Weight loss supplements that have illegal additives of pharmaceutical drugs or analogues have additional health risks, and customers may not be aware of what they are taking. This research is an essential investigation and quantification of illegally added pharmaceuticals or prescription medications, specifically fluoxetine, phenolphthalein, and sibutramine, in herbal weight loss supplements offered for sale in the United Arab Emirates (UAE). In this case, 137 weight loss supplements were collected and analyzed in this study. Reversed-phase high-performance liquid chromatography with UV absorption detection coupled to tandem mass spectrometry (RP-HPLC-MS/MS) analyses were used to determine the presence of the pharmaceutical chemicals. Among the weight loss supplements, 15.3% (95% CI: 9.2–21.4) contained undeclared sibutramine, 13.9% (95% CI: 8.01–19.7) contained undeclared phenolphthalein, and 5.1% (95% CI: 1.4–8.8) contained undeclared fluoxetine. Amongst all weight loss supplements, 17.5% (95% CI: 11.07–24) contained significant concentrations of either sibutramine, phenolphthalein, or fluoxetine. Whilst weight loss herbal supplements offered for sale in the UAE have relatively low percentages of undeclared pharmaceuticals, many people take several different supplements daily and may encounter quite high levels of combined exposure to toxic compounds.