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In this work we would like to represent the advantages of Electrospray ionization method (ESI-MASS) as a technique in mass spectrometry witch is widely used for molecular assemblies investigation in macrocyclic chemistry. ESI-MASS is especially useful in producing ions from macromolecules with sequential fragmentation; it is different from other atmospheric pressure ionization processes (e.g. MALDI) since it may produce multiple charged ions, effectively extending the mass range of the analyzer. With high-resolution mass technique this ESI-MASS method can provide the element analysis equivalent data.