Moriyama Y, Nelson N
J Biol Chem. 1987 Jul 5;262(19):9175-80.
The proton-ATPase of chromaffin granules was purified so as to maintain its proton-pumping activity when reconstituted into phospholipid vesicles. The purification procedure involved solubilization with polyoxyethylene 9 lauryl ether, hydroxylapatite column, precipitation by ammonium sulfate, and glycerol gradient centrifugation. The protease inhibitor mixture used in previous studies inhibited the proton-pumping activity of the enzyme; therefore, the protein was stabilized by pepstatin A and leupeptin. The enzyme was purified at least 50-fold with respect to both ATPase and proton-pumping activity. The ATP-dependent proton uptake activity of the reconstituted enzyme was absolutely dependent on the presence of Cl- or Br- outside the vesicles, whereas sulfate, acetate, formate, nitrate, and thiocyanate were inhibitory. Sulfate inhibition seems to be due to competition with Cl- on the anion-binding site outside the vesicles, whereas nitrate and thiocyanate inhibited only from the internal side. As with the inhibition by N-ethylmaleimide, the proton-pumping activity was much more sensitive to nitrate than the ATPase activity. About 20 mM nitrate were sufficient for 90% inhibition of the proton-pumping activity while 100 mM inhibited only 50% of the ATPase activity both in situ and in the reconstituted enzyme. The possible regulatory effect of anions on the ATP-dependent proton uptake in secretory granules is discussed.
嗜铬颗粒的质子 - ATP酶被纯化,以便在重构到磷脂囊泡中时保持其质子泵活性。纯化过程包括用聚氧乙烯9月桂基醚溶解、羟基磷灰石柱层析、硫酸铵沉淀和甘油梯度离心。先前研究中使用的蛋白酶抑制剂混合物会抑制该酶的质子泵活性;因此,用胃蛋白酶抑制剂A和亮抑蛋白酶肽使蛋白质稳定。该酶在ATP酶和质子泵活性方面至少纯化了50倍。重构酶的ATP依赖性质子摄取活性绝对依赖于囊泡外Cl-或Br-的存在,而硫酸根、乙酸根、甲酸根、硝酸根和硫氰酸根则具有抑制作用。硫酸根抑制似乎是由于与囊泡外阴离子结合位点上的Cl-竞争,而硝酸根和硫氰酸根仅从内部起抑制作用。与N - 乙基马来酰亚胺的抑制作用一样,质子泵活性对硝酸根的敏感性远高于ATP酶活性。约20 mM硝酸根足以使质子泵活性90%受到抑制,而100 mM硝酸根在原位和重构酶中仅抑制50%的ATP酶活性。本文讨论了阴离子对分泌颗粒中ATP依赖性质子摄取的可能调节作用。