Milano Shawn K, Szebenyi Marian D, Cerione And Richard A
Department of Chemistry and Chemical Biology, Cornell University, Ithaca, New York 14853, United States.
Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, New York 14853, United States.
Bio Protoc. 2022 Sep 20;12(18). doi: 10.21769/BioProtoc.4509.
Cancer cells often overexpress glutaminase enzymes, in particular glutaminase C (GAC). GAC resides in the mitochondria and catalyzes the hydrolysis of glutamine to glutamate. High levels of GAC have been observed in aggressive cancers and the inhibition of its enzymatic activity has been shown to reduce their growth and survival. Numerous GAC inhibitors have been reported, the most heavily investigated being a class of compounds derived from the small molecule BPTES (bis-2-(5-phenylacetamido-1,3,4-thiadiazol-2-yl)ethyl sulfide). X-ray structure determination under cryo-cooled conditions showed that the binding contacts for the different inhibitors were largely conserved despite their varying potencies. However, using the emerging technique serial room temperature crystallography, we were able to observe clear differences between the binding conformations of inhibitors. Here, we describe a step-by-step protocol for crystal handling, data collection, and data processing of GAC in complex with allosteric inhibitors using serial room temperature crystallography. Graphical abstract: Figure 1. Workflow for serial room temperature crystallography. Diagram showing the processing and scaling routine for crystals analyzed using serial room temperature crystallography.
癌细胞通常会过度表达谷氨酰胺酶,尤其是谷氨酰胺酶C(GAC)。GAC存在于线粒体中,催化谷氨酰胺水解为谷氨酸。在侵袭性癌症中已观察到高水平的GAC,并且已证明抑制其酶活性可降低癌细胞的生长和存活率。已报道了许多GAC抑制剂,研究最多的是一类源自小分子BPTES(双-2-(5-苯乙酰胺基-1,3,4-噻二唑-2-基)乙基硫醚)的化合物。低温冷却条件下的X射线结构测定表明,尽管不同抑制剂的效力不同,但其结合位点在很大程度上是保守的。然而,使用新兴的连续室温晶体学技术,我们能够观察到抑制剂结合构象之间的明显差异。在此,我们描述了一种使用连续室温晶体学对与变构抑制剂结合的GAC进行晶体处理、数据收集和数据处理的分步方案。图形摘要:图1.连续室温晶体学工作流程。该图展示了使用连续室温晶体学分析晶体的处理和缩放流程。