Stoll V S, Manohar A V, Gillon W, MacFarlane E L, Hynes R C, Pai E F
Department of Biochemistry, University of Toronto, Ontario, Canada.
Protein Sci. 1998 May;7(5):1147-55. doi: 10.1002/pro.5560070508.
The gene encoding the vancomycin resistance protein VanH from Enterococcus faecium, a D-lactate dehydrogenase, has been cloned into a thioredoxin expression system (pTRxFus) and expressed as a fusion protein. The use of several other expression systems yielded only inclusion bodies from which no functional protein could be recovered. Experiments to remove the thioredoxin moiety by enterokinase cleavage at the engineered recognition site under a variety of conditions resulted in nonspecific proteolysis and inactivation of the protein. The intact fusion protein was, therefore, used for kinetic studies and crystallization trials. It has been purified to greater than 90% homogeneity by ammonium sulfate precipitation followed by phenyl Sepharose chromatography. Based on k(cat)/KM for pyruvate, it is 20% as active as native VanH. Michaelis constants for NADPH, NADH, and pyruvate, of approximately 3.5 microM, 19.0 microM, and 1.5 mM, respectively, were comparable to those reported for the native VanH (Bugg TDH et al., 1991, Biochemistry 30:10408-10415). Like native VanH, maximum activity of the fusion protein requires the presence of an anion (phosphate or acetate), however, in addition, a strongly reducing environment is needed for optimal efficacy. Competitive inhibition constants for ADP-ribose, NAD+, and oxamate have also been determined. Crystallization by hanging drop vapor diffusion produced two different crystal forms, one hexagonal and the other tetragonal. Flash-frozen crystals of the tetragonal form diffracted to 3.0 A resolution at a synchrotron radiation source.
编码粪肠球菌中万古霉素抗性蛋白VanH(一种D - 乳酸脱氢酶)的基因已被克隆到硫氧还蛋白表达系统( pTRxFus )中,并表达为融合蛋白。使用其他几种表达系统仅产生包涵体,从中无法回收功能性蛋白。在各种条件下,通过肠激酶在工程化识别位点进行切割以去除硫氧还蛋白部分的实验导致蛋白质非特异性蛋白水解和失活。因此,完整的融合蛋白被用于动力学研究和结晶试验。通过硫酸铵沉淀,随后进行苯基琼脂糖层析,它已被纯化至大于90%的纯度。基于丙酮酸的k(cat)/KM ,其活性是天然VanH的20%。NADPH、NADH和丙酮酸的米氏常数分别约为3.5 microM、19.0 microM和1.5 mM,与报道的天然VanH的米氏常数相当(Bugg TDH等人,1991年,《生物化学》30:10408 - 10415)。与天然VanH一样,融合蛋白的最大活性需要存在阴离子(磷酸盐或乙酸盐),然而,此外,还需要强还原环境以达到最佳效果。还测定了ADP - 核糖、NAD +和草氨酸的竞争性抑制常数。通过悬滴气相扩散结晶产生了两种不同的晶体形式,一种是六方晶系,另一种是四方晶系。四方晶系的快速冷冻晶体在同步辐射源处衍射至3.0 Å分辨率。