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Abstract Pharmaceutical residues as emerging contaminants have a great interest in recent days. In Egypt, studies on the occurrence of pharmaceutical residues in municipal waste water is limited so it is important to assess its levels in municipal waste water as an initial step to evaluate the nature of the problem in different water masses in Egypt. This research was done to quantify the concentration of antibiotics from different classes (Macrolides: Azithromycin, Fluoroquinolones: Ciprofloxacin, Sulfonamides: Sulfamethoxazole), Nonsteroidal anti-inflammatory drugs (NSAID) (diclofenac) and central nervous system stimulant (caffeine). Furthermore, the study aimed to test the efficiency of layered double hydroxide nanomaterial (Zn-Fe LDH).in the removal of diclofenac. Samples were collected from both the influent and effluent of Tezmant waste water treatment plant, Beni-Suef governorate, Egypt in summer and winter seasons. Environmental protection agency method for detection of pharmaceutical was adopted (EPA,2007). The extraction process was done using Hydrophilic-Lipophilic-Balanced, reversed-phase sorbent solid phase extraction (HLB-SPE). The analysis was done using liquid chromatography tandem mass spectrometry (LC-MS/MS) with positive ion electrospray ESI (+). Limit of detection (LOD), Limit of quantification (LOQ) and recovery were calculated to validate the method. Recovery ranges from 58.5% to 80.97%. Zn-Fe LDH was prepared by co-precipitation method, characterized using different analytical techniques to investigate the properties of the adsorbent. Also, different experimental conditions such as pH and dose of adsorbent were tested to achieve the high removal efficiency. The present findings indicate the presence of all the studied pharmaceuticals in wastewater samples during the winter season and more than 85% were detected in summer samples. Antibiotics concentrations were high in winter season than summer that reflect the high use and low removal from waste water. Caffeine is the highest detected compound in all samples with maximum concentration of 27.85 µg/L in the influent of a winter season sample. Waste water treatment plant showed higher removal efficiency for caffeine and azithromycin while low removal rate is noticed for azithromycin and negative removal is noticed for sulfamethoxazole. Additionally, the calculated ecological risk is high for diclofenac, ciprofloxacin and sulfamethoxazole. The adsorption effectiveness of diclofenac using Zn-Fe LDH was high effective and showed rapid adsorption rate within the first 10 minutes. |