College of Chemistry and Chemical Engineering, Central South University, Changsha, Hunan, P R China.
Anal Chem. 2013 Apr 2;85(7):3660-6. doi: 10.1021/ac303624z. Epub 2013 Mar 11.
The development of new methods that meet the demand of high-throughput, high-fidelity screening of hit compounds is important to researching modalities of important diseases such as neurological disorders, HIV, and cancer. A surface plasmon resonance- (SPR-) based method capable of continuously screening enzyme inhibitors at a single chip with antibody-amplified signal enhancement has been developed. The proof of concept is demonstrated by monitoring the cleavage of chip-confined peptide substrates [a segment of the amyloid precursor protein (APP) with the Swiss mutation] by β-site APP-cleaving enzyme 1 (BACE1). In the presence of a noninhibitor, BACE1 clips the peptide substrate at the cleavage site, detaching a fragment that is homologous to the N-terminus of the amyloid beta (Aβ) peptide. Consequently, a subsequent injection of the Aβ antibody does not lead to any molecular recognition or SPR signal change at the chip. In contrast, suppression of the BACE1 activity by a strong inhibitor leaves the peptide substrate intact, and the subsequent antibody attachment produces an easily detectable SPR signal. Compared to the widely used FRET (fluorescence resonance energy transfer) assay, the method reported here is more cost-effective, as unlabeled peptide is used as the BACE1 substrate. Furthermore, the assay is faster (each screening cycle lasts for ca. 1.5 h) and can be continuously carried out at a single, regenerable SPR chip for more than 30 h. Consequently, excellent reproducibility (RSD < 5%) and throughput can be attained. Two inhibitors were screened, and their half-maximal inhibitory concentrations (IC50) determined by the SPR method were in excellent agreement with values deduced from ELISA and mass spectrometry.
开发满足高通量、高保真筛选命中化合物需求的新方法对于研究神经紊乱、HIV 和癌症等重要疾病的治疗方法非常重要。已经开发出一种基于表面等离子体共振(SPR)的方法,该方法能够在单个芯片上连续筛选具有抗体放大信号增强的酶抑制剂。通过监测芯片上限定的肽底物 [淀粉样前体蛋白(APP)的瑞士突变片段] 的切割来证明该概念,该肽底物由β-位点 APP 切割酶 1(BACE1)切割。在不存在非抑制剂的情况下,BACE1 在切割位点切割肽底物,分离与淀粉样 β(Aβ)肽的 N 末端同源的片段。因此,随后注入 Aβ 抗体不会导致芯片上发生任何分子识别或 SPR 信号变化。相比之下,通过强抑制剂抑制 BACE1 的活性会使肽底物保持完整,随后的抗体附着会产生易于检测的 SPR 信号。与广泛使用的荧光共振能量转移(FRET)测定法相比,该方法更具成本效益,因为未标记的肽被用作 BACE1 底物。此外,该测定法更快(每个筛选循环持续约 1.5 小时),并且可以在单个可再生 SPR 芯片上连续进行 30 小时以上。因此,可以获得出色的重现性(RSD <5%)和高通量。筛选了两种抑制剂,通过 SPR 方法确定的它们的半最大抑制浓度(IC50)与通过 ELISA 和质谱法推断的值非常吻合。