Tsumoto Hiroki, Murata Chie, Miyata Naoki, Kohda Kohfuku, Taguchi Ryo
Research Institute of Pharmaceutical Sciences, Musashino University, Shinmachi Nishitokyo-shi, Tokyo 202-8585, Japan.
Rapid Commun Mass Spectrom. 2007;21(23):3815-24. doi: 10.1002/rcm.3279.
We describe a convenient and useful method for the identification and relative quantification of proteins using light and heavy reagents, 1-(6-methylnicotinoyloxy)succinimides (6-CH(3)-Nic-NHS and 6-CD(3)-Nic-NHS, respectively). This method is based on the chemical derivatization of amino groups of tryptic peptides with these reagents, i.e., the basic moiety of the reagents thus incorporated into both the N-terminal amino group and the epsilon-amino group of the lysine residue would improve the ionization efficiency of tryptic peptides. An increase in protein sequence coverage is achieved by derivatization with these reagents or by combination of mass values before and after derivatization. Since a combination of 6-CH(3)-Nic-NHS and d(3)-labeled reagent (6-CD(3)-Nic-NHS) generates a 3 Da mass difference per reaction site, the d(3)-labeled reagent shifts the mass values of d(0)-labeled peptides according to the number of reactive amino groups in the peptides. In the case of tryptic peptides, the mass values of C-terminal arginine and lysine peptides are shifted by 3 and 6 Da, respectively. Further, the 3 Da mass difference between 6-CH(3)-Nic-NHS and 6-CD(3)-Nic-NHS offers a means for the relative quantification of protein by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.
我们描述了一种使用轻试剂和重试剂1-(6-甲基烟酰氧基)琥珀酰亚胺(分别为6-CH(3)-Nic-NHS和6-CD(3)-Nic-NHS)来鉴定和相对定量蛋白质的便捷且有用的方法。该方法基于用这些试剂对胰蛋白酶肽段的氨基进行化学衍生化,即试剂的碱性部分因此同时掺入到赖氨酸残基的N端氨基和ε-氨基中,这将提高胰蛋白酶肽段的电离效率。通过用这些试剂进行衍生化或通过衍生化前后质谱值的组合,可以提高蛋白质序列覆盖率。由于6-CH(3)-Nic-NHS和d(3)标记试剂(即6-CD(3)-Nic-NHS)的组合在每个反应位点产生3 Da的质量差异,d(3)标记试剂会根据肽段中反应性氨基的数量使d(0)标记肽段的质谱值发生偏移。对于胰蛋白酶肽段,C端精氨酸和赖氨酸肽段的质谱值分别偏移3 Da和6 Da。此外,6-CH(3)-Nic-NHS和6-CD(3)-Nic-NHS之间3 Da的质量差异为通过基质辅助激光解吸/电离飞行时间质谱对蛋白质进行相对定量提供了一种方法。