly binds the fluoride anion in polar DMSO-d₆ relative to CDCl₃. Compared to that of compound 1, the lowered affinity of 2 for the fluoride anion is attributable to its increased electron density resulting from the production of thesecondary amine groups.

Antifreeze proteins (AFPs) bind to the ice crystals and then are able to inhibit the freezing of body fluid at subzero temperatures. Type III AFPs are categorized into three subgroups, QAE1, QAE2, and SP isoforms, based on differences in their isoelectric points. We prepared the QAE2 (AFP11) and SP (AFP6) isoforms of the notched-fin eelpout AFP and their mutant constructs and determined their temperature gradients of amide proton chemical shifts (𝚫δ/𝚫T) using NMR. The nfeAFP11 (QAE2) has the distinct 𝚫δ/𝚫T pattern of the first 3₁₀ helix compared to the QAE1 isoforms. The nfeAFP6 (SP) has the deviated 𝚫δ/𝚫T values of many residues, indicating its backbone conformational distortion. The study suggests the distortion in the H-bonding interactions and backbone conformation that is important for TH activities.

The baseline flattened NMR spectrum has been achieved by several methodologies including pulse manipulation with a series of phase cycling. The background signal inherent in the probe is also main source of baseline distortion both in solution and solid NMR. The simple direct polarization with 90° pulse flipping the magnetization from the z-axis onto the receiver coil requires the strong rf pulse enough to encompass the wide frequency range to excite the resonance of interest nuclei. Albeit the perfect polarization 90° pulse, the signal from the unwanted magnetic fields such as background signal can not be completely suppressed by suitable phase cycling. Moreover, slowly baseline wiggling signal from the low 𝛾 nuclei is not easy to eliminate with multiple pulse manipulation. So there is still need to contrive the new scheme for that purpose in an adroit manner. In this article new triple pulse excitation schemes for TIP and modified DEPTH pulse sequence are analytically examined in terms of arbitrary phase and flip angle of pulse. The suitable phase cycling for these pulse trains is necessary for the good sensitivity and resolution of the spectrum. It is observed that the ¹³C sensitivity TIP experiment is almost equal to the CP/MAS with modified DEPTH sequence, both of which are applicable to both solid and solution state NMR.

Benzo[a]pyrene (BaP), one of the polycyclic aromatic hydrocarbons (PAHs), is an endocrine disruptor and carcinogenic. This study was conducted to investigate the metabolic changes of zebrafish short-term exposure to BaP using nuclear magnetic resonance (NMR) spectroscopy. In our results, the multivariate analysis showed that the metabolic responses were differed according to the exposure concentration. Also, it was observed that exposure to high concentration of BaP (162 ㎍/L and 1620 ㎍/L) increased the levels of creatine, histidine, and inosine in zebrafish, which means high concentration of BaP exposure affected the energy metabolism and immune function in zebrafish.

Protein structure determination using NMR spectroscopy requires a suite of heteronuclear 3-D NMR experiments that can take a couple of weeks for completion. During the experiments, protein samples may suffer from slow degradation due to co-purifying proteases, which complicates and slows down the assignment procedure. Here we describe a practical protocol to avoid unwanted proteolysis during the experiment.