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 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.
Department of Analytical Chemistry, Nutrition and Food Science, University of Santiago de Compostela, Santiago de Compostela, Spain.
Raquel
R
Sendón
Ana
A
Sanches-Silva
Juana
J
Bustos
Patricia
P
Martín
Nuria
N
Martínez
Ma Eugenia
ME
Cirugeda
D000269:Adhesives / Q000032:analysis*; D000434:Alcoholic Beverages / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005506:Food Contamination / Q000032:analysis; D018857:Food Packaging / Q000295:instrumentation; D010795:Phthalic Acids / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*
D000269:Adhesives; D010795:Phthalic Acids