rGBA conformational changes monitored by intrinsic fluorescence
and tryptic digestion. (a) Melting temperature (Tm) determined by tryptophan fluorescence of rGBA in the
absence (control) or presence of saturating concentrations of inhibitors
IFG 1, CBE 2, fluoro 3, or
β-epoxide ABPs 4 and 5. Statistical
analysis of n = 3 experiments, two-way ANOVA (***, p < 0.001). (b) Tm determined
by circular dichroism of rGBA in the absence or presence of saturating
concentrations of inhibitors 2 and 4. Statistical
analysis of n = 2, two-way ANOVA (***, p < 0.001). (c) rGBA fluorescence spectra at λEX 295 nm in the absence of additives (black dashed line) with a maximum
λEM of 335 nm, in complex with CBE 2 (yellow) with a maximum λEM of 333 nm, with ABP 4 (green) with a maximum λEM of 332 nm, and
with ABP 5 (red) with a maximum λEM of
331 nm. (d) rGBA fluorescence spectra showing fluorescence quenching
by ABP 5 (red) with the appearance of an emission peak
at 610 nm and ABP 4 (green) with the emergence of an
emission peak at 515 nm. All measurements were done in 10 mM phosphate
buffer, 150 mM NaCl, pH 7.4. (e) Time-resolved analysis of the tryptic
digestion of rGBA in complex with IFG 1, CBE 2, fluoro 3, ABP 4, or ABP 5. (f) Quantification of rGBA band densitometry during tryptic digestion
in the absence (black dashed line) and presence of ABP 5 (red), ABP 4 (green), fluoro 3 (magenta),
CBE 2 (yellow), or IFG 1 (cyan). Duplicate
quantifications ± SD.