A method for estimating of the ratio of stable carbon isotopes 13 С/ 12 С in the composition of phthalates from surface water at a trace concentration level is proposed. It is based on the concentration of hydrophobic components of water using an analytical reversed phase HPLC column followed by their gradient separation and detection of eluted phthalates using a high-resolution time-of-ight mass spectrometry (HRMS-TOF) in the form of molecular ions. The ratio of stable carbon isotopes 13 С/ 12 C in phthalates is calculated as a ratio of the peak areas of the monoisotopic masses [M + 1 + H] + and [M + H] + . Commercial phthalates, di-n-butyl phthalate (DnBP) and di-(2-ethylhexyl) phthalate (DEHP), were used as standards. The minimal concentration of DnBP and DEHP in water required for a reliable determination of δ 13 C value is estimated by the level of ca. 0.2 µg L − 1 . The technique has been veri ed during the monitoring of priority phthalates in the waters of Lake Baikal.