[Omeo33] Art 1063 - J Mol Liq, 2009, 144 (1-2), 32-39

[Gino Santini]

NMR water proton relaxation in unheated and heated ultrahigh aqueous  
dilutions of histamine: Evidence for an air-dependent supramolecular  
organization of water
Jean-Louis Demangeat

We measured 20-MHz R1 and R2 water proton NMR relaxation rates in  
ultrahigh dilutions (range 5.43 · 10− 8 M–5.43 · 10− 48 M) of  
histamine in water (Hist-W) and in saline (Hist-Sal), prepared by  
iterative centesimal dilutions under vigorous agitation in controlled  
atmospheric conditions. Water and saline were similarly and  
simultaneously treated, as controls. The samples were immediately  
sealed in the NMR tubes after preparation, and then code-labelled. Six  
independent series of preparations were performed, representing about  
7000 blind measurements. R2 exhibited a very broad scatter of values  
in both native histamine dilutions and solvents. No variation in R1  
and R2 was observed in the solvents submitted to the iterative  
dilution/agitation process. By contrast, histamine dilutions exhibited  
slightly higher R1 values than solvents at low dilution, followed by a  
slow progressive return to the values of the solvents at high  
dilution. Unexpectedly, histamine dilutions remained distinguishable  
from solvents up to ultrahigh levels of dilution (beyond 10− 20 in  
Hist-Sal). A significant increase in R2 with increased R2/R1 was  
observed in Hist-W. R1 and R2 were linearly correlated in solvents,  
but uncorrelated in histamine dilutions. After a 10-min heating/ 
cooling cycle of the samples in their sealed NMR tubes (preventing any  
modification of the chemical composition and gas content), all of the  
relaxation variations observed as a function of dilution vanished, the  
R2/R1 ratio and the scatter of the R2 values dropped in all solutions  
and solvents, and the correlation between R1 and R2 reappeared in the  
Hist-W samples. All these results pointed to a more organized state of  
water in the unheated samples, more pronounced in histamine solutions  
than in solvents, dependent on the level of dilution. It was suggested  
that stable supramolecular structures, involving nanobubbles of  
atmospheric gases and highly ordered water around them, were generated  
during the vigorous mechanical agitation step of the preparation, and  
destroyed after heating. Histamine molecules might act as nucleation  
centres, amplifying the phenomenon which was thus detected at high  
dilution levels.

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