Terrier Peran, Tortajada Jeanine, Zin Grégoire, Buchmann William
Laboratoire Analyse et Modélisation pour la Biologie et l'Environnement, Université d'Evry-Val d'Essonne, Evry, France.
J Am Soc Mass Spectrom. 2007 Nov;18(11):1977-89. doi: 10.1016/j.jasms.2007.07.028. Epub 2007 Aug 3.
MALDI-MS was evaluated as a method for the study of noncovalent complexes involving DNA oligonucleotides and various polybasic compounds (basic polypeptides and polyamines). Complexes involving single-stranded DNA were successfully detected using DHAP matrix in the presence of an ammonium salt. Control experiments confirmed that the interactions involved basic sites of the polybasic compounds and that the complexes were not formed in the gas phase but were pre-existing in the matrix crystals. Moreover, the pre-existence in solution was probed by isothermal titration calorimetry at concentration and ionic strength similar to those used for mass spectrometry. Spectra showed no important difference between negative and positive ion modes. The influence of nature and size of DNA and polybasic compound on the relative intensities and stoichiometries of the complexes was investigated. Despite the fact that relative intensities can be affected by ionization yields and the gas-phase stabilities of the different species, numerous trends observed in the MALDI study were consistent with the expected in-solution behaviors. Experimental conditions related to sample preparation were investigated also. Complex abundance generally decreased when increasing the ammonium acetate concentration. It was dramatically decreased when using ATT instead of DHAP. Penta-L-arginine is an exception to these observations. Lastly, in the case of complexes involving DNA duplex, the ATT matrix was shown to favor the observation of specific DNA duplex but not that of its complex with polybasic compounds. Inversely, DHAP was appropriate for the conservation of DNA-polybasic compound interaction but not for the transfer of intact duplex.
基质辅助激光解吸电离质谱(MALDI-MS)被评估为一种研究涉及DNA寡核苷酸和各种多元碱性化合物(碱性多肽和多胺)的非共价复合物的方法。在铵盐存在下,使用2,5-二羟基苯甲酸(DHAP)基质成功检测到了涉及单链DNA的复合物。对照实验证实,相互作用涉及多元碱性化合物的碱性位点,并且复合物不是在气相中形成的,而是预先存在于基质晶体中。此外,通过等温滴定量热法在与质谱分析所用浓度和离子强度相似的条件下,对溶液中的预先存在情况进行了探究。光谱显示负离子模式和正离子模式之间没有重要差异。研究了DNA和多元碱性化合物的性质和大小对复合物相对强度和化学计量比的影响。尽管相对强度可能会受到不同物种的电离产率和气相稳定性的影响,但在MALDI研究中观察到的许多趋势与预期的溶液行为一致。还研究了与样品制备相关的实验条件。当增加醋酸铵浓度时,复合物丰度通常会降低。当使用2-氨基-5-噻唑甲酸(ATT)代替DHAP时,复合物丰度会急剧下降。五聚-L-精氨酸是这些观察结果的一个例外。最后,在涉及DNA双链体的复合物的情况下,ATT基质有利于观察特定的DNA双链体,但不利于观察其与多元碱性化合物的复合物。相反,DHAP适合保留DNA-多元碱性化合物的相互作用,但不适合完整双链体的转移。