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).
Highlights
phthalic acid esters (PAEs) are mostly used as plasticizers, especially in polyvinyl chloride (PVC) and as additives in a variety of products [1]
diethylhexyl phthalate (DEHP) and dibuthyl phthalate (DBP) are classified as highly dangerous substances in EU regulations [17] and six PAEs (DBP, diethyl phthalate (DEP), dimethyl phthalate (DMP), di-n-octyl phthalate (DOP), DEHP and benzyl butyl phthalate (BBP)) have been included in the lists of priority pollutants by the European Union [18]
The method developed in the present work involves the on line liquid chromatography-gas chromatography (LC-GC) by means of the Through Oven Transfer Adsorption Desorption (TOTAD) interface using a fraction collector
Summary
PAEs are mostly used as plasticizers, especially in polyvinyl chloride (PVC) and as additives in a variety of products (among them, cosmetics, medical equipment, paints, lubricants, adhesives) [1]. PAEs are categorized as non-persistent organic pollutants because they are continuously being introduced into the environment, present a risk to human health and ecosystems. Low molecular weight PAEs, which means that contain between one and four carbon atoms in their alcohol side chain, such as DBP, DEP and DMP, are used in cosmetic and personal care product [2,3]. DEHP and DBP are phthalates more frequently used plasticizer in PVC [7]. DEHP and DBP are classified as highly dangerous substances in EU regulations [17] and six PAEs (DBP, DEP, DMP, di-n-octyl phthalate (DOP), DEHP and benzyl butyl phthalate (BBP)) have been included in the lists of priority pollutants by the European Union [18]. Some countries have banned phthalates in products designed for children [20,21]
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