New analytical method for determination of phthalates in wastewater by on line lc-gc-ms using the totad interface and fraction collector

Abstract

There is an increasing demand for automatic, reliable and sensitive analytical methods for determining trace levels of phthalic acid esters (PAEs) in environmental samples. While on line coupled liquid chromatography-gas chromatography (LC-GC) has been proof to be a powerful tool for trace-level analyses in complex matrices, the present work presents a new totally automated on line LC-GC method, using the Through Oven Transfer Adsorption Desorption (TOTAD) interface, for the analysis of four of the main phthalates, dibuthyl phthalate (DBP), diethyl phthalate (DEP), dimethyl phthalate (DMP) and diethylhexyl phthalate (DEHP), in a matrix as complex as leachate. The sample is directly injected into the LC injector valve with no sample pretreatment other than simple filtration. The LC step separates the target analytes from matrix interference. Two different LC fractions are collected in a purposely designed fraction collector and then transferred to the TOTAD interface, which concentrates the analytes, totally eliminates the solvent and transfers the analytes to the GC-MS system, where the analysis is carried out. The LOD of the method varied from 0.1 µg/L (DEHP) to 1.4 µg/L (DMP), RSD for retention time below 0.14% and for absolute peak areas below 12% and linearity from 1 µg/L to 1000 µg/L (R2 > 0.99), except in the case of DEHP (linearity from 1 to 250 µg/L, R2 = 0.94). The method was applied to the analysis of the target analytes in samples collected from a municipal solid waste (MSW) landfill in Rosario (Argentina).