Detection of migration of phthalates from agglomerated cork stoppers using HPLC ‐ MS / MS

Agglomerated stoppers are manufactured from natural cork granules and adhesives. Esters, such as phthalates and adipates, are commonly used in adhesives at concentrations of typically 2–5%. Because of this, and regarding consumer safety, it is necessary to ensure that these compounds do not migrate into the beverage where the cork stopper is used. A reversed‐phase high performance liquid chromatography method with tandem mass spectrometry detection is developed for the separation of nine phthalates into 12% ethanol, used as simulant of alcoholic beverages. The chromatographic separation was carried out with a Luna C 18 (2) HST column (50 × 3.0 mm, 2.5 μm) with a gradient elution of water/methanol with 0.1% acetic acid at 300 μL min −1 . The method was validated for four selected phthalates: di‐butylphthalate, di‐isononylphthalate, di‐isodecylphthalate, and butyl‐benzyl phthalate, with recoveries ranging between 95% and 112% and intralaboratory precision ( RSD ) between 5 and 14%, depending on the phthalate. The lowest quantification limit, 0.15 mg kg −1 , was achieved for di‐butylphthalate. Nevertheless, in all cases, the limits obtained guarantee the method utility if restriction limits set in Commission Regulation No 10/2011 for plastic materials are taken into account.