Fluorescence and NMR characterization and biomolecule entrapment studies of sol-gel-derived organic-inorganic composite materials formed by sonication of precursors
Jd. Brennan et al., Fluorescence and NMR characterization and biomolecule entrapment studies of sol-gel-derived organic-inorganic composite materials formed by sonication of precursors, CHEM MATER, 11(7), 1999, pp. 1853-1864
Optically clear sol-gel-derived organic-inorganic hybrid materials were pre
pared by a sonication method suitable for entrapment of biological compound
s. Sonication at pH 2.5 hydrolyzed mixtures of tetraethyl orthosilicate (TE
OS) and one of the organosilanes methyltriethoxysilane (MTES), propyltrimet
hoxysilane (PTMS), or dimethyldimethoxysilane (DMDMS). Buffer solutions con
taining the fluorescent probes 7-azaindole or prodan, or the proteins human
serum albumin (HSA) or lipase, were then added to promote gelation and the
resulting materials were aged at 4 degrees C over several months. The opti
cal clarity, hardness, and degree of cracking were examined, in conjunction
with solid-state Si-29 and C-13 NMR of the materials and fluorescence spec
tra of the entrapped probes. These studies revealed that MTES can be added
to TEOS up to a level of 20% (v/v) with retention of good physical characte
ristics, thus allowing control over the hydrophobicity and cross-linking wi
thin the matrix. Materials with more than 20% MTES, or incorporating PTMS o
r DMDMS at levels above 5%, showed significantly poorer physical characteri
stics, indicating phase separation. Proteins entrapped into these hybrid. m
aterials could be-examined by optical methods. Both entrapped HSA and lipas
e showed improvements in function with increased ormosil content, indicatin
g that such materials are suitable for encapsulation of lipophilic proteins
for optical sensor development.