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Monitoring crystallization in real time at the nanoscale can provide valuable new insights into the nucleation process. Herein, the application of nanopipettes as nanoreactors to study the nucleation of organic materials (pharmaceutical crystals) is demonstrated, using bicalutamide (BIC), an active pharmaceutical ingredient of the prostate cancer drug CASODEX, as a model. Crystallization is achieved using a nanoscale antisolvent system, whereby a nanopipette containing an aqueous inert salt solution is brought into contact with a dimethyl sulfoxide (DSMO) solution containing soluble BIC and the same inert salt (at the same concentration). Crystallization is driven and controlled by a combination of the applied bias between an electrode in the nanopipette and one in the bulk DMSO phase and mixing of the two solvents in the mouth of the nanopipette. Crystallization at the tip of the nanopipette causes transient blockages, as BIC particles form and translocate at the end of the nanopipette opening. At low in...

Confined Crystallization of Organic Materials in Nanopipettes: Tracking the Early Stages of Crystal Growth and Making Seeds for Unusual Polymorphs