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Simultaneous determination of seven phthalic acid esters in beverages using ultrasound and vortex‐assisted dispersive liquid–liquid microextraction followed by high‐performance liquid chromatography
Authors:Pelin Köseo?lu Y?lmaz  Abdulselam Erta?  Ufuk Kolak
Affiliation:1. Department of Analytical Chemistry, Faculty of Pharmacy, Istanbul University, Istanbul, Turkey;2. Department of Pharmacognosy, Faculty of Pharmacy, Dicle University, Diyarbakir, Turkey
Abstract:A sensitive, rapid, and simple high‐performance liquid chromatography with UV detection method was developed for the simultaneous determination of seven phthalic acid esters (dimethyl phthalate, dipropyl phthalate, di‐n‐butyl phthalate, benzyl butyl phthalate, dicyclohexyl phthalate, di‐(2‐ethylhexyl) phthalate, and di‐n‐octyl phthalate) in several kinds of beverage samples. Ultrasound and vortex‐assisted dispersive liquid–liquid microextraction method was used. The separation was performed using an Intersil ODS‐3 column (C18, 250 × 4.6 mm, 5.0 μm) and a gradient elution with a mobile phase consisting of MeOH/ACN (50:50) and 0.2 M KH2PO4 buffer. Analytes were detected by a UV detector at 230 nm. The developed method was validated in terms of linearity, limit of detection, limit of quantification, repeatability, accuracy, and recovery. Calibration equations and correlation coefficients (> 0.99) were calculated by least squares method with weighting factor. The limit of detection and quantification were in the range of 0.019–0.208 and 0.072–0.483 μg/L. The repeatability and intermediate precision were determined in terms of relative standard deviation to be within 0.03–3.93 and 0.02–4.74%, respectively. The accuracy was found to be in the range of –14.55 to 15.57% in terms of relative error. Seventeen different beverage samples in plastic bottles were successfully analyzed, and ten of them were found to be contaminated by different phthalic acid esters.
Keywords:Beverages  High‐performance liquid chromatography  Liquid–  liquid microextraction  Phthalic acid esters
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