Carbon fiber microelectrodes that support enzyme-containing redox polymer gels permit the amperometric detection of glutamate, choline, and glucose. These devices are of interest for in vivo neurochemical monitoring because their small dimensions may permit highly localized measurements within small brain nuclei. In vitro calibration procedures confirm that the sensors respond in a selective fashion towards their respective target analyte. In the current work, the selectivity of the in vivo response of the microsensors during pharmacological manipulations is considered. The response of choline and glucose microsensors during the local infusion of tetrodotoxin and neostigmine in rat striatum is reported. The results of this study support the conclusion that these microsensors respond selectively to their respective targets under in vivo conditions.