Monitoring persistent organic pollutants (POPs) with endocrine-disrupting properties poses significant analytical challenges due to labor-intensive, costly, and environmentally unsustainable procedures. This study developed an efficient and robust approach for the simultaneous detection of diverse groups of semi-volatile organics in water and sediment samples using gas chromatography-tandem mass spectrometry (GC-MS). Two extraction methods were studied for determining POPs in water and sediments. For water samples, the solid phase extraction (SPE) method was followed, while for sediments the sonication method was followed by using different solvents. The methods showed good accuracy, with recoveries of 96.41-100% for water and 85.65-100% for sediments, and relative standard deviations under 20%. In greywater, recoveries were 99.14-100% with a relative standard deviation under 18%, and in wastewater, recoveries were 90.52-98.63% with a relative standard deviation under 14%. Detection limits for water samples ranged from 0.023 to 0.037 μg L-1, while for sediments the detection limit ranges from 0.021 to 0.057 μg kg-1. These extraction methods are used to confirm the presence of POPs in environmental samples from the Gulf of Khambat, thereby validating their effectiveness and robustness for analyzing diverse environmental matrices and demonstrating their applicability in comprehensive environmental monitoring programs.