Bruno S, Schiaretti F, Burkhard P, Kraus J P, Janosik M, Mozzarelli A
Institute of Biochemical Sciences, University of Parma, 43100 Parma, Italy.
J Biol Chem. 2001 Jan 5;276(1):16-9. doi: 10.1074/jbc.C000588200.
Human cystathionine beta-synthase is a pyridoxal 5'-phosphate enzyme containing a heme binding domain and an S-adenosyl-l-methionine regulatory site. We have investigated by single crystal microspectrophotometry the functional properties of a mutant lacking the S-adenosylmethionine binding domain. Polarized absorption spectra indicate that oxidized and reduced hemes are reversibly formed. Exposure of the reduced form of enzyme crystals to carbon monoxide led to the complete release of the heme moiety. This process, which takes place reversibly and without apparent crystal damage, facilitates the preparation of a heme-free human enzyme. The heme-free enzyme crystals exhibited polarized absorption spectra typical of a pyridoxal 5'-phosphate-dependent protein. The exposure of these crystals to increasing concentrations of the natural substrate l-serine readily led to the formation of the key catalytic intermediate alpha-aminoacrylate. The dissociation constant of l-serine was found to be 6 mm, close to that determined in solution. The amount of the alpha-aminoacrylate Schiff base formed in the presence of l-serine was pH independent between 6 and 9. However, the rate of the disappearance of the alpha-aminoacrylate, likely forming pyruvate and ammonia, was found to increase at pH values higher than 8. Finally, in the presence of homocysteine the alpha-aminoacrylate-enzyme absorption band readily disappears with the concomitant formation of the absorption band of the internal aldimine, indicating that cystathionine beta-synthase crystals catalyze both beta-elimination and beta-replacement reactions. Taken together, these findings demonstrate that the heme moiety is not directly involved in the condensation reaction catalyzed by cystathionine beta-synthase.
人胱硫醚β-合酶是一种含磷酸吡哆醛的酶,包含一个血红素结合结构域和一个S-腺苷-L-甲硫氨酸调节位点。我们通过单晶显微分光光度法研究了一个缺乏S-腺苷甲硫氨酸结合结构域的突变体的功能特性。偏振吸收光谱表明,氧化型和还原型血红素可可逆形成。将还原型酶晶体暴露于一氧化碳中会导致血红素部分完全释放。这个过程可逆发生且无明显晶体损伤,便于制备无血红素的人酶。无血红素的酶晶体呈现出磷酸吡哆醛依赖性蛋白典型的偏振吸收光谱。将这些晶体暴露于浓度不断增加的天然底物L-丝氨酸中,很容易导致关键催化中间体α-氨基丙烯酸酯的形成。发现L-丝氨酸的解离常数为6 mM,与在溶液中测定的值相近。在L-丝氨酸存在下形成的α-氨基丙烯酸酯席夫碱的量在pH值6至9之间与pH无关。然而,发现α-氨基丙烯酸酯消失的速率(可能形成丙酮酸和氨)在pH值高于8时会增加。最后,在同型半胱氨酸存在下,α-氨基丙烯酸酯-酶吸收带很容易消失,同时形成内醛亚胺的吸收带,表明胱硫醚β-合酶晶体催化β-消除和β-取代反应。综上所述,这些发现表明血红素部分不直接参与胱硫醚β-合酶催化的缩合反应。