All pharmaceuticals are separated chromatographically using the liquid chromatographytime of flight/mass spectrometry (LC-ToF/MS) on a 5 µm, 2.1 mm × 250 mm, C18 column at 0.3 mL/min. The recovery is investigated at two spiking levels, 10 and 1 ng/mL; the mean recovery is higher than 77, 84, and 93% in sewage treatment plants (STP) influent, STP effluent, and surface water, respectively. The limit of quantification (LOQ) averages 29, 16, 7, and 2 ng/L in STP influent, STP effluent, surface water, and drinking water, respectively. The matrix effect is also evaluated in STP influent and effluent. It is observed that sulfamethoxazole, prednisolone, ketoprofen, and glibenclamide are highly impacted compared to other compounds, −99, −110, 77, and 91%, respectively. The results show that six out of nine pharmaceuticals, namely atenolol, acetaminophen, theophylline, caffeine, metoprolol, and sulfamethoxazole are detected in STP influent, STP effluent, and surface water. However, the means of concentration are 561, 3305, 1805, 3900, 78, and 308 ng/L for atenolol, acetaminophen, theophylline, caffeine, metoprolol, and sulfamethoxazole, respectively, in STP influent. Caffeine and acetaminophen are detected with the highest concentration, reaching up to 8700 and 4919 ng/L, respectively, in STP influent.