The enzymatic degradation of silk by protease XIV has been investigated by using scanning electron microscopy (SEM), Fourier transfer infrared spectroscopy (FTIR), solid-state 13C nuclear magnetic resonance of cross-polarization/magic angle spinning (13C CP/MAS solid state NMR) and electron paramagnetic resonance (EPR). Micro-morphology of protease XIV aged samples showed that microfilaments were stripped out from the surface of silk fibers. The results of FTIR and 13C CP/MAS solid-state NMR indicated that the enzymatic degradation process could be divided into two stages. The EPR spectra indicated that the enzymatic degradation process was related to the free radical with the g-factor value of 2.0043. We also proposed that at the first degradation stage, the free radicals were apt to lose activities due to the loose structure of the non-crystalline region; at the second degradation stage, the free radicals produced in the crystalline region tended to be stored.
Keywords: 13C CP/MAS solid state NMR; EPR; Enzymatic degradation; protease XIV.