Validation of a High-Performance Liquid Chromatography Method for the Online Determination of Phthalates in Water at a Trace Level

Abstract

A method for the determination of phthalates in water is validated. It includes the sorption of hydrophobic components of a sample on a liquid chromatography column and the separation of analyte concentrated by online reversed-phase HPLC: for the quantitative determination of priority phthalates (PPhs) in surface waters at a trace level; qualitative assessment of the ratio of stable carbon isotopes ¹³C/¹²C in the PPh composition. It is shown that there is no contribution of PPhs from the laboratory background to the measurement results. The limits of determination (0.15−0.22 μg/L) and the accuracy of the determination (±δ = 10−20%) are found using online reversed-phase HPLC and the UV detection of the analytes. The boundary values for the ¹³C/¹²C isotope ratio are substantiated for a qualitative assessment of the results of measuring the Δ¹³C value in the structure of di(2-ethylhexyl) phthalate and its ingress into waters of Lake Baikal from biogenic and abiogenic sources is revealed. A procedure for determining PPhs by reversed-phase HPLC with online UV detection is tested in the field using a portable liquid chromatograph; the concentration ranges for di-n-butyl phthalate (from <0.15 to 1.6 μg/L) and di(2-ethylhexyl) phthalate (from <0.22 to 1.6 µg/L) in the coastal zone of Lake Baikal are evaluated.