Since the 1970s, many analytical methods for the detection of illegal growth promoters, such as thyreostats, anabolics, β-agonists and corticosteroids have been developed for a wide range of matrices of animal origin, including meat, fat, organ tissue, urine and faeces.The aim of this study was to develop an analytical method for the determination of ngL −1 levels of estrogens, gestagens, androgens (EGAs) and corticosteroids in aqueous preparations (i.e. drinking water, drinking water supplements), commercially available on the ‘black’ market. For this, extraction was performed with Bakerbond C 18 speedisk, a technique commonly used in environmental analysis. After fractionation, four fractions were collected using a methanol:water gradient program. Gas chromatography coupled to electron impact multiple mass spectrometry (GC–EI-MS 2 ) screening for the EGAs was carried out on the derivatized extracts. For the detection of corticosteroids, gas chromatography coupled to negative chemical ionization mass spectrometry (GC–NCI-MS) was used after oxidation of the extracts. Confirmation was done by liquid chromatography coupled to electrospray ionization multiple mass spectrometry (LC–ESI-MS 2 ). The combined use of GC and LC coupled to MS enabled the identification and quantification of anabolics and corticosteroids at the low ngL −1 level. This study demonstrated the occurrence of both androgens and corticosteroids in different commercial aqueous samples.