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Beetroot ( Beta vulgaris L.) is known for being a rich source of phytochemicals, minerals and vitamins. This study aims to show how the combination of extraction/chromatography/mass spectrometry and NMR offers an efficient way to profile metabolites in the extracts of beetroot. Such combination may lead to the identification of more nutritional or medicinal compounds in natural products, and it is essential for our ongoing investigation to study the selective adsorption/desorption of these metabolites' on/off nanoparticles. The aqueous and organic extracts underwent analyses using UV-vis spectroscopy; GC-MS; LC-MS; 1 H, 13 C, 31 P, TOCSY, HSQC, and selective TOCSY NMR experiments. Polar Extract: The two forms of betalain pigment were identified by UV-vis and LC MS. Fourteen amino acids, sucrose, and other compounds, among which is riboflavin, were identified by LC-MS. Two-dimensional TOCSY showed the spin coupling correlations corresponding to some of these compounds. The HSQC spectrum showed 1 H/ 13 C spin correlation in sucrose, confirming its high abundance in beetroot. Organic Extract: GC-MS data enabled the identification of several compounds including six fatty acid methyl esters (FAME) with higher than, on average, 90% similarity score. Selective TOCSY NMR data showed the spin coupling pattern corresponding to oleic, linoleic, and linolenic fatty acids. 31 P NMR spectra indicate that phospholipids exist in both the organic and aqueous phase.

Amphiphilic phospholipid-iodinated polymer conjugates were designed and synthesized as new macromolecular probes for a highly radiopaque and biocompatible imaging technology. Bioconjugation of PEG 2000-phospholipids and iodinated polyesters by click chemistry created amphiphilic moieties with hydrophobic polyesters and hydrophilic PEG units, which allowed their self-assemblies into vesicles or spiked vesicles. More importantly, the conjugates exhibited high radiopacity and biocompatibility in in vitro X-ray and cell viability measurements. This new type of bioimaging contrast agent with a Mn value of 11 289 g mol-1 was found to have a significant X-ray signal at 3.13 mg mL-1 of iodine equivalent than baseline and no cytotoxicity after 48 hours incubation of with HEK and 3T3 cells at 20 μM (20 picomoles) concentration of conjugates per well. The potential of adopting the described macromolecular probes for bioimaging was demonstrated, which could further promote the development of a field-friendly and highly sensitive bioimaging contrast agent for point-of-care diagnostic applications.

Polymer-inorganic nanocomposites based on polymer-grafted nanocrystals (PGNCs) are enabling technologically relevant applications owing to their unique physical, chemical, and mechanical properties. While diverse PGNC superstructures have been realized through evaporation-driven self-assembly, this approach presents multifaceted challenges in experimentally probing and controlling assembly kinetics. Here, we report a kinetically controlled assembly of binary superstructures from a homogeneous disordered PGNC mixture utilizing solvent vapor annealing (SVA). Using a NaZn 13 -type superstructure as a model system, we demonstrate that varying the solvent vapor pressure during SVA allows for exquisite control of the rate and extent of PGNC assembly, providing access to nearly complete kinetic pathways of binary PGNC crystallization. Characterization of kinetically arrested intermediates reveals that assembly follows a multistep crystallization pathway involving spinodal-like preordering of PGNCs prior to NaZn 13 nucleation. Our work opens up new avenues for the synthesis of multicomponent PGNC superstructures exhibiting multifunctionalities and emergent properties through a thorough understanding of kinetic pathways.