Czuczy Noemi, Katona Maria, Takats Zoltan
Cell Screen Applied Research Center, Semmelweis University, Budapest, Hungary.
J Am Soc Mass Spectrom. 2009 Feb;20(2):227-37. doi: 10.1016/j.jasms.2008.09.010. Epub 2008 Sep 18.
A novel mass spectrometric method for the selective detection of specific protein-ligand complexes is presented. The new method is based on electrosonic spray ionization of samples containing protein and ligand molecules, and mass spectrometric detection using the precursor ion scanning function on a triple quadrupole instrument. Mass-selected intact protein-ligand complex ions are subjected to fragmentation by means of collision-induced dissociation in the collision cell of the instrument, while the second mass analyzer is set to the m/z of protonated ligand ions or their alkali metal adducts. The method allows for the detection of only those ions which yield ions characteristic of the ligand molecules upon fragmentation. Since the scan range of first analyzer is set well above the m/z of the ligand ion, and the CID conditions are established to permit fragmentation of only loosely bound, noncovalent complexes, the method is specific to the detection of protein-ligand complexes under described conditions. Behavior of biologically specific and nonspecific complexes was compared under various instrumental settings. Parameters were optimized to obtain maximal selectivity for specific complexes. Specific and nonspecific complexes were found to show markedly different fragmentation characteristics, which can be a basis for selective detection of complexes with biological relevance. Preparation of specific and nonspecific complexes containing identical building blocks was attempted. Complex ions with identical stoichiometry but different origin showed the expected difference in fragmentation characteristics, which gives direct evidence for the different mechanism of specific versus nonspecific complex ion formation.
本文介绍了一种用于选择性检测特定蛋白质 - 配体复合物的新型质谱方法。该新方法基于对含有蛋白质和配体分子的样品进行电喷雾电离,并在三重四极杆仪器上使用前体离子扫描功能进行质谱检测。质量选择的完整蛋白质 - 配体复合离子在仪器的碰撞池中通过碰撞诱导解离进行碎裂,同时将第二个质量分析器设置为质子化配体离子或其碱金属加合物的质荷比。该方法仅允许检测那些在碎裂时产生配体分子特征离子的离子。由于第一个分析器的扫描范围设置在配体离子的质荷比之上,并且建立的碰撞诱导解离条件仅允许松散结合的非共价复合物碎裂,因此该方法在所描述的条件下对蛋白质 - 配体复合物的检测具有特异性。在各种仪器设置下比较了生物特异性和非特异性复合物的行为。优化参数以获得对特异性复合物的最大选择性。发现特异性和非特异性复合物表现出明显不同的碎裂特征,这可为选择性检测具有生物学相关性的复合物提供依据。尝试制备含有相同构建块的特异性和非特异性复合物。具有相同化学计量但来源不同的复合离子在碎裂特征上显示出预期的差异,这直接证明了特异性与非特异性复合离子形成机制的不同。