Determination of six phthalic acid esters in orange juice packaged by PVC bottle using SPE and HPLC-UV: application to the migration study.

A high-performance liquid chromatographic assay is described for the determination of six phthalic acid esters (PAEs) in orange juice packaged in polyvinyl chloride (PVC) bottle. Samples were extracted by solid-phase extraction (SPE) cartridges and separated by a C₁₈ column. The calibration curves were all linear with a correlation coefficient r > 0.9900. The limits of detection for the assay ranged from 2.6 to 13.8 ng/mL. Expressed as the within- and between-day coefficient of variation (CV), precision was 1.4-13.4% and 1.9-13.3%, respectively, and relative errors were 7.6-12.8% and -9.0-14.2%, respectively. The recovery ranged from 76.8 to 112.3% with the CV from 0.3 to 11.3%. The proposed methodology was applied for studing the migration of the selected PAEs into orange juice packaged in PVC bottle. Di-ethyl phthalate (DEP) and di-(2-ethylhexyl) phthalate (DEHP) were detected in the orange juice without the other four PAEs. Concentrations would increase with the storage time and reach up to 0.385 μg/mL and 0.662 μg/mL, respectively, when the expiration date arrived. The level of DEHP was about 110 times higher than the limiting one in drink water (6 ppb) regulated by U.S. EPA. Results suggest that PVC plasticized by DEHP should not be used as the packaging material for orange juice.