The two di-substituted rhodamine-based thiacalix<参考文献原文>arene ethyldiamine amide derivative were synthesized from thiacalix<参考文献原文>arene and rhodamine B ethyldiamine by acylation. Under the experimental conditions, the derivatives and Fe3+ are able to form a 1∶1 complex. The formation of complex leaded to the moiety opening of rhodamine, and showed the good fluorescent and colorimetric performance. Among them, the selectivity of 1,3-thiacalix<参考文献原文> rhodamine ethylenediamine amide-2,4-ester to Fe3+ is higher than 1,3-thiacalix <参考文献原文> rhodamine ethylenediamine amide-2,4-acid. The analysis feature of the probes response to Fe3+ was studied by spectroscopy, and synthetic samples were determinec.