Validation of the method for determining priority phthalates by GC-MS at trace concentrations in surface water with a background pollution level

Abstract

A methodology for determining priority phthalates (PP) at trace concentrations in surface waters with a background pollution level has been validated. Lake Baikal, the largest natural reservoir that retains up to 20% of the world’s fresh surface waters, was chosen as a natural model for the study. Baikal is characterized by a minimal content of suspended organic matter, a low degree of mineralization and a background level of organic pollutants. Four priority phthalates were found in Baikal water: dimethyl phthalate, diethyl phthalate di-n-butyl phthalate and di-(2-ethylhexyl) phthalate present in the concentration range from 0.01 to 0.66 μg/liter. The method for phthalate determination includes a single liquid-liquid extraction of phthalates (Vsample = 1 liter) and direct analysis of the extracts by GC-MS. Considering the minimum content of suspended particles in water and the use of high sensitivity of the mass spectrometry, the stages of sample filtration and concentration of extracts are excluded from the procedure. Deuterated phthalates are used as surrogate internal standards for the quantitative determination of priority phthalates. The laboratory background of phthalates was assessed using reagent-blank methods, exhaustive multiple extraction and subsequent exclusion of the resulting value from the determination result as a systematic error. The limits of phthalate determination (0.01 – 0.17 μg/liter) and the error of determination (±δ from 12 to 38%) were assessed in the concentration range from 0.01 to 0.66 μg/liter. The method was validated during monitoring of persistent organic pollutants in water of Lake Baikal for the period 2015 – 2023.