Xylazine is a synthetic compound that has escalated concern within United States health and law enforcement agencies due to its increased use as an adulterant in the illicit street drug fentanyl. Numbers of opioid overdoses continue to be significant and the detection of xylazine as an adulterant in illicit drugs is increasing each year. Thus, interest to be able to measure this drug rapidly and effectively in mixed lab samples is escalating. A technique utilizing a chromatography-free workflow by Direct Analysis in Real Time ionization coupled with mass spectrometry (DART-MS) offers simple, quick identification of xylazine. For this study, a mixture containing xylazine, fentanyl, and chlorpromazine spiked into drug-free urine was used to demonstrate the effectiveness of DART-MS. The linear responses of the drugs with respect to the QC samples and across a large detection range ensure that this chromatography-free workflow will be able to detect samples at referenced levels. The ability to conduct rapid analysis of such drugs allows for quicker and more confident treatment decisions to overdose victims, who may not fully respond to current overdose treatments.