Highly phosphorylated nucleotides were investigated to assure whether the eucaryotic Aspergillus niger produce these substances or not during the differentiation. Investigation was extended to see how organic phosphate interacts with inorganic polyphosphate during development, and high molecular weight RNA-polyphosphate complex was detected in 2.6% polyacrylamide gel by electrophoresis. Guanosine tetraphosphate was found in vesicle and phialide forming mycelia and spore forming body by PEI cellulose TLC. It is revealed that guanosine tetraphosphate is a common substance for spore formation in eucaryotic microorganisms as well as in procaryotic. Especially, prior to sporulation, protein bound RNA and protein bound phosphate may occur as a result of reorganization of cellular materials. The evidence was obtained by the fact of differential increase of optical density ratio between the samples from different developmental stages of this fungus. In 2.6% polyacrylamide gel which was run to electrophoresis, high molecular weight RNA (mostly rRNA) was found to couple and to make RNA-polyphosphate complex. The complex was examined with enzymes and radioactive isotope of $^{32}P$. (enzymic test was not reported here.) RNA-polyphosphate complex might be another sort of highly phosphorylated nucleotide or rRNA beside guanosine-tetraphosphate.