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Detection of migration of phthalates from agglomerated cork stoppers using HPLC ‐ MS / MS
Author(s) -
Sendón Raquel,
SanchesSilva Ana,
Bustos Juana,
Martín Patricia,
Martínez Nuria,
Cirugeda Ma Eugenia
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201100871
Subject(s) - chromatography , chemistry , cork , phthalate , detection limit , high performance liquid chromatography , mass spectrometry , acetic acid , wine , biochemistry , organic chemistry , food science
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.