Barber M J, Salerno J C, Siegel L M
Biochemistry. 1982 Mar 30;21(7):1648-56. doi: 10.1021/bi00536a027.
The relaxation behavior of the EPR signals of MoV, FAD semiquinone, and the reduced Fe/S I center was measured in the presence and absence of other paramagnetic centers in milk xanthine oxidase. Specific pairs of prosthetic groups were rendered paramagnetic by poising the native enzyme or its desulfo glycol inhibited derivative at appropriate potentials and pH values. Magnetic interactions were found between the following species: Mo--Fe/S I (100-fold increase in microwave power required to saturate the MoV EPR signal at 103 K when Fe/S I is reduced as opposed to oxidized), FAD--Fe/S I and FAD--Fe/S II (70-fold increase in power required to saturate the FADH.EPR signal at 173 K when either Fe/S center is reduced), and Fe/S I--Fe/S II (2.5-fold increase in power to saturate the reduced Fe/S I EPR signal at 20 K when Fe/S II is reduced). The Mo--Fe/S I interaction was also detected as a reduced Fe/S I induced splitting of the MoV EPR spectrum at 30 K. No splittings of the FADH. or Fe/S center spectra were detected. No magnetic interactions were found between FAD and Mo or between Mo and Fe/S II. These results, together with those of Coffman & Buettner [Coffman, R. E., & Buettner, G. R. (1979) J. Phys. Chem. 83, 2392-2400], were used to estimate the following approximate distances between the electron carrying prosthetic groups of milk xamthine oxidase: Mo--Fe/S I, 11 +/- 3 A; Fe/S I-Fe/S II, 15 +/- 4 A; FAD-Fe/S I, 16 +/- 4 A; FAD-Fe/S II, 16 +/- 4 A. A model for the arrangement of these groups within the xanthine oxidase molecule is suggested.
在有和没有牛奶黄嘌呤氧化酶中其他顺磁中心存在的情况下,测量了MoV、FAD半醌和还原态Fe/S I中心的电子顺磁共振(EPR)信号的弛豫行为。通过将天然酶或其脱硫二醇抑制衍生物置于适当的电位和pH值,使特定的辅基对呈现顺磁性。在以下物种之间发现了磁相互作用:Mo--Fe/S I(当Fe/S I被还原而不是氧化时,在103 K下使MoV EPR信号饱和所需的微波功率增加100倍)、FAD--Fe/S I和FAD--Fe/S II(当任何一个Fe/S中心被还原时,在173 K下使FADH·EPR信号饱和所需的功率增加70倍)以及Fe/S I--Fe/S II(当Fe/S II被还原时,在20 K下使还原态Fe/S I EPR信号饱和所需的功率增加了2.5倍)。在30 K时,Mo--Fe/S I相互作用也被检测为还原态Fe/S I诱导的MoV EPR谱分裂。未检测到FADH·或Fe/S中心谱的分裂。在FAD与Mo之间或Mo与Fe/S II之间未发现磁相互作用。这些结果与科夫曼和布特纳[科夫曼,R.E.,&布特纳,G.R.(1979年)《物理化学杂志》83,2392 - 2400]的结果一起,用于估计牛奶黄嘌呤氧化酶的载电子辅基之间的以下近似距离:Mo--Fe/S I,11±3 Å;Fe/S I - Fe/S II,15±4 Å;FAD - Fe/S I,16±4 Å;FAD - Fe/S II,16±4 Å。提出了这些基团在黄嘌呤氧化酶分子内排列的模型。