Linear Alkylbenzene Sulfonates (LAS) are among the priority organic pollutants in sludge owing to their high concentrations, due to its use as a major cleaning agent (surfactant) in laundry detergents and household cleaning products, and to the concentration limits of 2,600 mg/kg outlined in the EU directive draft for land application of sludge. In this work, a method has been optimized and validated for the accurate quantification of LAS homologues C10-C13 in different types of samples in the sludge treatment and disposal process including primary, secondary, and digested sludge, compost, and soil. The type of matrix had a significant impact on the method’s validation process, resulting in the need of the use of distinct dilution factors for each matrix. Overall, the procedure propose involves a cost-effective and user-friendly technique that combines both extraction and clean-up in a single step (ultrasound-assisted extraction and dispersive solid phase extraction). Analytical determination is conducted using liquid chromatography-tandem mass spectrometry. The method demonstrated excellent accuracy (relative recoveries exceeding 84.5 % across all types of sludge samples) and the limit of quantification enables the measurement of LAS concentrations up to 1000 times lower than the concentration limits stipulated in the EU directive draft. For an accurate quantification, three calibration approaches were tested (external calibration, standard addition, and matrix-matched calibration). Standard addition was the preferred method for quantitative analysis. It helps mitigate matrix effects that could otherwise distort the accuracy of analyte measurements, making it crucial for quality control, especially in monitoring applications where matrix effects may introduce bias into concentration calculations.