This paper describes an enhanced gas chromatography mass spectrometry (GC-MS) strategy for the analysis of Miconazole in water samples. In this study, determination of Miconazole has been carried out according to standard method for water and waste water analysis. Samples of collected water were agriculture stream water, River Nile water and Hospital waste water samples from El-Gharbia governorate in Egypt. Miconazole was extracted by solid - liquid extraction and analyzed by GC-MS. The chromatographic separation was performed using a ZB5 column (30 m ×0.53 mm, 1.50 µm), and helium as a carrier gas. The limit of detection and limit of quantification for Miconazole were 0.75and 2.50 ng/mL respectively. The intra- and inter-day precisions were lower than 0.85% while the accuracy ranged from 98.55% to 101.53. Finally, solid phase extraction (SPE) in combination with GC-MS is a sensitive and effective method for the determination of Miconazole in water samples.