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

R Sendón, A Sanches‐Silva, J Bustos… - Journal of separation …, 2012 - Wiley Online Library
R Sendón, A Sanches‐Silva, J Bustos, P Martín, N Martínez, ME Cirugeda
Journal of separation science, 2012Wiley Online Library
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 …
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 C18 (2) HSTcolumn (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.
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