Iyer Janaki Krishnamoorthy, Otvos Reka A, Kool Jeroen, Kini R Manjunatha
Department of Biological Sciences, Faculty of Science, National University of Singapore, Singapore.
AIMMS Division of BioAnalytical Chemistry, Faculty of Sciences, VU University Amsterdam, Amsterdam, Netherlands.
J Biomol Screen. 2016 Feb;21(2):212-20. doi: 10.1177/1087057115602648. Epub 2015 Aug 31.
Thrombin and factor Xa (FXa) are critical enzymes of the blood coagulation cascade and are excellent targets of anticoagulant agents. Natural sources present an array of anticoagulants that can be developed as antithrombotic drugs. High-resolution, online screening techniques have been developed for the identification of drug leads from complex mixtures. In this study, we have developed and optimized a microfluidic online screening technique coupled to nano-liquid chromatography (LC) and in parallel with a mass spectrometer for the identification of thrombin and FXa inhibitors in mixtures. Inhibitors eluting from the nano-LC were split postcolumn in a 1:1 ratio; half was fed into a mass spectrometer (where its mass is detected), and the other half was fed into a microfluidic chip (which acts as a microreactor for the online assays). With our platform, thrombin and FXa inhibitors were detected in the assay in parallel with their mass identification. These methods are suitable for the identification of inhibitors from sample amounts as low as sub-microliter volumes.
凝血酶和凝血因子Xa(FXa)是血液凝固级联反应中的关键酶,也是抗凝剂的理想靶点。天然来源提供了一系列可开发为抗血栓药物的抗凝剂。已开发出高分辨率在线筛选技术,用于从复杂混合物中鉴定药物先导物。在本研究中,我们开发并优化了一种与纳升液相色谱(LC)联用并与质谱仪并行的微流控在线筛选技术,用于鉴定混合物中的凝血酶和FXa抑制剂。从纳升LC洗脱的抑制剂在柱后以1:1的比例分流;一半送入质谱仪(检测其质量),另一半送入微流控芯片(用作在线分析的微反应器)。利用我们的平台,可在分析中并行检测凝血酶和FXa抑制剂并鉴定其质量。这些方法适用于从低至亚微升体积的样品量中鉴定抑制剂。