Development and validation of an ultra high performance liquid chromatography-tandem mass spectrometry method for the determination of phthalate esters in Greek grape marc spirits

Abstract

An Ultra High Performance Liquid Chromatography – Tandem Mass Spectrometry method has been developed for the analysis of 12 phthalate esters in Greek grape marc spirits. The phthalates were separated on a U-VDSpher PUR 100 C18-E (100 mm x 2.0 mm, 1.8 μm) column by gradient elution. The analytes were ionized by positive electrospray ionization using the multiple reaction monitoring mode. The standard addition method was used for quantification and the Student’s t-test was carried out to evaluate the matrix effect. The accuracy of the method was assessed by recovery experiments resulting in values from 81.6 to 109.6%. The detection limits ranged from 0.3 to 33.3 μg L−1.The proposed method was validated and successfully applied to the analysis of 45 samples collected from Greece and Cyprus. All phthalate esters proved to be present at least once in the analysed grape marc spirits samples, except only in cases of diphenyl phthalate and diisodecyl phthalate, while for the regulated phthalates only bis (2-ethylhexyl) phthalate was quantified above the legislative concentration limits.