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Histidine Polypeptide-Hybridized Nanoscale Metal–Organic Framework (fH12/ZIF-8) can be produced effectively in water at room temperature without using any additives. The fluorescein label also provides a useful method to quantify the extent to which the anti-cancer drug doxorubicin (DOX) is loaded into or released from the resulting MOFs. In vitro studies have shown that fH12/ZIF-8 has the useful property of dissolving and controlled rates at low pH. It ruptured fastest in PBS buffer solution with pH 6.3, and the release rate reached 50% at 4 h. Furthermore, it showed that the addition of histidine polypeptides increases uptake by HepG-2 cells. This study integrates drug loading and detecting aspects into a single theranostic platform by a simple and efficient strategy, opening a new route for the construction of advanced drug delivery systems.