The current chapter delves into a comprehensive overview of recent developments in the field of analytical methods for quantification of a new group of chemicals currently classified as chemicals of emerging concern (CECs). This class of emerging contaminants involves compounds from pharmaceuticals and personal-care products, pesticides, steroid hormones, perfluorinated compounds, alkylphenolethoxylates, bisphenol A, phthalates, etc., to name a few. Typically present in extremely low concentrations in environmental samples, CECs typically occur in complex matrices that demand extensive extraction as well as sensitive and specific clean-up procedures. With these requirements in hindsight, the current chapter explores sample extraction techniques and usage of state-of-the-art instrumentation necessary for its quantitation in liquid samples. Current trends in instrumentation point towards usage of liquid chromatography for separation of CECs (in lieu of gas chromatography); development and application of multi-class methods; and also, the increasing popularity of mass spectrometry technique, combined with a veer towards the usage of liquid and gas chromatography. Overall, a review of recent advances in instrumentation hints towards significant progress in analytical techniques for estimation of CECs in liquid samples.