tAlkylphenol polyethoxylates (APEO), surfactants used in the production of textiles, have the potential tomove from the fabric to the skin of the person wearing the clothes, posing an inherent risk of adversehealth consequences. Therefore, the textile industry needs a fast, robust method for determining aqueousextractable APEO in fabrics.The currently-favored HPLC methods are limited by the presence of a mixture of analytes (due to themolecular weight distribution) and a lack of analytical standards for quantifying results. As a result, it hasnot been possible to reach consensus on a standard method for the determination of APEO in textiles.This paper addresses these limitations through the use of reaction-based head space-gas chromatog-raphy (HS-GC). Specifically, water is used to simulate body sweat and extract APEO. HI is then used toreact the ethoxylate chains to depolymerize the chains into iodoethane that is quantified through HS-GC,providing an estimate of the average amount of APEO in the clothing. Data are presented to justify theoptimal operating conditions; i.e., water extraction at 60◦C for 1 h and reaction with a specified amountof HI in the headspace vial at 135◦C for 4 h.The results show that the HS-GC method has good precision (RSD < 10%) and good accuracy (recoveriesfrom 95 to 106%) for the quantification of APEO content in textile and related materials. As such, themethod should be a strong candidate to become a standard method for such determinations.